Radiation Curing Test Methods - infoHouse

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RADIATION CURING
TEST METHODS
AUTHOR
Camille J. Kallendorf
Technical Committee Chair
Radtech International
Borden Chemical
Cincinnati, Ohio
David Cyterski
Lord Corporation
Erie, Pennsylvania
CO-AUTHORS
Anne Spinks
Henkel Corporation
La Grange, Illinois
David Dreifus
Loctite Corporation
Newington, Connecticut

President's Message
RadTech International is pleased to present this First Edition of the RadTech International Radiation
Curing Test Methods.
As the use of radiation curing technology expands there has been a stated need from the users for
a single-source reference for test methods directly related to this technology. With this in mind, the
RadTech International Radiation Curing Test Methods book was prepared by the Technical
Committee of RadTech International for distribution at RadTech's first major event: The RadTech
'88 -- North America Conference and Exposition in New Orleans, April 24-28, 1988 -- the largest
radiation curing exposition to date. RadTech will hold these Conferences in North America biannually.
The Technical Committee proposes to update this manual every two years in conjunction with
the North American Conferences. RadTech International believes this text will be of service to you
as you evaluate your UV/EB coatings, inks and adhesives.
RadTech International was founded in mid-1986 as a nonprofit organization to serve the needs of
all of the radiation curing and processing industry -- supplier, user, and prospective user. Membership
in the association is open to any individual engaged in or interested in the radiation curing and
processing industry. In just 21 months, RadTech International membership has grown to 400 individuals,
primarily users. The association currently operates through seven committees: Membership,
Technical, Marketing, Program, Editing, Exhibit and Users.
Additional information about membership, publications, seminars and other activities may be obtained
from RadTech International, 60 Reevere Drive, Suite 500, Northbrook, Illinois 60062 U.S.A.,
312/480-9576.
Alice Pincus
President
RadTech International
NOTI= By publishing this book, RadTech International and its members do not warrant the information and test
methods contained herein as proper under all conditions and expressly disclaim any responsibility for damages arising
from the use, application or reliance on the information and test methods contained herein.
0 1988 RadTech International
All RiPhts Reserved
ASTM Standards included in this Manual are reprinted with permission from the Annual Book of ASTM Standards,
copyright American Society for Testing and Materials, 1916 Race Street, Philadelphia, Pennsylvania 19 103.
..
11

(m Designation: D 5403 - 93
Standard Test Methods for
Volatile Content of Radiation Curable Materials'
1. !hope
1.1 These test methods cover procedures for the determination
of weight percept volatile content of coatings, inks,
and adhesives designed to be cud by exposure to ultraviolet
light or to a beam of accelerated electrons.
1.2 Test Method A is applicable to radiation curable
materials that arc essentially 100 96 reactive but may contain
traces (no more than 3 %) of volatile materials as impurities
or introduced by the indudon of various additives.
1.3 Test Method B is applicable to all radiation curable
matenah but must be uscd for materials that contain volatile
solvents intentionally introduced to control application viscosity
and which am intended to bc removed from the
material prior to cwc.
I .4 These test methods may not bt applicable to radiation
curable materials wherein the volatile material is water, and
other procedures may be substituted by mutual consent of
the producer and user.
1.5 This stondard does not purport to address all of the
sdety problems: Q any, associated with its use, It is the
responsibiIity of the user of this stan&rd to establish appro
priate safay and health practices and determine the applicability
of regulatory limitations prior to use. A spec& hazard
statement is given in Note 9.
2. Referenced Documents
2.1 ASTM Standards:
D 2369 Test Method for Volatile Content of Coatings2
E 145 Specification for Gravity Convection and Forced
Ventilation Ovens3
E 177 Practice for Use of the Terms Precision and Bias in
ASTM Methods3
E 69 1 hdce for Conducting an Interlaboratory Study to
Determine the Precision of a Tcst Method'
3. Terminology
3.1 Definitions:
3.1.1 me-the condition of a wating after conversion to
the final state of cun as measured by tests generally related
to end use performance and mutually agreeable to supplier
and purchaser.
3.1.2 ultraviolet (Uv) curing-conversion of a coating
from its application state to its final use state by means of a
mechanism initiated by ultraviolet radiation generated by
equipment dcsigned.for that purpose.
3.1.3 electron beam (EB) curing-wnversion of a coating
its application state to its final use state by means of a
mechanism initiated by elcctron beam radiation generated
by equipment designed for that purpose.
3.1.4 processing volatile-loss in specimen weight under
test mnditims that arc desigoed to simulate actual industrial
cum processing conditions.
3.1.5 potential vofatiles-loss in specimen weight upon
heating at 1 IO'C for 60 ruin after radiation curing.
D1scu5910~-Thi~ value is an estimation of volatile loss that may
occur during aghg or under extreme storage conditions. Potential
4
volatiles may also be rcfd to as residual volatila.
3.1.6 total volatiles-sum of the proCessing volatiles and
the potential volatila.
I from
4. Summary of Test Methods
4.1 A designated quantity of material is weighed before
and after a cure step that simulates normal industrial
proctssing. The test specimen is weighed again after heating
at 110 f 5% for 60 dn. The percent volatile is calculated
From the losses in weight.
5. Significance and Usa,
5.1 Thest test methods an the procedures of choice for
determining volatile content of materials designed to be
cured by exposure to ultraviolet light or electron beam
irradiation. These types of materials contain liquid reactants
that react to become part of the film during cure, but, which
under the test conditions of Test Method D2369, will be
erroneously measured as volatiles. The conditions of these
test methods am Similar to Test Method D2369 with the
inclusion of a step to curc the material prior to weight loss
determination. Volatile content k determined as two separate
components-pmmsing volatiles and potential
~olatilm. processing v~latiles L z measilre of voiatiic ioss
during the actual CUR process. Potential volatiles is a
measure of volatile loss that might occur during aging or
under extreme storage conditions. Thesc volatile content
measurements an useful to the producer and user of a
material and to environmental interests for determining
emissions.
6. Interferences
6.1 The degree to which the results of thest procedures
accurately measure the volatiles emitted during actual use is
absolutely dependent upon proper cure during the test
procedure. Although overcure will have little or no effect
upon measured volatiles, undercure may lead to erroneously
1
W

@ D5403
high values. Since various pieces of cure equipment may
vary widely in efficiency, it is essential that dialogue between
matvial manufactunr and Wng laboratory establish a cure
schedule appropriate both to the material to be tested and to,
the cure equipment to be used in the procedure. 1
7. scope
TE!X METHOD A
7.1 This test method is applicable to radiation curable
mataids with solvent content less than or equal to 3 %.
e a. ~ p p u ~ t ~
8.1 Aluminum Substrae, stan&ud test pan& ( 102 mm by
305 nun) or heavy gage (0.05 mm minimum) foil. Test
pan& an most convenient and may be cut into smaller
pieccs for east of weighing. Pncondition the substrate for 30
min at 110 i j% and Store in a desiccator prior to use.
8.2 Fod Drd Oven, Type IIA or Type IIB E;S specified
in Specification E 145.
8.3 Ultraviolet L&ht or Electron Beam Curing Equip
ment-Thm arc Lmcral cml"m supplim of labratory
scale equipment that simulatts industrial curing processts?
9. Procedure
9.1 Mix the sample, if ncctssBry, to ensure uniformity.
Hand stirring is recommended to avoid the entrapment of
air bubbles.
9.2 Weigh the preconditioned aluminum substrate, (8.1)
to 0.1 mg (A). The sire of the aluminum substrate must
allow a minimum of Oi2 g of material to be applieQ at the
supplier's rccOmmcndcd film thickness. Usc rubber gloves or
tongs, or both, to handle samples.
9.3 Apply a minimum of 0.2 g of test specimen to the
aluminum substrate and reweigh to 0.1 mg (B). Preparc a
total of three test Specimens.
9.4 Cun the test &men by exposur~ to W or EB as
pnscribed by the supplier of the material.
9.5 Allow the test specimen to cool 15 min at room
temperatwe and d g h to 0.1 mg (C).
9.6 Heat the test specimcp in a forced draft oven (8.2) for
60 min at 110 f YC.
NOTE 3-MUuiaIs that can react with atmospheric moisture during
port cure, thu 4 UV ationicuuabk epoxy mataials, may exhibit a
wWt gain d e procedure in 9.6. If this OCCUIJ, the sample should be
retatad md rllowtd to port cun at room temperature for 48 h OAer
procedure h 9.5, and then rcwigkd prior to procedure in 9.6. The
weight aAer post cure should then be used as Weight C in the calculation
of percent potential volatila in 10.1.
9.6 Allow the test specimen to cool to room temperature
in a desiccatOr and d g h to 0.1 mg, (D).
10. cal~tioar
10.1 Calculate the weight percent volatiles as follows:
pnxxssine VOlatileJ - 100 [(B - c)/(B - A)]
Potential Volatiles = 100 [(C - D)/(B - A)J
Total volatiles - 96 procesinS Volatiles + 96 Potential Volatiles
whm
A = weight of aluminum substrate, g,
B = weight of aluminum substrate plus test specimen, g,
(1)
(2)
C = wight of aluminum substrate plus test specimen after
a, gl and
D = weight of aluminum substrate plus cured test specimen
after heating.
11. Reiish and Bias
1 1.1 Interlaboratory Test Program-An interlaboratory
studf of volatile content of radiation cured materials (Test
Method A) was conducted in accordance with Practice E 69 1
in nine laboratories with three materials, with each laboratory
obtaining three test results for each material.
11.2 Test Result-The precision information given below
for volatile content in weight percent is for the comparison of
two test results, each of which is the average of three test
determinations.
1 1.3 Precision:
Roardw Vohtila
95 Z reprt.bility limit (within Lbontory)
95 Z rrprodudbiiity limit (khwan kbonlorics)
Potential VoLtila
95 % rcpat.bility Limit (within Lbontory)
95 I nproducibiiity limit (baw&n kbontorics)
Total Vdrtiies
95 % npatability limit (within Lbomlory)
95 % ~ucibility limit (baw&n Lbontoria)
Perant
0.9
I .6
2.1
4.2
The terms repeatability limit and reproducibility limit are
used as spcci6cd in Practice E 177. The rtspaCtive standard
deviations among test results may be obtained by dividing
the limit values by 2.8. The form of this pdon statement
is in accordance with Practice E 177,31.1.
11.4 Bias--Since there is no accepted reference material
or method, or laboratory suitable for determining the bias for
$e p&m in *w *db method €O€ mzasuring the voiatiie
content of radiation cured mate% no statement of bias is
being made.
TE2T METHOD B
12. scope
12.1 This test method is applicable to all radiation curable
materials that will cure properly at the designated specimen
2.3
3 9
2

7
,
(9 D5403
weight, which corresponds to a film thickness of 50 to 75 pm
depending upon solvent content. Test Method B is the
method of choice for all radiation curable materials with
solvent content greater than 3 X.
12.2 This test method is not applicable to maten&
containing styrene due to its volatility at 50'C.
13. Apparatus
13.1 Aluminum Foil Dish, 58 mm in diameter by 18 mm
in height with a smooth (planar) bottom surface. Precondition
the dishes for 30 min in an oven at I10 f 5'C and store
in a desiccator prior to use.
13.2 Forced DraJ Oven, Type IIA or Type IIB as specified
in Specification E 145.
NOTE &The shelves of the oven must be level.
13.3 Syringe, 1 mL, capable of properly dispensing the
material under test at suficient rate that the specimen can be
dissolved in the solvent. Disposable syringes are recommended.
13.4 Ultraviolet Light or Electron Beam Curing Equip
menf-There an several commercial suppliers of laboratory
scale equipment that simulates industrial curing proctsses.'
14. Reagents
14.1 Purify of Reagenfs-Reagent grade chemicals shall
be used in all tests. Unless otherwise indicated, it is intended
that all reagents shall conform the specifications of the
Committee on Analytical Reagents of the American Chemical
Society, where such specifications are available.6 Other
grades may be used, provided it is first ascertained that the
reagent is of sufficiently high purity to permit its use without
lessening the accuracy of the determination.
15. Procedure
15.1 Mix the sample, if necessary, to ensure uniformity.
Hand stimng is recommended to avoid the entrapment of
air bubbles.
15.2 Weigh a preconditioned aluminum dish (1 3.1) to 0.1
mg (A). Use rubber gloves or tongs, or both, to handle
sample dishes.
15.3 Using the syringe (see 13.3) weigh to 0.1 mg (B), by
difference, 0.3 f 0.1 g of test specimen into the foil dish to
which has been added 3 f 1 mL of acetone. Add the material
dropwise, swirling the dish to disperse it completely in the
acetone. If the material forms a lump that cannot be
dispersed, discard the test specimen and prepare a new one.
Prepare a total of three samples.
NOTE 5-Be sure to wipe the outer surface of the syringe clean after
obtaining the test specimen. Pull the syringe plunger up 114 of an inch to
pull the material away from the neck of the syringe. Cap and weigh the
syringe. Ancr dispensing the test specimen, do not wipe the tip of the
syringe. Remove the material from the neck of the syringe by pulling up
the plunger. Cap and reweigh the syringe. Note that sample weight (B)
equals initial weight syringe minus final weight syringe.
NOTE &Use disposable rubber doves or polyethylene to handle the
syringe.
NOTE 7-If the material is not compatible with acetone,
tetrahydrofuran (THF) or a blend of acetone and THF may be
substituted.
15.4 Heat the samples in the forced draft oven (see 13.2)
for 30 min at 50 i 2'C.
3
N m I-This step is Critical since I large amount of solvent present
in the sample during cure will interfere with the cure process and an
inadequate degree of cure may result, which could produce erroneous
volatile results (see 6.1). If the material contains only very fast solvents,
a lower temperature/shomr time may be substituted if it can be
demonstrated that the conditions arc adequate to remove at leas( 90 %
of the original solvent in the composition. Any remaining solvent will be
removed during the subsequent cun and heating steps. In the case of
samples that contain volatile solvents for control of application viscosity,
this step also simulates the industrial p d n g stage nccQsary
to remove the solvent prior to cure.
15.5 Cure the test specimen by exposure to UV or EB as
prescribed by the supplier of the material (see Note 2).
15.6 Allow the test specimen to cool for 5 min at room
temperature and reweigh (0.
15.7 Heat the test specimen in the forced draft oven (see
13.2) for 60 min at 110 f 5%.
NOTE 9 Precaution-In addition to other precautions, provide adequate
ventilation, consistent with accepted laboratory practice, to
prevent solvent vapon from accumulating to a dangerous level.
15.8 Allow test specimen to cool to room temperature in a
desiccator and reweigh (D).
16. Calculations
16.1 Calculate the weigh percent volatiles as follows:
Processing Volatiles - 100 (B - (C - A)]/B (3)
Potential volatiles = 100 ((C - D)/B]
Total Volatiles - 96 Processing Volatiles + 96 Potential Volatiles
where:
A = weight of aluminum dish, g,
B = weight of test specimen, g,
C = weight of aluminum dish plus test specimen after initial
heating and cure, g and
D = weight of aluminum dish plus cured test specimen after
final heating, g.
17. Precision and Bias:
1 7.1 Interlaboratory Test Program-An interlaboratory
study of volatile content of radiation cured materials (Test
Method B) was conducted in accordance with Practice E 69 1
in eleven laboratories with three materials, with each Igboratory
obtaining three test results for each material.
17.2 Test Result-The precision information given in
17.3 for volatile content in weight percent is for the
comparison of two test results, each of which is the average
of three test determinations.
1 7.3 Precision:
Fbcasing Volatila
95 96 repeatability limit (within laboratory)
95 I reproducibility limit (between Irbontoria)
Potential Volarila
95 96 repeatability limit (within laboratory)
95 96 reproducibility limit (ktmcn Irbontoria)
Total Vohh
95 96 rrpertability limit (within laboratory)
95 96 reproducibility limit (between labontoria)
Percent
2.0
3.4
1.1
4.1
2.0
5.1
The terms repeatability limit and reproducibility limit are
'Supporting data uc available from ASTM Hcadquuun. Request "I-
1083.
(4)

(& D5403
I
used as specified in Practice E 177. The respective standard
deviations among test results may be obtained by dividing
the limit values by 2.8. The form of this precision statement
is in accodmce with Practice E 177,31.1.
c
17.4 Bim4ince then is no accepted refennix material,
method, or laboratory for determining the bias for the
p d m in this test method for measuring volatile content
of radiation Cured materials, no statement on bias is being
made.
18*
18.1 elcctron beam curing; radiation curable material;
radiation curing; ultraviolet curing; volatile content
4

Table of Contents
..
President's Message ............................................. 11
Chapter 1: Coatings
Introduction .......................................................... 2
Color .................................................................... 2
Density ................................................................. 2
Reactivity ............................................................. 2
Refractive Index ................................................... 2
Rheology .............................................................. 4
Shelf-life Stability ................................................ 4
Surface Tension ................................................... 4
Chemical Functionality ........................................ 6
Wear Resistance (Abralion) ................................ 6
Surface Slip .......................................................... 6
Hardness .............................................................. 6
Gloss .................................................................... 8
Glass Transition Temperature .............................. 8
Tensile Properties ................................................ 8
Flexibility ............................................................. 8
Chemical Resistance ............................................ 8
Barrier Properties ................................................ 10
Adhesion ............................................................. 10
Residual Unsaturation ......................................... 10
Residual Monomer .............................................. 10
Volatiles .............................................................. 10
Exposure Testing ................................................ 10
Conclusion .......................................................... 11
Chapter 2: Inks
Introduction ......................................................... 15
Grind ................................................................... 15
Tack .................................................................... 15
Hardness ............................................................. 15
Color and Strength .............................................. 15
...
111

Chapter 3: Adhesives
Introduction ......................................................... 18
Rheology ............................................................. 18
Tensile Tests ....................................................... 18
Volatiles .............................................................. 18
Barrier Properties ................................................ 18
Hardness ............................................................. 20
Refractive Index .................................................. 20
Flexibility ............................................................ 20
Tack .................................................................... 20
Electrical ............................................................. 20
Thermal Properties .............................................. 20
Strength of Bonds ............................................... 21
Peel ..................................................................... 21
Fatigue Life ......................................................... 22
Solvent Resistance .............................................. 22
Exposure Testing ................................................ 22
Temperature and Humidity Testing .................... 22
Chapter 4: Troubleshooting
Before Processing ............................................... 26
During Processing ............................................... 28
After Exposure to Radiation ............................... 28
t
Chapter 5: Glossary
Glossary .............................................................. 31
Appendixes
1 . 12 Test Methods ...........................................
38
13 ASTM Methods ....................................... 43
14 Common Abbreviations and Symbols .... 428
15 Common Units and Conversion Factors . 429
16 Temperature Conversion Table .............. 430
17 Advertiser Index ..................................... 433
iv

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CHAPTER 1
COATINGS
1

I
INTRODUCTION
Radiation cured inks, coatings and adhesives are formulated
for a variety of end uses, and have a wide range of
desired properties; however, certain basic properties are
universal, regardless of application. In many cases these properties
are inter-related, that is, alteration of one causes another
to change.
This book is a reference document only. The book draws
upon the experience of the technical committee of RadTech
International. Where appropriate, ASTM (American Society
for Testing Materials) test procedures are referenced. If
the method is not an ASTM procedure, the method is provided
in the appendix as are the ASTM methods. The
usefulness of the various tests is discussed, as well as the advantages
and disadvantages of the procedures.
In addition, there is a chapter on troubleshooting radiation
curable materials. A glossary of terms applicable to radiation
curing is at the end of the book, as well as some useful
tables.
For all cured film properties, the method and extent of
cure will affect the results.
LIQUID COATING PROPERTIES
COLOR
It is often desirable for radiation curable clear coatings
to function as a protective topcoat for a substrate without altering
the color of the substrate. Many of these coatings possess
a pale tan to yellow/gold tint. Variation in color from batch
to batch of a given formulation may indicate differences in
concentration of individual components or the presence of
a contaminant. Properties such as viscosity and cure speed
should be checked if a variation in color is noted.
Of the three methods listed, the Gardner Color Scale is
the quickest. It is, however, based upon the comparative
judgement of what the operator sees, and as such it is a subjective
test. For greater accuracy the Platinum-Cobalt Scale
or the Hunter Color Difference Methods are recommended.
The latter two procedures require the purchase of spectrophotometers,
and therefore are more expensive. In addition,
they are more difficult to perform and require more time
than does the Gardner Color Scale.
Name: Gardner Color Scale.
r’ropeny Xeasured: Coior.
Method: ASTM D1209
Comments: See ASTM D2849 for the preparation and
calibration of standards. Color standards can be purchased from
companies such as Hellige Inc., Garden City, N.J.
Necessary Equipment: Calibrated color standards. Gardner-
Holdt tubes, clear glass with flat bottoms.
Name: Platinum-Cobalt Scale.
Property Measured: Color.
Method: ASTM D2849.
Comments: See ASTM D2849 for the preparation and
calibration of standards.
Necessary Equipment: Calibrated color standards, Nessler tubes
(matched, lOOml, tall form), and spectrophotometer.
Name: Hunter Color Difference.
Property Measured: Color.
Method: ASTM E450.
Comments: Measures the color of low colored liquids
regardless of hue. Water is used as the reference.
Necessary Equipment: Hunterlab Color Difference Meter,
absorption cells, and pure water.
DENSITY
Since radiation curable coatings are near 100% reactive
(i.e. non-volatile products), knowledge of the density of the
liquid is indicative of the weight of the film per area of coated
substrate, i.e. the mileage. Variations in coating density from
batch to batch of the same formulation may indicate potential
variation in the concentration of its components. Reproducibility
of .2#/gal is normal. The test is easy to perform and
rapid.
Name: Weight per Volume.
Property Measured: Density.
Method: ASTM D1475.
Comments: Test must be run at constant temperature.
Necessary Equipment: Weight per gallon cup or pycnometer,
thermometer, and laboratory balance, accurate to .01 gram.
REACTIVITY
Reactivity test methods are designed for quality control.
The speed of cure of a “test” batch is compared to that of
an “acceptable” batch. A “test” batch that is slower or faster
in cure may indicate either a concentration variation of one
or more of the components or the presence of a contaminant.
The method is also used to evaluate the relative cure speed
of new formulations.
The Speed of Cure Versus a Standard is easily done but
is subjective in nature. The Infrared Spectroscopy Method
measures the diszppearance of double bonds. Since the IR
is not very quantitative, this method is also not very accurate
and in addition, it requires the use of an infrared spectrophotometer.
Name: Speed of Cure Versus Standard.
Property Measured: Reactivity.
Method: See Appendix 1.
Necessary Equipment: Curing apparatus.
Name: Infrared Spectroscopy.
Property Measured: Reactivity.
Method: See Appendix 2.
Necessary Equipment: Curing apparatus and infrared
spectrophotometer.
REFRACTIVE INDEX
The refractive index of a substance is the ratio of the
speed of light through a vacuum to the speed of light through
a sample. The refractive index of a substance is very sensitive
to compositional variations. Therefore, the method is
useful to check the uniformity of batches or the presence of
contamination.
Name: Refractive Index.
Method: ASTM D1218.
Comments: Liquids must be light colored. Test liquid must be
2

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free of bubbles. Temperature affects the results.
Necessary Equipment: Thermometer and refractometer such as
Bausch & Lomb’s “Precision Type Range 1.33 to 1.64 for the
Sodium D line.”
RHEOLOGY
Rheology deals with the flow or deformation of the
coating. Depending upon the application of the coating, the
rheology of the coating is specified. Since rheology is a
measurement of the movement of the fluid, changes in this
property affect the properties of leveling, flowout, sag
resistance, etc.
The major aspect of rheology is viscosity, which is the
internal friction of a fluid. Viscosity differences may be indicative
of formulational differences, which can manifest
themselves in other properties such as toughness, flexibility,
abrasion resistance, etc. (2)
A cup type of viscometer measures the time it takes for
the coating to empty through an orifice in the bottom of the
cup. For this type of viscometer the coating needs to be
Newtonian or near-Newtonian (viscosity is not dependent
upon shearing forces) or else it is difficult to judge the break
in the flow of the coating stream. The closer the orifice is
to a capillary, the more accurate the test. The cup methods
are easy to use and rapid, but are limited in viscosity range
to relatively fluid materials. They are not precise, but are
practical and cleanup is rapid. Cup type viscometers are frequently
used during application to assure the viscosity of the
coating is within the viscosity range of the equipment and
the process.
Coatings which are more viscous are measured either
on a Laray viscometer or on an inkometer. The latter simulates
the operation of an offset press. The former measures
the resistance of a rod coated with a test material to falling
through a narrow collar.
The most accurate method is the Rotational Viscometer
Method. The procedure can measure coatings over a wide
range of viscosities. It is slower than cup methods, but is still
practical. Modifications to the procedures permits the
measurement of thixotropy. Thixotropic coatings are materials
whose viscosity decreases upon application of shear.
Name: Viscosity by Zahn Cup.
Property Measured: Rheology.
Method: ASTM D1084, ASTM D4212.
Comments: Must be measured at constant temperature. If
viscosity is shear dependent use ASTM D2556.
Necessary Equipment: Zahn viscosity cup set, stopwatch or
other timing device, and thermometer.
Name: Viscosity by Ford Cup.
Property Measured: Rheology.
Method: ASTM D1200.
Comments: Must be measured at constant temperature. If
material is thixotropic use ASTM D2196.
Necessary Equipment: Ford viscosity cup set, stopwatch or
other timing device, and thermometer.
Name: Yield Value by Falling Rod Viscometer (Laray).
Property Measured; Rheology.
Method: See Appendix 3.
4
Necessary Equipment: Laray Viscometer with photoelectric
timer, constant temperature bath, thermometer, programmable
calculator or computer or calibrated graph paper, and plastic
spatula.
Name: Tack by Inkometer.
Property Measured: Rheology.
Method: ASTM D4361.
Comments: Needs to be measured at constant temperature and
constant rpm.
Necessary Equipment: Inkometer and calibrated ink pipet.
Name: Viscosity by Rotational Viscometer.
Property Measured: Rheology.
Method: ASTM D1084, Method B.
Comments: Must be measured at constant temperature,
normally 25 C. For non-Newtonian materials, viscosity may
vary with speed and spindle, therefore these items should also
be reported.
Necessary Equipment: Rotational viscometer, such as
Brookfield model LV or RV, and thermometer.
Name: Thixotropy by Viscometer.
Property Measured: Rheology.
Method: ASTM D2196.
Comments: Must be measured at constant temperature.
Necessary Equipment: Rotational viscometer with at least 4
speeds, thermometer, and high speed mixer.
SHELF-LIFE STABILITY
Measurement of this property is indicative of the storage
stability of the coating prior to use. The test does not tell how
long the coating is stable. It gives stability in contrast to a
reference material.
Name: Oven Aging.
Property Measured: Shelf-Life Stability.
Method: ASTM D4144.
Comments: Container composition may vary results. Control
should be run simultaneously. Since oxygen inhibits the
polymerization reaction, the proportion of headspace to coating
will affect the results. Can also measure the change in viscosity
with heating instead of gellation point.
Necessary Equipment: Container, thermometer, and constant
temperature oven.
SURFACE TENSION
Surface tension is indicative of such properties as wettability,
purity, crawling, cratering, foaming, and adhesion.
Coatings tend to flow from areas of low surface tension to
areas of high surface tension. Wetting is the unforced instantaneous
spreading of a liquid to cover a solid substrate. In
order to wet a substrate, the surface tension of the liquid must
be lower than the surface free energy of the substrate. Crawling
occurs if a coating of high surface tension is applied to
a substrate with lower surface free energy. When this happens
the coating puddles. Failure to properly wet the substrate
reduces the adhesion of the coating. Cratering is often caused
by a contaminant of low surface tension on the substrate’s
surface or in the coating. The coating tends to flow away from
the contaminant. In order to achieve good leveling, materials
of low surface tension are often added to the coating. These
materials, however, often cause foaming.

.
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Name: Surface Tension.
Method: ASTM D1331, Method A.
Comments: Should be reported at constant temperature. All
equipment must be clean.
Necessary Equipment: Tensiometer and container, at least 6 cm
in diameter.
CHEMICAL FUNCTIONALITY
Analysis of the coating for chemical functionality is
useful in evaluating it for performance in a particular end use.
For example, the acid number is indicative of residual acid
which may be present. The acid is often acrylic acid. Residual
acid can be corrosive to some substrates.
In a similar manner, the alkalinity number is indicative
of residual base which may be present and be detrimental
to certain end uses. The hydroxyl number is the number of
-OH groups present. These groups are polar and are also
potentially reactive sites.
The unsaturation aspect of the test determines the number
of double bonds in the coating. These are also potentially
reactive sites. The determination of water is valuable since
if it is present as a contaminant, it may have a significant
effect upon properties such as viscosity, cure speed, tensile
strength, percent elongation, modulus, refractive index, surface
tension, hardness, and wear resistance among others.
The disadvantages of these tests are that they do require some
knowledge of chemistry and are time consuming.
Name: Chemical Functionality.
Properties Measured: Acid number, alkalinity number, hydroxyl
number, unsaturation, and water content.
Method: ASTM D2849.
Comments: Care must be taken with chemicals involved.
Necessary Equipment: Erlenmeyer flask, buret, ethanol,
hydrochloric acid, phenolphthalein indicator, potassium
hydroxide, sodium hydroxide, benzene, pipet, balance, mercuric
acetate, methanol, sodium bromide, beaker, Karl Fischer
reagent, and Karl Fischer titrator.
CURED FILM PROPERTIES
WEAR RESISTANCE (ABRASION)
Abrasion resistance is related to the properties of hardness,
tensile strength, elastic modulus, and toughness. Abrasion
or wear resistance is the ability of a coating in bulk to
withstand mechanical forces which tend to progressively
remove the coating. Mar resistance is the ability of the surface
of the coating to withstand these forces. The greater the
elasticity of the coating, the better able it is to deform and
therfore the more abrasion resistant it tends to be. As tensile
strength increases, the coating exhibits greater wear resistance.
(3)
The Taber Abrasion Test is more destructive than the
Sutherland Rub Test. Addition of slip agents can improve the
results of the Sutherland Rub Test, but tend to have little effect
on the results of a Taber Test. The Taber Test is difficult
to reproduce between laboratories. The Sutherland Rub Test
is designed to simulate the rubbing of materials during shipment.
Foreign materials, coating thickness, and temperature
will affect the results of both tests.
6
Name: Sutherland Rub.
Property Measured: Wear Resistance.
Method: Tappi RC- 183 (4).
Comments: Specify the weight and number of rubs used. Also
specify the surfaces to be rubbed (for example, coating to
stock).
Necessary Equipment: Rub test equipment such as that from
Sutherland Paper Co. (Kalamazoo, Mich.).
Name: Taber Abrasion.
Property Measured: Wear Resistance.
Method: ASTM D4060.
Comments: Specify wheel, weight per wheel, and number of
cycles. Reproducibility between labs is poor.
Necessary Equipment: Taber Abrasion tester.
SURFACE SLIP
Surface slip is important for shipping and handling coated
substrates. The greater the surface slip, or the lower the coefficient
of friction, the easier materials slide past each other.
This test measures the resistance to movement. As the surface
slip increases, often the surface is more resistant to marring
and abrasion. In addition to the test methods listed there
is also the Three Point Sled Method. The tests are dependent
upon complete cure of the surface of the coating.
Name: Horizontal Plane.
Property Measured: Surface Slip.
Method: ASTM D3247.
Necessary Equipment: Friction testing apparatus such as that
supplied by American Glass Research (Butler, Pa.) or Altek
Co. (Torrington, Ct.).
Name: Inclined Plane.
Property Measured: Surface Slip.
Method: ASTM D3334.
Necessary Equipment: Timer, inclined plane, and sled.
HARDNESS
One advantage of radiation curable coatings is their high
degree of hardness. The harder a coating is, the more it resists
indentation and scratching. Hardness tests are dependent upon
the coating’s thickness, substrate, and adhesion. The Durometer
Test measures the amount of penetration of a needle into
the coating. For soft coatings a Shore A durometer is used,
for harder. coatings the Shore D durometer is used. The Steel
Wool Rotary Test measures the resistance to abrasion by
rotating steel wool at a force of 12 psi.
For the ?encii Hardness Test, hardness is determined by
a set of numbered pencils. The first pencil which scratches
the surface is reported as the coating’s hardness. The test has
the advantage of being rapid. It is, however, operator dependent.
The “squareness” of the point, the applied force, and
the angle affect the results. In addition to the listed tests, there
are also the Knoop Hardness Test (ASTM D1474) and fingernail
scratching which is a subjective indicator of surface
hardness.
Name: Durometer.
Property Measured: Hardness.
Method: ASTM D2240.
Comments: Results can be temperature, thickness, and applied

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eliminate the effect of applied pressure.
Necessary Equipment: Durometer.
Name: Steel Wool Rotary Test.
Property Measured: Hardness.
Method: See Appendix 9.
Necessary Equipment: #OOOO steel wool and rotary holder for
the steel wool designed to deliver 12 psi.
Name: Pencil Hardness.
Property Measured: Hardness.
Method: ASTM D3363.
Comments: Should be tested at ambient temperature. Results
can vary with substrate composition and film thickness.
Necessary Equipment: Calibrated set of drawing leads or
equivalent set of calibrated pencils meeting the following
hardness scale:
Soft: 6B-5B-4B-3B-2B-lB-HB-F-H-2H-3H-4H-5H-6H: Hard.
GLOSS
Gloss is the property of a surface which causes it to
reflect light; high gloss is often a desirable aesthetic feature
of radiation curable coatings. A glossmeter is used to quantitatively
measure light reflected from a surface at various
angles.
Property Measured: Gloss.
Method: ASTM D523.
Comments: Gloss is affected by substrate color and texture as
well as method of application.
Necessary Equipment: Glossmeter (60 degree for mid-range
gloss, 85 degree for low gloss, and 20 degree for high gloss).
GLASS TRANSITION TEMPERATURE
Properties such as refractive index, modulus, coefficient
of thermal expansion, rupture strength, percent elongation,
and dielectric constant change significantly at the glass transition
temperature. It is, therefore, desirable to know the
temperature at which the coating changes from a soft, rubbery
state to a more brittle material. The glass transition
temperature is detected with a differential scanning
calorimeter. Although this test is very useful for the prediction
of performance, it is both time-consuming and expensive.
Name: Differential Scanning Calorimeter.
Property Measured: Glass Transition Temperature.
Method: ASTM D3248.
Comments: Sensitive to heating rate.
Necessary Equipment: Differential scanning calorimeter and
sample pans.
TENSILE PROPERTIES
Mechanical properties are important to the performance
of radiation-cured systems. A tensile (pulling) load is applied
using a tensile testing instrument to determine properties such
as modulus, elongation at break, and strength. Rupture
strength is the greatest stress a coating can withstand prior
to ripping. Modulus is a measure of the stress required to
elongate the coating a given distance. Elongation is required
if the coated substrate must be post-formed. The test is sensitive
to edge effects, so a precision cutter is recommended.
8
In addition, the tests are sensitive to both temperature and
humidity. Actual values vary with the rate at which the sample
is elongated.
Name: Modulus, Rupture Strength, % Elongation, Tensile
Strength.
Properties Measured: All of the above.
Method: ASTM D882.
Comments: Can be used to test free film or coated surface.
ASTM D638 should be used if film thickness is greater than 1
mm. Values may vary with the degree of cure and sample
conditioning.
Necessary Equipment: Tensile tester, such as a Instron.
FLEXIBILITY
The flexibility of a coating is its ability to be twisted and
bent. Usually, the more flexible a film is, the better able it
is to resist cracking. Also, thicker films are usually less flexible.
Flexibility is affected by not only the film’s ability to
move but also by adhesion. As the temperature increases,
most films become more flexible. If the film absorbs humidity,
the water can act as a plasticizer. The rate at which the
film is tested affects the results. The faster the test is run,
the less flexible it appears to be. In addition to the test listed
below, the Cylindrical Mandrel Test, the T-Bend Test, and
the Impact Test, which measures instantaneous flexibility, also
are used to measure this property.
Name: Conical Mandrel Bend.
Property Measured: Flexibility.
Method: ASTM D522.
Comments: Flexibility will be affected by both the substrate and
applied film thickness, therefore, these factors should be kept
constant when doing comparisons.
Necessary Equipment: Conical Mandrel Flexibility tester.
CHEMICAL RESISTANCE
Chemical attack of a coating by solvents, water, acid,
or base can result in loss of adhesion, loss of gloss, reduction
of tensile properties, and swelling. The Covered Spot
Test provides contact between a coating and various chemical
substances to give a qualitative measure of the relative
resistance of a coating. In the Solvent Rub Test the solvent
is rubbed with a cloth across the surface of a coating. This
test, run with methyl ethyl ketone, is often used as an indicator
of completeness of cure.
Name: Covered Spot Test.
Property Measured: Chemical Resistance.
Method: ASTM D1308.
Comments: Applied film thickness can affect results. To assure
uniform contact with low viscosity solvents, a 1” square of
tissue can be saturated and placed on the test surface.
Necessary Equipment: Watch glass approximately 2“ in
diameter and 1” square tissue.
Name: Solvent Rub.
Property Measured: Chemical Resistance.
Method: See Appendix 8.
Comments: Choose chemicals to which the coating will be
exposed during use.
Necessary Equipment: Cloth, pipet, distilled water, and solvent.

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BARRIER PROPERTIES
Radiation cured coatings, particularly those used in
packaging applications may be required to exclude moisture.
The barrier properties of a coating are expressed either as
water vapor transmission rate or as a moisture vapor transmission
rate, which are calculated from the amount of water
transmitted through an area of coating under precise
temperature, pressure, and relative humidity conditions.
Moisture can cause loss of adhesion, substrate corrosion, or
degradation of the substrate. For the tests, film preparation
is critical. A pin hole in the coating can have a large
adverse effect. The tests are very temperature and relative
humidity dependent.
Name: Moisture Vapor Permeability.
Property Measured: Moisture Barrier.
Method: ASTM D1653.
Necessary Equipment: Analytical balance, controlled
environment.
Name: Water Vapor Transmission Rate.
Property Measured: Water Barrier.
Method: ASTM E96.
Necessary Equipment: Sealable test specimen, mounting dishes,
constant temperature and humidity environment, analytical
scale.
ADHESION
Adhesion tests measure the force needed to remove a
coating from the substrate. The qualitative adhesion of a
coating to a specific substrate can be tested by observing the
amount of scored coating which is removed from the substrate
by pressure sensitive tape. Any surface preparation done to
the substrate can affect adhesion. Adhesion is improved by
good lay, good wetting, and dry substrates. Lack of through
cure of a coating will give poor results in adhesion testing.
Name: Tape Test.
Property Measured: Adhesion.
Method: ASTM D3359.
Comments: Test tape used should be specified. Test is only for
films less than 5 mils in thickness.
Necessary Equipment: Pressure sensitive tape, steel ruler, and
single-edge razor blade.
RESIDUAL UNSATURATION
The Permanganate Stain Test is a qualitative measure of
the extent of cure of a coating by observation of the intensity
of color after staining. This intensity is proportional to the
amount of residual unsaturation.
Name: Permanganate Stain Test.
Property Measured: Residual Unsaturation.
Method: See Appendix 7.
Comments: Test is qualitative only. Residence time of solution
affects the results.
Necessary Equipment: 1% potassium permanganate solution and
stopwatch.
RESIDUAL MONOMER
Radiation curing normally involves “ 100% solids”
systems in which ultraviolet cure gives optimum properties.
If cure is partial the film can slowly continue curing which
10
changes the properties. In addition, unreacted monomer can
act as a plasticizer. As it is removed, the film properties can
change. The Extractables by Gas Chromatography Test detects
uncured monomers which have been extracted from the
coating with solvent. The quantitative gravimetric method
provides a determination of the extend of cure by measuring
the weight of uncured monomer.
Name: Extractables by Gas Chromatographic Analysis.
Property Measured: Residual Monomer.
Method: See Appendix 6.
Necessary Equipment: 25 mi screw cap vial, sample shaker,
gas chromatograph, standard solutions, tetrahydrofuran, and
syringe.
Name: Extractables by Gravimetric Determination.
Property Measured: Residual Monomers.
Method: See Appendix 5.
Necessary Equipment: 25 ml screw cap vial, sample shaker,
crystallizing dish, analytical balance, tetrahydrofuran, and
cotton gloves.
VOLATILES
Volatile materials in radiation curable formulations may
contribute odor and undesirable emissions, and may decrease
performance properties. This baking method quantitatively
measures volatiles as a loss of sample weight after baking.
Name: Volatiles by Baking.
Method: ASTM D1259, Appendix 4.
Comments: Can be used on cured film or on uncured coating.
Necessary Equipment: Petri dish or aluminum pans, constant
temperature forced air oven, analytical balance, stopwatch,
syringe, and cotton gloves.
EXPOSURE TESTING
For coatings used in outdoor applications it is desirable
to simulate the effect of exterior exposure upon the coating.
Artificial testing done with UV accelerated weatherometers
and fadeometers is done considerably faster than exterior exposure
testing. The artificial testing, however, may not accurately
simulate the effects of weathering.
Name: Exterior Exposure Test.
Property Measured: Weathering.
Method: ASTM D1006.
Comments: Test needs to be run for an extended period
of time.
Necessary Equipmerit: Testing site and method to hang the
specimens.
Name: Xenon-arc Lamp.
Property Measured: Weathering.
Method: ASTM G26.
Comments: Method is for light exposure and water spray.
Necessary Equipment: Xenon-arc and water spray test
equipment.
Name: Fluorescent U.V. Condensation.
Property Measured: Weathering.
Method: ASTM G53.
Comments: Correlation with weathering tests done outside may
be difficult.
Necessary Equipment: Test equipment with fluorescent U.V.
light, temperature probe, timer, and water spray.

.
CONCLUSION
REFERENCES
The purpose of various tests for radiation curable clear
topcoats was presented including the advantages and disadvantages
of each test. In addition, the inter-relationships of
various properties were examined. Where appropriate, comments
to aid in testing were added.
The test methods and equipment cited in this book are
intended for reference only. The committee does not endorse
any method or equipment.
(1) American Society of Testing Materials. All ASTM
methods cited are available from this society: 1916 Race
St., Philadelphia, Pa. 19103.
(2) Kallendorf, Camille J. and Singleton, Mitchell, Correlation
Between the Properties of Wet Ultraviolet Coatings
and Cured Films, Conference Proceedings, Radcure ’84,
Sept. 1984.
(3) Sward, G.G., Paint Testing Manual, ASTM, 1972, pp.
301-302.
(4) Technical Association of the Pulp and Paper Industry: 360
Lexington Ave. New York.
This chapter is reprinted courtesy of the authors of the book and
the Society of Manufacturing Engineers. Copyright 1987, from the
Radcure ’86 Conference Proceedings.
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.
CHAPTER 2
INKS
13

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INTRODUCTION
The test methods cited in the coatings chapter are applicable
to radiation cured inks and are therefore not cited
in this section. The methods listed here are used for conventional
inks but are applicable to radiation cure. They deal with
how pigment can affect the formulation in the areas of grind,
tack, hardness and color.
GRIND
Fineness of grind is indicative of how well dispersed a
pigment is in the oligomer-monomer. Failure to obtain a good
grind will affect cylinder wear, color strength, water uptake
and the tack of an ink. The printed surface can have piling,
lower gloss, areas of pickoff, streaking, and reduced rub or
abrasion resistance. The grind tests will also indicate partial
gellation of a radiation-curable ink.
Name: Npiri Grind.
Property Measured: Dispersion.
Method: ASTM D1316.
Comments: Dust particles will give false readings so grind
gauge and scraper must be well cleaned. Ink should be sampled
from the bulk, not the surface.
Necessary Equipment: Npiri grind gauge.
Name: Hegman Grind.
Property Measured: Dispersion.
Method: ASTM D1210.
Comments: Same as above.
Necessary Equipment: Hegman grind gauge.
TACK
Tack is the measurement of the “stickiness” of a
substance. It is desirable to have the tack as high as possible
to produce the sharpest print; however, too high a tack will
cause picking of the substrate. Improper tack will cause poor
transfer of the ink on the rolls and subsequently to the
substrate, as well as misting and slinging problems. Smearing
can also be caused by having improper tack.
The most common method to measure tack is the inkometer
test. The inkometer measures the force required to
cause inked rollers to rotate in contact with each other.
Temperature must remain constant, since higher temperatures
tend to break down an ink and lower the reading. The amount
of ink applied to the rollers, the speed of the rollers, the time
the ink has been on the roiiers and the pressure applied to
the rollers all affect the reading. The finger tapout test is very
quick and inexpensive, but also is highly subjective.
Name: Tack by Inkometer.
Property Measured: Stickiness of an Ink.
Method: See Appendix 10.
Comments: Amount of ink, temperature, roller pressure, time,
and roller speed affect the reading.
Necessary Equipment: Inkometer, ink pipet, spatula and
stopwatch.
Name: Finger Tapout Test.
Property Measured: Stickiness of Ink.
Method: See Appendix 11.
Comments: Highly subjective.
HARDNESS
The methods cited in the coatings chapter are also applicable
to inks and are commonly used in the industry. The
addition of pigment to make an ink will tend to soften the
film. The softer the film, the easier it will abrade.
Name: Rocker Hardness.
Property Measured: Hardness.
Method: ASTM D2134.
Comments: Incompletely cured ink will allow monomers and or
oligomers to migrate to the surface and slow the rocker which
will produce inaccurate results. Plasticizers which could
migrate to the surface also affect results.
Necessary Equipment: Sward Hardness Rocker, Model C.
COLOR AND STRENGTH
As with conventional inks, color and strength are critical
to the print. The test cited below is visual and therefore subjective,
yet it is reproducible with experience in performing
the test. The test consists of drawing down the test ink versus
a standard and comparing the color. Strength is measured
by diluting both inks with the same amount of white tinting
ink and comparing drawdowns. For white inks, black ink may
be used for the test. Colormeters are available to measure
the color of a print.
Name: Strength and Color of Ink.
Properties Measured: Strength, Color.
Method: ASTM D387.
Comments: Test is visual and therefore subjective. Test is not
applicable to white ink; however, ASTM D332 is the method
for white.
Necessary Equipment: Drawdown bar, anilox roller, quick peek,
and Little Joe press or appropriate equipment to make print.
15

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CHAPTER 3
ADHESIVES
17

INTRODUCTION
Radiation-curable adhesives are formulated to bond a
wide variety of substrates together. If the adhesive is being
cured between the two substrates, care must be taken to assure
adequate ultraviolet or electron-beam energy reaches the
adhesive through the substrate. As with radiation-curable inks
and coatings, the method of application and extent of cure
affect the results and performance of the cured adhesive.
LIQUID ADHESIVE PROPERTIES
RHEOLOGY
Rheology is the study of the deformation or flow of a
material when stress is applied. In a perfectly viscous liquid
the observed stress is dependent upon only the rate of deformation.
The material has no memory of previously applied
stresses. The work used to produce the stress is instantaneously
dissipated. The stress at a given instant is dependent only
on how rapidly it is deformed at that moment. Such materials
are called Newtonian or non-thixotropic. A non-Newtonian
or thixotropic material changes viscosity as the stress is
changed. The method of application determines the necessary
viscosity for the adhesive.
Name: Viscosity of Adhesive.
Property Measured: Viscosity.
Method: ASTM D1084-Method B.
Comments: Method should be used for non-thixotropic
adhesives (Newtonian). This method applies to adhesives
between 50 and 200,000 CP in viscosity. Viscosity is highly
temperature dependent so temperature must be held constant.
Viscosity also varies with the speed of rotation and the spindle
used. The viscometer is less accurate at the high and low
portion of the scale (less than 20 and greater than 80). Damage
such as scratches to the spindle or cup noticeably alters the
results, as does a bent spindle connector. Amount of sample
used will change the results and therefore the quantity must be
specified.
Necessary Equipment: Rotational viscometer, such as
Brookfield LV or RV models, and thermometer or temperature
controller.
Name: Apparent Viscosity of Adhesives Having Shear-Rate-
Dependent Flow Properties.
Property Measured: Viscosity.
Method: ASTM D2556-69.
Comments: Method should be used for thixotropic adhesives
(non-Newtonian). All other comments for D-1084, Method B
apply.
Necessary Equipment: Rotational viscometer, such as
Brookfield LV or RV models, and thermometer or temperature
controller.
CURED ADHESIVE PROPERTIES
BULK MATERIALS
PROPERTIES-PHYSICAL
18
TENSILE TESTS
Adhesives must be able to withstand the stresses to which
the substrates will be exposed without loss of tensile
properties. In the test, a tensile or pulling load is applied to
the sample and the properties of modulus, elongation at break,
rupture strength, and tensile strength are determined. Tensile
strength is the maximum stress (load) the sample withstands
without breaking. Rupture strength is the stress which occurs
at break. Both tensile strength and rupture strength are
reported in psi. Percent elongation is the elongation of the
sample at break expressed as a percentage of the original
gauge length. Modulus is the ratio of the stress to the
corresponding strain (amount which the sample is stressed).
It is also called the elastic modulus or Young’s modulus. The
higher the modulus value, the harder it is to stretch the
sample.
Name: Tensile Properties of Plastics.
Properties Measured: Tensile strength, rupture strength,
% elongation, modulus.
Method: ASTM D638.
Comments: Results are dependent upon the degree of cure, the
thickness of the sample, and the rate of the crosshead.
Temperature and humidity change the results, therefore
preconditioning of the sample is recommended. Nicks in the
edge of the sample create stresses which alter the results.
Necessary Equipment: Sample cutter, micrometer, and tensile
testing machine with constant rate of crosshead movement.
VOLATILES
Volatiles from an adhesive can migrate to an interface
of the adhesive and substrate causing loss of bond strength.
Volatiles can also destroy the properties of nearby components
and are therefore carefully monitored in the aerospace and
electronics industries. For environmental reasons, VOCs
should be minimized. For non-electronic applications, the
method can be modified using a conventional oven.
Name: Total Mass Loss and Collected Volatile Condensable
Materials From Outgassing in a Vacuum Environment.
Property Measured: Volatiles.
Method: ASTM E595.
Necessary Equipment: Vacuum oven and analytical balance.
BARRIER PROPERTIES
In packaging applications, it is desirable for the adhesive
to act either as a moisture barrier or water barrier in addition
to bonding the two substrates. With both of the following
tests, application of the adhesive is critical since a pinhole
can indicate failure of the adhesive to act as a barrier. Both
tests are sensitive to temperature and humidity.
Name: Moisture Vapor Permeability.
Property Measured: Moisture Barrier.
Method: ASTM D1653.
Necessary Equipment: Analytical balance and controlled
environment.
Name: Water Vapor Transmission Rate.
Property Measured: Water barrier.
Method: ASTM E96.
Necessary Equipment: Sealable test specimen mounting dishes,

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constant temperature and humidity environment, and analytical
scale.
HARDNESS
For bonding in certain applications it is desirable to match
the hardness of the adhesive to that of the substrate. The
harder the adhesive, the more it resists indentation under applied
stress. This affects the ability of the adhesive to withstand
stress prior to it moving and losing bond strength.
Name: Rubber Property-Durometer Hardness.
Property Measured: Hardness.
Method: ASTM D2240.
Comments: Results are dependent upon the degree of cure,
temperature, humidity and applied pressure. Use of a weight to
apply the pressure can eliminate the effect of pressure. Use a
Shore A durometer for soft adhesives and a Shore D durometer
for harder adhesives.
Necessary Equipment: Durometer.
REFRACTIVE INDEX
Refractive index is the ratio of the speed of light in a
vacuum to the speed of light in a sample. It measures a fundamental
property of a substance and is therefore useful for
the control of purity or composition. For optical parts, the
refractive index of the adhesive is critical. For bonding of
transparent substrates, if the refractive index is not carefully
selected, distortion will occur. The method referenced is for
cured adhesives. If the refractive index of uncured adhesives
is desired use the method cited in the coatings section.
Name: Index of Refraction of Transparent Organic Plastics.
Property Measured: Refractive Index.
Method: ASTM D542.
Comments: Temperature affects results, so it should be reported
with the refractive index.
Necessary Equipment: Abbe refractometer and thermometer.
FLEXIBILITY
If the bonded substrates in the end use must withstand
flexing, the adhesive must be able to bend with the substrates.
Name: Mandrel Bend.
Propem Measured: Flexibility.
Method: ASTM D3111.
Comments: This test is useful for comparing radiation cured
adhesive specimens for flexibility. Flexibility will be affected by
the substrates selected and the thickness of the adhesive
applied. Therefore, these factors should be kept constant during
comparisons.
TACK
Tack is the stickiness of a substance. In radiation curing
it is often desirable to bond only onesubstrateduring exposure
to UV or EB radiation and to have the adhesive remain tacky
so a second substrate can be bound. Tack is measured as being
the maximum force necessary to break the bond between
the adhesive and the probe. The method is useful for both
rigid and flexible substrates.
Name: Pressure Sensitive Tack of Adhesives Using an Inverted
Probe Machine.
Property Measured: Tack.
20
Method: ASTM D2979.
Comments: Test is temperature sensitive.
Necessary Equipment: Polyken Probe Tack Tester or equivalent
equipment.
ELECTRICAL
It is important to measure the electrical properties of the
adhesive in any application where an electric field is present.
For example, if the adhesive is bonding an insulator, it is
desirable for the adhesive to also perform as an insulator.
The dielectric strength is the voltage an insulating material
can withstand prior to breakdown or penetration. The dielectric
constant indicates the ability of an insulator to store electrical
energy. The dissipation factor indicates the amount of
energy or power loss which occurs in virtually all dielectric
materials. Resistivity is the resistance to leakage either along
the surface of a material or through the body of a material.
Name: Dielectric Breakdown Voltage and Dielectric Strength of
Solid Electrical Insulating Materials at Commercial Power
Frequencies.
Property Measured: Dielectric Strength.
Method: ASTM D149.
Comments: Caution must be exercised since lethal voltages are
used and if done improperly a fire hazard exists. Dielectric
strength is influenced by temperature and moisture content so
conditioning is recommended. Sample must be solid.
Necessary Equipment: Voltage source, voltmeter, and
electrodes.
Name: A-C Loss Characteristics and Permittivity (Dielectric
Constant) of Solid Electrical Insulating Materials.
Properties Measured: Dielectric Constant, Dissipation Factor.
Method: ASTM D150.
Comments: Sheet specimens are preferred.
Necessary Equipment: Electrodes, capacitance bridge.
Name: D-C Resistance or Conductance of Insulating Materials.
Properties Measured: Surface and Volume Resistivity.
Method: ASTM D257.
THERMAL PROPERTIES
A change in the volume of an adhesive with a change
in temperature in the end use can cause stress on delicate
parts resulting in failure. For example, in fiber optics, a
change in volume of an adhesive can cause microbending
which increases the signal loss. Also, depending on the use
it can be desirable for the adhesive to conduct heat from one
component to another.
Name: Coefficient of Linear Thermal Expansion of Plastics.
Property Measured: Thermal Expansion.
Method: ASTM D696.
Comments: Method ignores the effect of moisture content,
plasticizer loss, and stress relaxation. The adhesive cannot be
distorted by application of dilatometer.
Necessary Equipment: Fused-quartz dilatometer, linear scale,
liquid temperature bath, and thermometer.
Name: Thermal Conductivity Measurements by Means of a
Twin Standard Comparative Instrument and Its Use with
Liquids.
Property Measured: Thermal Conductivity.

Method: See Appendix 1.
Necessary Equipment: Heater, two standards with known
thermal conductivity, "0" ring, and thermocouples.
STRENGTH OF BONDS
The purpose of any adhesive is to bond two substrates
together. Therefore, a critical property to be measured is the
strength of that bond. The test selected to measure this property
should be the one which best simulates the end use of
the adhesive. The suggested methods need to be modified to
radiation curing from conventional cure and to the desired
substrates. Adhesive bonds are sensitive to temperature,
humidity, degree of cure, and substrate preparation. It is
recommended that samples be preconditioned.
Shear is the stress which tends to make one part of a
body slide over the adjacent part. Creep is the strain which
develops when a constant stress is applied. Compression is
a pushing type of force. Torque is the force that tends to cause
torsion or rotation. Impact is the energy absorbed from a falling
object.
Name: Determining Strength Development of Adhesive Bonds.
Property Measured: Minimum dose for fixture.
Method: ASTM D1144.
Comments: Modify method to determine the lowest dose for
fixture, not the time for fixture. Test is often used in
metaheta1 bonds which undergo a heat cycle after radiation
curing. Method is useful for both liquid and paste adhesives.
Name: Shear Strength of Adhesive Bonds Between Rigid
Substrates by the Block Shear Method.
Property Measured: Shear Strength.
Method: ASTM D4501.
Comments: The substrates are bonded together and the
minimum force to shear them apart is measured. Test is
applicable to plasticfplastic, plastdmetal, and plasticfglass
bonds. The moduli of the substrates must be greater than the
modulus of the adhesive.
Necessary Equipment: Tensile testing equipment with shearing
fixture.
Name: Creep Properties of Adhesive in Shear by Compression
Loading.
Property Measured: Creep.
Method: ASTM D2293.
Comments: Constant compressional stress is imposed and the
strain at subsequent times is monitored. Test is applicable if the
bond will be expected to withstand constant stress.
Necessary Equipment: Compression creep test apparatus and
microeyepiece.
Name: Creep Properties of Adhesives in Shear by Tension
Loading.
Property Measured: Creep.
Method: ASTM D2294.
Commenrs: Method is similiar to above with stress being
tensile.
Necessary Equipment: Tension creep test apparatus and
microscope.
Name: Strength Properties of Adhesives in Shear by Tension
Loading.
Propem Measured: Tensile shear.
Method: ASTM D1002.
21
Comments: Method measures the comparative shear strengths
of adhesives by applying tension (load) to failure in shear area.
This test is widely used in adhesive industry.
Necessary Equipment: Tensile testing equipment.
Name: Strength Properties of Double Lap Shear Adhesive
Joints by Tension Loading.
Property Measured: Tensile Shear.
Method: ASTM D3528.
Comments: Method determines the tensile shear strengths when
tested under low peel conditions. Results vary with
configuration used, speed of test, and testing environment.
Necessary Equipment: Tensile testing equipment.
Name: Determining the Torque Strength of Ultraviolet Light
Cured GlasdMetal Adhesive Joints.
Property Measured: Torsional Shear.
Method: ASTM D3658.
Comments: Test gives comparative torque strength to failure
data. Test is not limited to gladmetal bonds. Method is
primarily used to test aluminum hexagonal blocks to glass
plate bonds.
Necessary Equipment: Test provides specifications for holder,
light bug, and UV source.
Name: Impact Strength of Adhesive Bonds.
Property Measured: Impact Shear.
Method: ASTM D950.
Comments: Method determines the comparative impact values
of adhesive bonds in shear. The impact value is the energy
absorbed by the specimen when sheared by a single blow of the
test machine hammer. Test indicates the relative toughness of
bonds. Test should be run in the mid-range of the equipment,
since accuracy is reduced at the top and bottom of the range.
Name: Tensile Strength of Adhesives by Means of Bar and Rod
Specimens.
Property Measured: Tensile Strength.
Method: ASTM D2095.
Comments: Test reports maximum load carried by specimen at
failure. Modification of test is frequently used where specimen
is bonded to 3"x3"x%" glass plate.
Necessary Equipment: Tensile testing equipment.
PEEL
Peel strength is the stripping strength. As with bond
strength, the tests are sensitive to humidity, temperature, cure,
and surface preparation and therefore preconditioning is
recommended. Selection of peel test should be determined
by the substrates involved.
Name: Peel or Stripping Strength of Adhesive Bonds.
Property Measured: Peel Strength.
Method: ASTM D903.
Comments: Gives comparative peel characteristics where one
substrate must be flexible and non-extensible. Separation angle
is 180 degrees.
Necessary Equipment: Tensile testing equipment.
Name: Relative Peel Resistance of Adhesive Bonds When
Substrates are Flexible.
Property Measured: Peel Resistance.
Method: ASTM D1876.
Comments: Test measures relative peel resistance of adhesive
bonds when substrates are flexible. Test angle is 90 degrees.

Necessary Equipment: Tensile testing equipment.
Name: Strength Properties of Adhesives in Cleavage Peel by
Tension Loading.
Property Measured: Cleavage Peel.
Method: ASTM D3807.
Comments: Test measures cleavage peel of semi-rigid
substrates. Testing angle is less than 30 degrees.
Necessary Equipment: Tension testing equipment.
ADHESIVE PROPERTIES-DURABILITY
FATIGUE LIFE
The method determines the resistance of the adhesive
to cyclic loading. Substrates must be flexible.
Name: Fatigue Properties of Adhesives in Shear by Tension
Loading.
Property Measured: Fatigue Life.
Method: ASTM D3166.
Comments: Test is sensitive to humidity, temperature, cure
dose, and surface preparation.
Necessary Equipment: Test machine capable of applying
sinusoidal cyclic axial load.
SOLVENT RESISTANCE
In the lifetime of an adhesive, it is often exposed to
various solvents which can cause loss of bond strength. The
test exposes the cured adhesive to various solvents and compares
the bond strength of exposed adhesive and a control
sample.
Name: Resistance of Adhesive Bonds to Chemical Reagents.
Property Measured: Solvent Exposure.
Method: ASTM D896.
Comments: Select bond strength test which is applicable to end
use. Modification which is frequently used is to immerse the
samples in 188 F pressurized vessels.
Necessary Equipment: Appropriate solvents, jars, and tensile
testing equipment.
EXPOSURE TESTING
For adhesives used in outdoor applications it is desirable
to determine if sunlight adversely affects the adhesive.
Artificial testing may not accurately simulate outdoor
weathering.
Name: Ultraviolet Light Aging of Adhesive Bonded Joints.
Property Measured: UV Exposure.
Method: ASTM D904.
Comments: Substrates must be translucent. Adhesive fails when
it turns yellow or milky.
Necessary Equipment: Carbon arc light source.
TEMPERATURE AND HUMIDITY TESTING
Both temperature and humidity affect the bond strength
of an adhesive. The test is designed to determine the extent
each affects the bond strength.
Name: Effect of Moisture and Temperature on Adhesive Bonds.
Method: ASTM D115 1.
Comments: Select appropriate strength test for end use.
Necessary Equipment: Conditioning cabinets and tensile testing
equipment.
22

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CHAPTER 4
TROUBLESHOOTING - WHAT IF?
25

BEFORE PROCESSING
1. What if the batch is cloudy?
a. Stir the material.
b. Make sure the material is at the recommended
temperature.
c. Excess humidity or moisture could be present.
d. Check the data sheet to determine if material should
be cloudy.
e. Consult your supplier.
2. What if the batch is clear but develops haze or cloudiness
with time?
a. Check to determine if anything has changed in the
storage facility.
b. Check to be sure container is properly sealed.
C. Check other containers to determine if they have the
same problem.
d. Check the date of expiration.
e. A radiation source may be affecting your bulk
material. Check cover, room lighting, and stray radiation
from equipment.
f. Check for contamination from lines as well as storage
container.
g. Make sure material is at the recommended temperature.
h. Excess humidity or moisture may be present.
i. Check the data sheet to determine if this is normal.
j. Consult the supplier.
3. What if the viscosity is too high?
a. Run the shelf-life stability test.
b. Temperature may be too low.
c. Run the refractive index test as a check for contamination.
d. Radiation source may be raising the viscosity. Check
cover, room lighting and stray radiation from
equipment.
e. Run density test to determine consistency in concentration
of components.
f. If possible, dilute product to reduce the viscosity.
g. Raising the temperature will lower the viscosity, but
caution is needed since excessive temperature will cure
the material.
h. Run appropriate rheology test to determine how much
the viscosity is out-of-spec.
i. Mix well and remeasure viscosity.
j. Prior to use in production, test the material on the
substrate.
k. Consult the supplier.
4. What if the viscosity is too low?
a. Temperature may be too high.
b. Run the refractive index test as a check for contamination.
Water and other solvents may lower the viscosity.
c. Run density test to determine the consistency in concentration
of components. Water and solvents will
change the density.
d. Mix well and re-measure the viscosity.
26
e. Prior to use in production, test on substrate.
f. Run appropriate rheology test to determine how the
material is out-of-spec.
g. Consult the supplier.
5. What if the color of the batch is different from standard?
a. Stir the material.
b. Make sure the material is at the recommended temperature.
c. Check for accidental exposure to heat and light.
d. Prior to use in production, test on substrate.
e. Determine if color difference is noticeable in cured
product.
f. Run appropriate color test to determine how much the
color is out-of-spec.
g. Consult the supplier.
6. What if the smell is different from standard?
a. Smell can be indicative of a change in composition.
Run density test to determine consistency in concentration
of components. Different solvents can change
odor.
b. Run refractive index test as check for contamination.
c. Check for sources of contamination.
d. If possible, have the material analyzed.
e. Check all other important properties to see if performance
is changed.
f. Consult the supplier.
7. What if the supplied material is solid?
a. Slowly bring the material to recommended temperature.
b. Check for heat and light sources in storage area.
c. Check the shelf-life with appropriate test.
d. Consult the data sheet to determine if this is normal.
If so follow instructions to re-liquify.
e. Consult the supplier.
8. What if there are suspended particulates and/or a
sediment?
a. Stir well and bring to recommended temperature.
b. Filtration may be useful, but check performance of
material prior to use in production.
c. Check the shelf-life with appropriate test.
d. Consult the supplier.
9. What if the material when applied to the substrate exhibits
surface defects such as pinholes, craters, etc.?
a. Stir well and make sure bulk material and substrate
are at the recommended temperature.
b. Check the preparation of the substrate.
c. Make sure the application equipment is at the proper
temperature.
d. Measure the viscosity by the appropriate method. If
incorrect, refer to questions 3 and 4.
e. Run refractive index test as a check for contamination.
Small variations in silicone concentration greatly
affect the lay.
f. Heat coating, substrate and/or coated substrate to
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entrapment.
g. Run surface tension test. Improper surface tension will
cause the material to not wet the substrate.
h. If material is ink, check the grind with the appropriate
test.
10. What if material foams?
a. Stir gently and bring to recommended temperature.
Excessive stirring may create foam.
b. Run appropriate viscosity test. If incorrect, refer to
questions 3 and 4.
c. Run refractive index test as a check for contamination.
d. Run density test as a check for compositional changes
or contamination.
e. Heat coating to facilitate bubble release in the
reservoir.
f. Prevent any free fall of material which can cause
bubbles.,
g. Heat coated substrate to accelerate bubble release from
surface of coated substrate.
h. Consult the supplier.
11. What if the material is acceptable at first but upon reuse
it cannot be dispensed?
a. Check to be sure material was stored in light proof
container or if it was exposed to UV light.
b. Check for contamination from cured material.
c. Consult the supplier.
DURING PROCESSING
1. What if the material smokes while being cured?
a. Check the line speed.
b. Check the thickness of the material. If it is too thick,
heat from the lamps may be causing degradation.
c. Check the distance of coated substrate from the radiation
source. Heat from the bulbs may be causing
degradation.
d. Radiation source may be too intense for particular composition
or the substrate causing volatilization.
e. If any of the above are faulty, consult the equipment
supplier. If not, consult the materials supplier.
2. What if the coated “cured” substrate “hangs up” on the
processing line?
a. Run the appropriate reactivity test to verify cure.
b. Run appropriate surface slip test and compare the
results to the standard.
c. Check your conveyor unit.
d. Such a situation can cause aBre. Immediately remove
W source from the substrate either through automatic
interlock system or manually shut off the lamps.
e. Consult the suppliers.
3. What if there is a noticeable different odor upon cure?
a. Although cured UV or EB coatings often possess some
odor, it is normally much less than that of the uncured
coating. Often such differences in odor upon curing
emanate from the substrate itself, printing inks, etc.
Should the odor be traced to the cured coating, there
are additives which the coating supplier can incorporate
to “mask” (not eliminate) the odor in favor of
one which is less offensive.
b. Run the appropriate residual monomer test. Uncured
monomer could cause the odor.
4. What if after exposure to radiation there is no apparent
change in the material, Le., it’s wet?
a. Ensure that cure unit is properly operating.
b. Mix coating thoroughly prior to use.
c. Determine recommended cure speed from product
data sheetskoatings supplier.
d. Run the appropriate reactivity test.
e. Consult the supplier of the material.
5. What if the material is hazy after exosure to radiation?
a. Determine if “haze” is due to the surface deposition
of some kind or whether it is present within the cured
coating itself (can “haze” be wiped off or not?).
b. Check with product technical literaturehpplier to
determine if this occurrence is to be expected.
c. Consult the supplier.
6. What if the material develops blush after exposure to
radiation?
a. This occurrence is most likely due to a non-reactive
additive migrating to the surface of the cured coating
and is likely to worsen with time. Coating reformulation
is required.
7. What if the material is tacky?
a. Consult product technical literaturehpplier to determine
recommended cure speed for the product.
b. Ensure the curing unit is operating properly.
c. Mix coating thoroughly prior to use.
d. Did the material become contaminated? Water and
other contaminates can slow the cure.
e. Run the appropriate reactivity test.
f. Run the glass transition temperature test. Coatings
above their glass transition temperature will be soft
and rubbery; below their glass transition temperature
they will be hard and brittle.
g. Consult the product technical literature/supplier to
determine if the cured surface is expected to be tacky
$.e., very soft).
AFTER EXPOSURE TO RADIATION
1. What if the gloss is too low?
a. Consult product technical literaturehpplier for the
gloss range that can be expected at a given film thickness
and cure conditions.
b. Run the appropriate gloss test.
c. Consult coating supplier regarding adjustments that
may be made to cure conditions and/or coating to alter
gloss to the desired level.
28

2. What if the gloss is too high? c. Determine if smoothing bar can be employed after
a. Consult product technical literaturehpplier for gloss
coating but before curing.
range that can be expected at given film thickness and d. Contact the supplier.
cure conditions.
7. What if there are pinholes, craters or fisheyes?
b. Consult coating supplier regarding adjustments that
a. Ensure material was properly mixed prior to use.
may be made to cure conditions and/or coating to alter
b. Heat substrate and/or coating to promote flow. Conthe
gloss to the desired level.
tact supplier for heating recommendation.
c. Ensure the coating is thoroughly mixed prior to use.
c. Determine if smoothing bar can be employed after
d. Depending upon the mechanism of gloss reduction
coating but before curing.
which the product employs, heating to 100’-140’ F
d. Run the appropriate rheology test.
(38’-59’ C) may enhance the gloss reduction.
e. Run the surface tension test. Changes in surface tene.
Run the appropriate gloss test.
sion of either substrate or applied material can result
f. Consult the supplier.
3. What if the material is tacky?
a. Consult the product technical literature/supplier to determine
the recommended cure speed for the product.
b. Ensure that the curing unit is operating properly.
c. Mix the coating thoroughly prior to use.
d. Consult product technical literaturehpplier to determine
if the cured surface is expected to be tacky (Le.,
very soft).
e. Run the appropriate reactivity test to determine the
rate of cure.
f. Run the glass transition temperature test. Materials
above the glass transition temperature will be soft and
rubbery, below the glass transition temperature they
will be hard and brittle.
g. Run the residual unsaturation test.
4. What if the material does not adhere as the standard does?
a. Ensure that the material is properly mixed prior to use.
b. Ensure that the material is applied at the same film
thickness and cured under the same conditions as the
standard.
c. Contact coating supplier and substrate supplier regarding
methods to improve adhesion.
d. Run the surface tension test using a standard.
e. If the material is an adhesive, run the appropriate tack,
strength of bond, peel, and temperature and humidity
tests.
5. What if the color is different from the standard?
a. Ensure the material is applied at the same film thickness
and cured under the same conditions as the standard.
b. Compare suspect material and standard “side by side”
to eliminate application and curing variables.
c. Run the appropriate color test to determine how much
the color is out-of-spec.
d. Over-curing the film can cause it to darken.
e. Check the expiration date. Old material can darken.
f. Check for exposure to heat.
g. If the material is an ink, check the tack.
h. Consult the supplier.
6. What if there is orange peel or wrinkling?
a. Ensure material was properly mixed prior to use.
b. Heat substrate and/or coating to promote flow. Contact
supplier for heating recommendation.
29
in surface deformations.
f. If the material is an ink, check the grind.
g. Contact the supplier.
8. What if the material has sagged?
a. Refer to the technical literature/supplier to determine
if the viscosity/rheology of the material is suitable for
application without sagging. If needed, run the appropriate
viscosity or rheology test.
b. Contact the supplier.
9. What if the abrasion is not within the specification range?
a. Run the appropriate abrasion test.
b. Ensure the material was thoroughly mixed prior to
application.
c. Check for particulates which could abrade.
d. Ensure the material was applied and cured as recommended
by the supplier.
e. Contact the supplier.
10. What if the mar resistance is not within the specification
range?
a. Perform the appropriate test for mar resistance using
a standard.
b. Ensure the material is thoroughly mixed prior to
application.
c. Ensure that the material was applied and cured under
the recommended conditions.
d. Contact the supplier.
11. What if the wear resistance is not within the specification
range?
a. Perform the appropriate test for wear resistance using
a standard.
b. Ensure the material is thoroughly mixed prior to
application.
c. Ensure that the material was applied and cured under
the recommended conditions.
d. Contact the supplier.
12. What if the slip is not within the specification range?
a. Perform the appropriate test for slip (COF) using a
standard.
b. Ensure the material is thoroughly mixed prior to
application.
c. Ensure that the material was applied and cured under
the recommended conditions.

13. What if the hardness is not within the specification range?
a. Perform the appropriate test for hardness using a
standard.
b. Ensure the material is thoroughly mixed prior to
application.
c. Ensure that the material was applied and cured under
the recommended conditions.
d. Contact the supplier.
14.
15. What if the tensile properties are not within the specification
range?
Perform the appropriate test for tensile properties using
a standard.
Ensure the material is thoroughly mixed prior to
application.
Ensure that the material was applied and cured under
the recommended conditions.
Contact the supplier.
16.
17.
d. Contact the supplier.
What if the chemical resistance is not within the specification
range?
a. Perform the appropriate test for chemical resistance
using a standard.
b. Ensure the material is thoroughly mixed prior to
application,
c. Ensure that the material was applied and cured under
the recommended conditions.
d. Contact the supplier.
What if the flexibility is not within the specification
range?
a. Perform the appropriate test for flexibility using a
standard.
b. Ensure the material is thoroughly mixed prior to
application.
c. Ensure that the material was applied and cured under
the recommended conditions.
d. Contact the supplier.
What if the barrier properties are not within the specification
range?
a. Perform the appropriate test for barrier properties
using a standard.
b. Ensure the material is thoroughly mixed prior to
application.
c. Ensure that the material was applied and cured under
the recommended conditions.
d. Contact the supplier.
18.
19.
What if the accelerated weathering is not within the
specification range?
a. Perform the appropriate test for weathering using a
standard.
b. Ensure the material is thoroughly mixed prior to
application.
c. Ensure that the material was applied and cured under
the recommended conditions.
d. Contact the supplier.
What if the VOC level needs to be calculated?
a. The VOC of a product can be calculated having only
the weight/gallon and the weight solids of the material,
which can normally be found on the technical literature
for the product. The general formula for VOC is:
(lbs./gal.) (100-solids)
voc =
100
In instances where one is mixing various materials at
the job site and needs to determine the VOC of the
mixture, one needs to determine the VOC of each of
the individual components as described above and incorporate
these values into the following:
voc =
(VOC 1) (gal. 1) + (voc 2) (gal. 2) + . * .
gallons 1 + gallons 2
b . Run the volatiles test.
c. Contact the supplier.
20 * What if the coated substrate becomes distorted upon
curing?
Contact the supplier of the substrate to determine the
sensitivity of the material to parameters such as heat.
Contact the curing equipment supplier to determine
a means of reducing the amount of heat to which the
coated substrate is exposed. This may involve the installation
of quartz filters, a more efficient lamp cooling
mechanism, a “cooled” conveyor system, “chill”
rollers, etc.
If distortion is due to coating shrinkage upon curing,
a reduction in coating thickness should reduce the
amount of distortion.
Contact the supplier.
21. What if there is a different odor upon cure?
a. Run the residual monomer test.
b. Run the volatiles test.
c. Consult the supplier.
30

CHAPTER 5
GLOSSARY
31

ABRASION RESISTANCE
The ability of a material to withstand mechanical action such
as rubbing, scraping or erosion, that tends to progressively
remove material from the surface.
ACCELERATION
Increasing power or energy of electrons through an electrical
field (usually 50 to 350,000 volts or more) in a vacuum.
ACID NUMBER
The quantity of base, expressed in milligrams of potassium
hydroxide, that is required to neutralize the free acids present
in the sample.
ACRYLATES
Chemical materials, usually monomers and oligomers, which
contain the grouping CH, = CHC-0- .
II
ADHESION 0
The state in which two surfaces are held together by interfacial
forces which may consist of valence forces or interlocking
action, or both.
ADHESIVE
Any substance that is capable of bonding other substances
together by surface attachment.
ALKALINITY NUMBER
The quantity of base, expressed as milligrams of potassium
hydroxide, present in a sample.
ANGSTROM
A unit of linear measure commonly used in measurement of
wavelengths of frequencies of the electromagnetic spectrum
(lo-'' meter).
AROMATIC KETONE
A group of chemical materials most of which are sensitive
to light and readily form free radicals. The structure is
ArCOR (Ar). Some of these are useful photoinitiators.
BARRIER PROPERTIES
The properties of a substance which allow it to act as a barrier
especially to water vapor or moisture.
BENZOIN ETHER
A group of chemical materials most of which are sensitive
to light and readily form free radicals. Chemical structure
is ArCOCHORAr. Some of these are useful photoinitiators.
BLUSH
Precipitation of water vapors on the surface of a film.
BOND STRENGTH
The strength of the union between materials.
CATALYST
Any material which aids completion of a chemical reaction
without itself becoming part of the product.
CATIONIC (IONIC) CURE
A cationic reactive species generated from a stable molecule
by energy absorption which initiates polymerization of cationically
sensitive monomers such as epoxides.
CLEAVAGE/PEEL STRENGTH
The average load per unit width of bond line required to produce
progressive separation of two bonded, semirigid
adherends under specified conditions.
COEFFICIENT OF FRICTION
The measure of the relative difficulty with which the surface
of one material will slide over an adjacent surface of itself
or of another material.
COEFFICIENT OF THERMAL EXPANSION
The measure of the change in length of a material when subjected
to specified temperatures.
COMPRESSION
A pushing type of force.
CRATERING
The result of rapid spreading of a component or contaminant
over the surface of the applied material characterized
by scattered depressions at the film surface.
CRAWLING
The retraction of a liquid from the substrate over large
regions.
CREEP
The dimensional change of a material with time under load.
The strain which develops when a constant stress is applied.
CROSSLINKING AGENT
A reactive chemical material which will form bonds between
other molecules in a formula.
CURE
Conversion of a material from a raw state to a finished and
useful condition by chemical reaction.
DARK REACTION
Reactions which take place in closed containers of radiation
curable formulations - usually premature polymerization.
DEFOCUSED SYSTEM
A curing system in which the substrate is positioned either
closer to or farther away than the facial distance.
DEGRADATION
The chemical breakdown of a high molecular weight material.
DENSITY
The weight per unit voiume of a materiai usuaiiy expressed
in gramskc.
DIELECTRIC CONSTANT
An indication of the ability of an insulator to store electrical
energy.
DIELECTRIC STRENGTH
The voltage an insulating material can withstand prior to
breakdown or penetration.
DISSIPATION FACTOR
A measure of the amount of energy or power loss which occurs
in virtually all dielectric materials.
32

DOPED LAMPS
The specific wavelengths emitted from an ultraviolet lamp
are mainly dependent upon the fill. Using mercury as the
norm, the spectral output can be changed by the addition of
dopants such as beryllium or iron.
DOSE
Energy absorbed per unit mass usually in Megarads. One
Megarad equals 1 million rads, 10' erg& 2.30 caloriedg,
4.3 BTU'sAb., 10 wattsecond& or 4.54 kW seconds/lb.
DOSE RATE
Dose per unit time, usually Mradshecond.
DOUBLE BOND
A type of chemical bond wherein two pairs of electrons are
shared between two atoms.
ELASTICITY
Recovery, partial or complete, of original shape after deforminn
forces are removed.
-
ELECTROMAGNETIC SPECTRUM
The entire range of wavelengths or frequencies of electromagnetic
radiation extending from gamma rays to the
longest radio waves, including visible light.
ELECTRON
An electron is a negatively charged particle with a mass of
9.21 times grams.
ELECTRON BEAM
A beam of electrons displaced from a metallic filament by
a high voltage source of acceleration.
ELECTRON CURTAIN
An electron beam generated via a linear source (or cathode),
as opposed to a scanned source.
ELECTRON PENETRATION
The depth of penetration into a substrate by the accelerated
electrons. DeDth of Denetration deDends on the kinetic energy
v-
imparted to the electron by the accelerating voltage.
EPOXY GROUP
A reactive part of a chemical molecule with structure
YO\
-CH -CH-.
FISH EYES
The moving away of a coating to form a circular deformation,
usually caused by contamination or wetting difficulties.
FLAME RETARDANT
A material which when added to a formulation decreases its
flammability.
FLASH XENON (PULSED XENON)
Lamp containing xenon gas which produces UV radiation
using a special electric transformer system.
FLEXIBILITY
The ability of a material to twist and bend.
FLOW OUT
The ability of an applied material to eliminate surface markings
to produce a smooth, uniform surface on drying.
FOAMING
The dispersion of a gas in a liquid or solid.
FOCAL DISTANCE
The distance from a lamp with reflector at which the peak
energy can be obtained.
FOCUSED SOURCE
An electron beam which is generated through a simple filament
source, as opposed to a linear cathode source.
FREE RADICAL
A reactive species having an unpaired electron which initiates
a reaction with a double bond, e.g., acrylic polymerization.
It is produced from its stable paired state by energy
absomtion.
FREE RADICAL REACTION
A chemical reaction which takes place only when a free
radical or molecule which has lost one electron is generated.
Y
FU"UJTY
(WITH REFERENCE T o
The number of groups on any one molecule which can readily
react.
GELLATION POINT
The point at which a liquid forms a semi-solid system.
GLASS TRANSITION TEMPERATURE
The temperature at which a material changes from a soft,
rubbery state ta a more brittle state.
EXTRACTABLES
Any materid which can be removed from a curd film by
solvents, usually measured as a weight difference.
GLOSS
FATIGUE LIFE The property
~-
of a surface which causes it to reflect light.
The number of cycles of stress or strain (of a specified
character) that a sample can sustain before failure of a
specified nature occurs.
FILL
Ultraviolet is enegry generated when specific materials are
sufficiently excited so that the electrons in the material change
their energy level. The material used in an ultraviolet lamp
which undergoes this change is called the fill e.g. in a mercury
vapor lamp, the fill is mercury.
33
GRIND
The dispersion of particles (usually pigments) in a coating,
ink or adhesive.
HARDNESS
The property of a material which causes it to resist indentation
and scratching.
HAZE
That percentage of transmitted light which in passing through

the specimen deviates from the incident beam by forward
scattering.
HEAT CURE (THERMAL CURE)
A curing reaction which takes place when the materials are
subjected to a form of heat.
HYDROXYL NUMBER
The number of milligrams of potassium hydroxide equivalent
to the number of -OH groups present in the sample.
IMPACT
The energy absorbed by a specimen when subjected to a falling
object.
INERT ATMOSPHERE
The blanketing (usually from air) by a nonreactive gas (usually
nitrogen, sometimes a mixture of nitrogen and carbon
dioxide).
INFRARED ENERGY
Photon energy having wavelengths between 1 and 100
microns.
INFRARED REACTION
Normally a heat or thermal reaction induced by application
of infrared energy.
INSULATOR
A material that is a poor conductor of electricity.
IONIZATION REACTION
Reaction of molecules having lost or gained an electron pair.
LEVELING
The ability of a material to cover a dry surface easily and
uniformly and to hold its level without sagging or running.
LINE SPEED
The rate of travel of the substrate under the beam or curtain,
usually expressed in meters or feet per minute.
LINEAR CATHODE OR LINEAR SOURCE
See electron curtain.
MAR RESISTANCE
The ability of the surface of a material to withstand
mechanical forces.
MEGARAD OR Mrad
On Mrad equals one million rads. The megarad is the term
usually used to describe the dose given: i.e., 0.5 Mrad, 2
Mrads, etc.
MEGAVOLT OR MeV
A megavolt is one million electron volts. This is the kinetic
energy acquired by an electron accelerated across a potential
of one million volts (1,000,000 volts).
MERCURY LAMP
Lamp in which light is generated through presence of mercury
vapor. Most UV lamps are mercury vapor lamps.
MICROWAVE
Energy having wavelengths between 1 and 10 millimeters.
MISTING
Emission into the air of small amounts of material during
processing.
MODULUS
A measure of the ratio of the stress on a material versus strain.
MOISTURE VAPOR TRANSMISSION RATE
The rate at which water permeates a cured film under
specified conditions.
MONOMER
A molecule of relative low molecular weight and simple structure
capable of combining with itself or other similar
molecules through reactive sites to form a polymer.
NANOMETER
A unit of distance commonly used in measuring wavelength
in the electromagnetic spectrum - one billionth of a meter
meter).
NEWTONIAN
A liquid whose viscosity is not dependent on shearing forces.
NITROGEN BLANKETING
The practice of using nitrogen gas to exclude air from the
surface of the product to be cured during radiation processing.
OLIGOMER
A lower molecular weight resin or polymer which is used
in a radiation curable formula. Usually oligomers are liquid
or easily liquifiable.
ORANGE PEEL
A wrinkling, contoured surface usually caused by differential
curing of the surface as compared to the bulk of the
material.
OXYGEN INHIBITION
The effect of oxygen which terminates or retards the rate of
polymerization.
OZONE
A different form of oxygen that occurs when high energy electrical
discharge is present (OJ.
OZONE SAFETY
Measures taken to ensure that buildup of ozone concentration
does not occur.
PEEL STRENGTH
Stripping strength.
PERCENT ELONGATION
The increase in length produced by a tensile load, expressed
as a percentage of the gauge length.
PHOTOACTIVITY
The process of using photon energy (light) to start some type
of chemical reaction.
PHOTOINITIATOR
A molecule which when exposed to a specific wavelength of
energy forms a reactive species which starts the chain reaction
to cause polymer formation.
34

PHOTOSENSITIZER
A chemical which will transfer energy and form free radicals
by interacting with another chemical.
PHOTOPOLYMER
A composition which will either crosslink or depolymerize
on exposure to light, forming a physical differentiation between
the exposed and unexposed portion.
PICK OFF
Loss of adhesion usually discovered during a tape adhesion
test.
PIN HOLE
Surface imperfection of a material caused by the breaking
of bubbles.
PLASMA
A vapor in which there are energetic free radicals, ions or
molecules. These species are usually formed by radio frequency
discharge.
PLASTICIZER
A compound added to increase the flexibility and toughness
of the final product.
POLAR
Description of a molecule in which the positive and negative
electrical charges are permanently separated.
POLYMER
A macromolecule consisting of an indefinite number of
monomer units. The molecular weights may range from about
20,000 into the millions.
POLYMERIZATION
A chemical reaction usually carried out with a catalyst, heat,
or energy in which two or more relatively simple compounds
or molecules combine to form a macromolecule.
POST CURE
Continuation of reactions of materials in the ink or coating
after exposure to radiation has ceased.
PULSED XENON
See flash xenon.
QUALITATIVE
A description of the quality of a material.
QUANTITATIVE
A description of the amount of a material.
QUARTZ TUBE
A lamp made from a silicate material called quartz which
is fitted with electrical connections to form an irradiator. It
may be made into an infrared emitter or it may be filled with
mercury vapor to produce ultraviolet light.
RAD
The unit of dose equal to an energy absorption of 100 ergs
per gram.
RADIATION
Radiation as generally applied to coatings, inks and adhesives
35
comprises three energy groupings: high velocity electrons
(electron beam and scanning linear cathode), ultraviolet and
infrared energy.
RADIATION HAZARDS
Physiological hazards caused by high energy photons, electrons
or x-rays.
RADIO FREQUENCY
Electrical energy produced in the 10 to 10" Hz range. At
some frequencies it can be used to ionize or excite various
chemical molecules, both inorganic and organic, without
direct electrical contact.
REACTIVE DILUENT
A chemical which serves two purposes in a formulation: thinning
or viscosity reduction and providing reactivity with other
ingredients for curing or polymerization.
REFRACTIVE INDEX
Measurement of the ratio of the speed of light through a
vacuum to the speed of light through a sample.
RESIN
A polymeric material, either natural or synthetic, which is
usually considered an ingredient in formulation.
RESISTIVITY
The resistance to leakage of a material.
RHEOLOGY
Measurement of the movement of a fluid.
RUPTURE STRENGTH
The greatest stress a material can withstand prior to ripping.
SAG
The movement of the surface layer of a wet film (on a vertical
surface) downwards.
SAG RESISTANCE
The ability of the surface layer of a wet film to resist
downward motion (on a vertical surface).
SCAN
A method of controlling or focusing an electron beam; usually
done with high energy beams.
SHEAR
The stress which tends to make one part of a body slide over
the adjacent part.
SHELF LIFE
The amount of time a material may be stored under specified
conditions with no significant changes in properties.
SLINGING
Emission into the air of large quantities of material during
processing.
SOLVENT
A substance capable of dissolving another substance to form
a uniform, dispersed mixture at the molecular or ionic level.
STABILIZERS
Additives to coating, ink or adhesive formulations which help

extend shelf life and resist heat or other degradation.
SUBSTRATE
The unfinished product upon which a finishing (e.g., coating,
ink or adhesive) is placed.
SURFACE FREE ENERGY
The energy which exists at the surface/air interface of a film
as compared to the energy in the bulk of the film.
SURFACE SLIP
The ability and ease of sliding of the surface of one material
over the surface of itself or another material.
SURFACE TENSION
The attractive force exerted by the molecules below the surface
upon those at the surface/air interface.
TACK
The stickiness of a substance.
TENSILE STRENGTH
The rupture strength (stress-strain product at break) per unit
area of a material subjected to a specific dynamic load.
THIOGENE REACTION
Descriptive term for type of radiation catalyzed polymerization
in which sulfur containing unsaturated chemicals are
utilized.
THIXOTROPY
A property of a liquid whereby it’s viscosity decreases upon
application of shear and increases when the shear is
discontinued.
THROUGH CURE
The curing of the bulk of a material down to and including
the materiallsubstrate interface as opposed to a surface cure
where only the material/air interface is cured.
TORQUE
A force which tends to cause torsion or rotation.
TOUGHNESS
The stiffness, rigidity or resilience of a material.
TOXICITY
A life-threatening physiological behavior of materials.
ULTRAVIOLET LIGHT (UV)
That light emitted in the 200-400 nm wavelength range.
ULTRAVIOLET LIGHT PROCESSORS
Engineered equipment for UV curing which includes UV
lamps with conveying equipment for “in-line” operation.
ULTRAVIOLET BACK LIGHT
Ultraviolet light built to operate at low power using a low
pressure lamp.
ULTRAVIOLET WHITE LIGHT
Ultraviolet light built to operate near the visible spectrum.
This may be more nearly similar to a fluorescent lamp.
UNSATUR ATION
A double bond in a chemical molecule (usually between carbon
atoms or between carbon and another atom) which is
reactive to free radical initiation.
VISCOSITY
The internal resistance to flow exhibited by a fluid.
VOLATILES
Solid or liquid materials which pass into the vapor state at
a given temperature.
WATER VAPOR TRANSMISSION RATE
The steady water vapor flow in unit time through unit area
of a material under specified conditions.
WEAR RESISTANCE
The ability of a coating in bulk to withstand mechanical
forces.
WETTABILITY
The ability of the substrate surface to be wet by a liquid
material.
WETTING
The unforced, instantaneous spreading of a liquid to cover
a solid substrate.
WINDOW
A metallic foil in an electron beam generating unit that allows
passage of energetic electrons from the beam.
36

APPENDIXES
1-12 TEST METHODS
13 ASTM TEST METHODS
14 COMMON ABBREVIATIONS AND SYMBOLS
15 COMMON UNITS AND CONVERSION FACTORS
16 TEMPERATURE CONVERSION TABLE
17 ADVERTISER INDEX
37

APPENDIX 1: SPEED OF CURE
VERSUS STANDARD
1. On appropriate substrate apply coating to be examined
on left, and coating with known cure characteristics on
right.
2. Cure the coatings.
3. By fingernail scratch or MEK rubs, determine if trial
coating is more, less, or equally cured compared to the
standard.
4. If appropriate, repeat procedure with faster or slaver curing
standard.
APPENDIX 2: REACTIVITY BY
INFRARED SPECTROSCOPY
The test involves measurement in the reduction of the
infrared absorbtion of the characteristic bands for the double
bonds which react during polymerization. The principle
frequency examined is 810 cm-1 which is the twisting motion
of the CH2=CH- group. Other bands which result from
the double bond and can be examined in an infrared spectrum
are: 720cm- 1 (methylene rock) ,907 cm- 1 (out-of-plane
C-H bend), 1645 cm-1 (C=C stretch), and 3050 cm-1
(olefinic C-H stretch).
APPENDIX 3: YIELD VALUE BY
FALLING ROD VISCOMETER
EQUIPMENT
1. Laray viscometer with photoelectric timer.
2. Plastic ink spatula.
3. Water bath.
4. Thermistor temperature sensor.
5. TI 58-C or TI-59 programmed calculator.
METHODIPROCEDURE:
Inks should be previously conditioned at 25 C and then worked
up on the slab prior to testing. Temperature sensor should
be kept in the hole provided in the collar.
1. Place a small quantity (approx. 5g.) around the bottom
of the rod, with the rod held in the up position.
2. Estimate the weight required to cause the rod to drop in
15 sec. Place this weight on top of the rod. Remove the
support arm and allow the rod to fall. Do not record the
first drop time. The drop time should be about 15 sec.
3. Remove weight from rod, pull rod up slowly and replace
the support arm under the rod.
4. Using only a plastic spatula remove the accumulated ink
at the top of the rod and replace it on the bottom of the
rod next to the collar.
5. Add or subtract weight as needed to obtain the 15 sec.
drop time.
6. Reset timer.
7. Remove the rod support.
8. Record the drop time.
9. Repeat steps 3 through 8.
10. The procedure is to be repeated until two readings are
within .2 sec of each other.
11. Time measurement should be taken at three weight levels,
increased by 100 grams at each level.
12. Average time readings at each weight.
Procedure for TI 59 calculator attached to a PC lOOC printer:
1. Turn printer on.
2. Make sure print button is up on the printer.
3. Put programmed card through calculator. Clear calculator
each time card is put through.
4. Enter temperature in degrees Celsius.
5. Press Sto.
6. Press 2 6.
7. Press C.
8. Enter the lowest weight.
9. Press A.
10. Enter the average time in sec.
11. Press B.
12. Repeat steps 8 through 11 for the other weights and times.
13. Press D.
APPENDIX 4: VOLATILITY OF COATINGS
EQUIPMENT
1. Petri dish with cover.
2. 10 cc disposable syringe.
3. Dessicator with dessicant.
4. Conventional convection forced air oven.
5. Cotton gloves.
6. Analytical balance.
7. Stopwatch.
PROCEDURE:
1. Place petri dish in oven with cover at 82 C for 5 minutes.
2. Place the petri dish and cover in the dessicator to cool
for 5 minutes.
3. Weigh the petri dish and cover (initial weight).
4. Using a syringe, add 2 cc of the coating to the petri dish
and reweigh the petri dish, the cover, and the sample.
5. Place the sample in the 82 C oven with the lid removed
for 5 minutes.
6. Cool in the dessicator for 5 minutes.
7. Weigh the petri dish, cover, and sample (final weight).
8. Calculations:
Initial Weight - Final Weight = Weight loss of sample.
% Volatility = weight loss x 100
initial weight
Note: Cotton gloves should be worn when handling all containers
in this procedure.
38

1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
APPENDIX 5:
GRAVIMETRIC DETERMINATION
OF % EXTRACTABLES
Cut cured film into slices. This increases the surface area
and aids the extraction process.
Weigh 25 ml screw cap vial on analytical scale.
Add approximately 1.0 gram of film sample to vial.
Determine exact weight by reweighing vial plus sample
on analytical balance and calculating the weight
difference.
Add approximately 20 ml. of reagent grade tetrahydrofuran
to vial and seal.
Shake on shaker for 1 hour.
Allow vial to sit overnight.
Shake on shaker for 1 hour.
Filter the THF solution into a preweighed (via analytical
balance) crystallizing dish. Rinse with an additional 5-10
mls THE
Allow the THF to flash off. When a constant weight is
attained for the crystallizing dish calculate the extract
weight by difference. Air drying overnight is adequate.
Calculate the % extractables as follows:
% extractables = extract weight x 100
sample weight
Perform above in triplicate and report the results as an
average.
Note: All containers which are weighed in above procedure
should be handled wearing cotton gloves.
APPENDIX 6: GAS CHROMATOGRAPHIC
ANALYSIS OF EXTRACTABLES
1. Cut film into thin slices. This is to increase the surface
area and aids in the extraction process.
2. Weigh 25 ml screw cap vial on analytical balance.
3. Add approximately 1 .O gram of the film sample to vial.
4. Determine the exact weight by reweighing vial plus the
sample on analytical balance and calculating the weight
by difference.
5. Pipet 10 mls of reagent grade tetrahydrofuran into vial
and seal.
6. Shake in shaker for 1 hour.
7. Allow vial to sit overnight.
8. Shake on shaker for 1 hour.
9. Prepare standard solutions of suspect components (suggested
concentration: 20 mg of each standard in 10 mls
of THF).
10. Inject 1 ml of the sample into gas chromatograph equipped
with the appropriate column and detector.
11. Inject 1 ml of each standard into gas chromatograph.
12. Identify the extractables by comparing the peaks in
sample chromatogram to peaks in the standard chromatograms.
APPENDIX 7: PERMANGANATE
STAINING TEST
1. Prepare a 1 % solution of potassium permanganate in
deionized or distilled water.
2. Apply a sufficient quantity of the solution to the cured
film in order to cover an area approximately Yz inch
square. (The area covered is not critical, however, a large
area will allow an easier reading of stain intensity).
3. Allow the solution to remain in contact with the film for
5 minutes. Then rinse with water.
4. In the area where the solution was in contact with the
coating, a brown stain will be apparent. The intensity
of the stain will be proportional to the residual unsaturation
in the coating.
This test is qualitative only. Residence time of the solution
is important.
APPENDIX 8: MEK RESISTANCE
EQUIPMENT
1. TWO pound ball peen hammer.
2. 4” x 4” square of felt to cover ball on hammer.
3. 6” x 12” drawdown coated with batch to be tested.
4. Methyl ethyl ketone.
5. Oven.
6. Meyer bar.
PROCEDURE:
1. Apply coating to substrate and cure.
2. Apply MEK to felt attached to the hammer.
3. Stroke the drawdown with a back and forth motion at a
constant rate.
4. Each back and forth motion is counted as a double rub.
5. Care must be taken to keep the handle of the hammer
level with the table top and no downward pressure should
be exerted on the hammer.
6. Stroke the hammer until the first sign of the substrate
shows. Discount any breakthrough at the pivot point on
each end of the stroke.
APPENDIX 9: STEEL WOOL ROTARY TEST
This severe abrasion test uses a 1.25 inch square pad
of commercially available 0000 grade steel wool. The steel
wool pad is loaded with appropriate weights to give either
12 psi or 24 psi pressure. The pad is rotated on the substrate
five times. Results are reported as an increase in the percent
haze.
APPENDIX 10: TACK BY INKOMETER
The inkometer is an instrument designed to measure the
effective consistency of printing inks under conditions in
39

which the degree of working the ink closely approximates
that which takes place during printing.
Results are obtained in numerical values for the torque
required to “work” the ink film at known rates, with
predetermined film thickness and temperature.
Records can be made either in the form of consistency
curves or of numerical values for tack and length. In addition
to consistency, the inkometer is useful for the following:
1. Tack Readings
To determine the tack of process inks. The numerical tack
value would have a characteristic level for each “down”.
For example a printing sequence of yellow, red, blue and
black might have tack readings of 14, 13, 12 and 10
respectively.
2. Press Stability
To determine press stability - this can be gauged by noting
the percentage tack increase with time. Generally a 10 minute
period is used. Tack readings are to be taken each minute
from 1 to 10. The stability should be reported as the highest
tack value measured over the 10 minute cycle.
3. Misting or Flying
To determine misting Or flying of a particular ink under controlled
conditions to simulate the ink’s behavior on a commercial
press or decorator. This test provides controlled
speed, temperature, film thickness, and roller contact
pressure.
EQUIPMENT
1. Inkometer.
2. Ink pipette.
3. 3” spatula.
4. Stopwatch.
PROCEDURE:
1. Check water bath to make sure it is 90 F.
2. Set roller RPM at:
a. For tack and stability, use 1200 RPM or as specified.
b. For misting, use 90 F/1200 RPM or as specified.
3. Balance the machine at the operating speed to be used
in subsequent tests. This is accomplished by moving the
locking lever to the left to release the beam and adjusting
the counterweight at the left rear of the machine to bring
the indicating pointer in line with the middle line at the
beam end.
4. Prior to the first inkometer test of the day, zero the instrument
using the 10 and 25 check weights.
5. Prior to each determination (unless the inkometer is being
run continuously) run the instrument dry for 15
minutes with the top roller and vibrating roller in contact
with the brass roller.
6. Prior to the first inkometer test of the day, condition the
rollers by running an ink for at least 1 minute. Clean up
with recommended solvents. Dry rollers with isopropyl
alcohol.
7.
8.
9.
10.
11.
12.
Fill the ink metering device with the ink to be tested.
Push the piston all the way out and then allow it to return
slowly, working the ink into the cup with a spatula to
eliminate air bubbles. Make sure the piston is completely
down and screwed tight. Scrape off the excess ink by
passing the edge of the spatula across the end of the
pipette, at such an angle that the surface will be completely
level.
Spread the ink evenly across the upper roller. Wipe off
any ink remaining in the pipette on the vibrator roll.
Obtain initial distribution by turning the motor coupling
by hand. Distribute the ink for 10 seconds at 400 RPM
prior to the start of the 1 minute tack reading.
Switch the RPM to 1200 and start the timer immediately.
Move the sliding weight so that the beam is continuously
in balance. Release the beam only when taking a
reading and at the designated times. Take readings at one
minute intervals.
Standard tack readings are at 1200 RPM at 90 F for 60
seconds.
NOTES
1. To determine press stability, note the percentage change
in tack with time. The greater the rate of change, the
lower the ink stability.
2. To determine flying and misting, suspend a piece of white
paper under the roller and allow the inkometer to run
at operating speed for one minute. At the end of this
period, examine the paper for the presence of ink.
3. Calibration weights can be purchased to check the
mechanical integrity of the inkometer.
4. A rubber durometer can be purchased to monitor the condition
of the rubber rollers.
APPENDIX 11: FINGER TAPOUT TEST
The test consists of placing a small amount of ink on
the index finger and tapping the finger on a rigid surface,
such as a piece of glass. The subjective resistance to movement
or the stickiness of the ink is noted. The test is usually
run by an experienced person or with a control ink. The test
is highly subjective. Temperature will affect results. This test
is not recommeded for acrylated materials.
APPENDIX 12: THERMAL CONDUCTIVITY
MEASUREMENTS BY MEANS OF A
TWIN STANDARD COMPARATIVE
INSTRUMENT AND ITS USE WITH LIQUIDS
The twin standard comparative method of measuring
thermal conductivity utilizes two standards of known thermal
conductivity material, which are placed on either side
of an unknown sample. An axial flow of heat is caused to
flow through this stack by placing a heater on one side of
40

the stack and a liquid cooled heat sink on the other side. Thermocouples
are then used to measure the interface temperatures.
The test stack is well insulated laterally so that the
heat flow is almost unidirectional. Since small heat losses
do occur at the sides, the two standards are used, one measuring
the heat flow into the sample and the other measuring
the heat flow out of the sample. To contain a liquid use an
0 ring. The average measurements of the two standards
represents a good value for the heat flow through the
unknown sample. If we say the average heat flux through
the two standards is equal to the heat flux through the sample,
we have:
Q/A (standards) = QIA (sample)
where QIA equals the heat flow per unit area, Btu/hr-sq. ft.
and (k T/ X) (standard) = (k T/ X (sample)
where k = thermal conductivity, Btu-in/hr-sq. ft.-F
T = temperature difference, F
X = thickness normal to heat flow, inches
Thus: k (sample) = K (standard) ( T/ X) (std.) ( X/ T) (sample)
Since all quantities to the left are known or can be measured,
the thermal conductivity of the sample can be determined.
Convection or motion of the fluid is considered to be
negligable. The standards used are %" thick by 2" diameter
disks of fused silica (quartz) .p
41

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APPENDIX 13
ASTM TEST METHODS
43

I' Annual
Wb
Designation: D 149 - 81
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
DIELECTRIC BREAKDOWN VOLTAGE AND DIELECTRIC
STRENGTH OF SOLID ELECTRICAL INSULATING
MATERIALS AT COMMERCIAL POWER FREQUENCIES'
This standard is issued under the fixed designation D 149: the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval.
This method has been approved for use by agencies of the Department of Defense to replace Method 4031 of Federal Test Method
Standard 406 and for listing in the Do D Index of Specifications and Standards.
1. scope
1.1 This method covers the procedure for
determination of the dielectric strength of solid
insulating materials at commercial power frequencies,
under specified conditions.
1.2 Unless otherwise specified, the tests shall
be made at 60 Hz. However, this method may
be used at any frequency from 25 to 800 Hz.
At frequencies above 800 Hz dielectric heating
may be a problem.
1.3 This method is intended to be used in
conjunction with the ASTM standard or other
document that refers to this method. References
to this document should specify the particular
options to be used (see 4.4).
1.4 It may be used at various temperatures,
and in any suitable gaseous or liquid surrounding
medium.
1.5 This method is not intended for measuring
the dielectric strength of materials that are
fluid under the conditions of test.
1.6 This method is not intended for use in
determining intrinsic dielectric strength, directvoltage
dielectric strength, or thermal failure
under electrical stress (see Method D 3 15 i j.
1.7 The method is most commonly used to
determine the dielectric breakdown voltage
through the thickness of a test specimen (puncture).
It may also be used to determine dielectric
breakdown voltage along the interface between
a solid specimen and a gaseous or liquid
surrounding medium (flashover). With the addition
of instructions modifying Section 1 I, this
method may be used for proof testing.
1.8 The method appears in
sections:
Subject
Apparatus
Applicable Documents
Calculations
Calibration
Conditioning
Procedure
Precision and Accuracy
Report
Safety Precautions
Sampling
Scope
Significance
Summary of Method
Terminology
Test Specimens
the following
Section
6
2
13
IO
I I
12
15
14
7
8
I
4
3
5
9
2. Applicable Documents
2.1 ASTM Standards:
D 374 Tests for Thickness of Solid Electrical
Insulation2
D 6 I8 Conditioning Plastics and Electrical
Insulating Materials for Testing'
D 877 Test for Dielectric Breakdown Voltage
of Insulating Liquids Using Disk Electrodes"
D 171 1 Definitions of Terms Relating to
Electrical Insulation2s ''
' This method is under the jurisdiction of ASTM Committee
D-9 on Electrical Insulating Materials and is the direct
responsibility of Subcommittee D09.12 on Electrical Tests.
Current edition approved Jan. 30, I98 I. Published March
1981. Originally published as D 149-22 T. Last previous edition
D 149-75.
'Annual Book of ASTM Standards, Part 39.
Book of ASTM Standards. Part 40.
44

D 2413 Preparing and Electrical Testing of
Insulating Paper and Board Impregnated
with a Liquid Dielectric',
D 2436 Specification for Forced-Convection
Laboratory Ovens for Electrical Ovens2
D 3 15 1 Test for Thermal Failure Under
Electric Stress of Solid Electrical Insulating
Materials'
D 3487 Specification for Mineral Insulating
Oil Used in Electrical Apparatus3
2.2 Other Standards:
International Electrotechnical Commis~ion:~
Pub. 243 Recommended Methods of Test for
Electrical Strength of Solid Insulating Materials
at Power Frequencies
American National Standards Institute
Standard:4
C68.1 Techniques for Dielectric Tests, IEEE
Standard No. 4
3. Summary of Method
3.1 Alternating voltage, at a commercial
power frequency (60 Hz, unless otherwise specified)
is applied to a test specimen. The voltage
is increased from zero or from a level well
below the breakdown voltage, in one of three
prescribed methods of voltage application, until
dielectric failure of the test specimen occurs.
3.2 Most commonly, the test voltage is applied
using simple test electrodes on opposite
faces of specimens. The specimens may be
molded or cast, or cut from flat sheet or plate.
Other electrode and specimen configurations
may be used to accommodate the geometry of
the sample material, or to simulate a specific
application for which the material is being
evaluated.
4. Significance and Use
4.1 The dielectric strength of an electrical
insulating material is a property of interest for
any application where an electrical field wil: be
present. In many cases the dielectric strength of
a material will be the determining factor in the
design of the apparatus in which it is to be
used.
4.2 Tests made as specified herein may be
used to provide part of the information needed
for determining suitability of a material for a
given application; and also, for detecting
changes or deviations from normal characteristics
resulting from processing variables, aging
conditions, or other manufacturing or environmental
situations. This method is useful for
process control, acceptance or research testing.
4.3 Results obtained by this method can seldom
be used directly to determine the dielectric
behavior of a material in an actual application.
In most cases it is necessary that these results
be evaluated by comparison with results obtained
from other functional tests or from tests
on other materials, or both, in order to estimate
their significance for a particular material.
4.4 Documents specifying the use of this
method should also specify:
4.4.1 Method of voltage application,
4.4.2 Voltage rate-of-rise, if slow rate-of-rise
method is specified,
4.4.3 Specimen selection, preparation, and
conditioning,
4.4.4 Surrounding medium and temperature
during test,
4.4.5 Electrodes, and
4.4.6 Any desired deviations from the recommended
procedures as given.
4.5 If any of the requirements listed in 4.4
are missing from the specifying document, then
the recommendations for the several variables
shall be followed.
4.6 Appendix X1 contains a more complete
discussion of the significance of dielectric
strength tests.
5. Terminology
5.1 Refer to Definitions D 171 1 for definitions
of the following terms:
5.1.1 dielectric breakdown voltage,
5.1.2 dielectric failure,
5.1.3 dielectric strength, and
5.1.4 flashover.
6. Apparatus
6.1 Voltage Source-Obtain the test voltage
from a step-up transformer supplied from B
variable sinusoidal low-voltage source. The
transformer, its voltage source, and the associated
controls shall have the following capabilities:
6.1.1 The ratio of crest to root-mean-square
(rms) test voltage shall be equal to h k 5 9%
(1.34 to 1.48), with the test specimen in the
Available from American National Standards Institute,
1430 Broadway, New York, N.Y. 10018.
45

D 149
circuit, at all voltages greater than 50 96 of the
breakdown voltage.
6.1.2 The capacity of the source shall be
sufficient to maintain the test voltage until
dielectric breakdown occurs. For most materials,
using electrodes similar to those shown in
Table 1, an output current capacity of 40 mA
is usually satisfactory. For more complex electrode
structures, or for testing high-loss materials,
higher current capacity may be needed.
The power rating for most tests will vary from
0.5 kVA for testing low-capacitance specinlens
at voltages up to 10 kV, to 5 kVA for voltages
up to 100 kV.
6.1.3 The controls on the variable low-voltage
source shall be capable of varying the
supply voltage and the resultant test voltage
smoothly, uniformly, and without overshoots
or transients, in accordance with 12.1. Under
no circumstance shall the peak of any voltage
transient exceed 1.48 times the indicated rms
test voltage. Motor-driven controls are preferable
for making short-time (see 12.1.1) or slowrate-of-rise
(see 12.1.3) tests.
6.1.4 Equip the voltage source with a circuitbreaking
device that will operate within three
cycles. The device shall disconnect the voltage
source equipment from the power service and
protect it from overload as a result of specimen
breakdown causing an overload of the testing
apparatus. If prolonged current follows breakdown
it will result in unnecessary burning of
the test specimens, pitting of the electrodes, and
contamination of any liquid surrounding medium.
6. I .5 The circuit-breaking device should
have an adjustable current-sensing element in
the step-up transformer secondary, to allow for
adjustment consistent with the specimen characteristics
and arranged to sense specimen current.
Set the sensing element to respond to a
current that is indicative of specimen breakdown.
6.1.6 The specimen current-sensing element
may be in the primary of the step-up transformer.
Calibrate the current-sensing dial in
terms of specimen current.
6.1.7 Exercise care in setting the response of
the current control. If the control is set too
high, the circuit will not respond when breakdown
occurs; if set too low, it may respond to
leakage currents, capacitive currents, or partial
discharge (corona) currents or, when the sensing
element is located in the primary, to the
step-up transformer magnetizing current.
6.2 Voltage Measurement-A voltmeter
must be provided for measuring the rms test
voltage. A peak-reading voltmeter may be used,
in which case divide the reading by h to get
rms values. The overall error of the voltagemeasuring
circuit shall not exceed 5 96 of the
measured value. In addition, the response time
of the voltmeter shall be such that its time lag
will not be greater than 1 96 of full scale at any
rate-of-rise used.
6.2.1 Measure the voltage using a voltmeter
or potential transformer connected to the specimen
electrodes, or to a separate voltmeter
winding, on the test transformer, that is unaffected
by the step-up transformer loading.
NOTE-Those test sets making use of test transformer
primary voltage measurement as an indication
of the voltage across the specimen electrodes is in
violation of this issue of the method unless calibrated
at the specific breakdown voltage and current. Calibration
will be dependent upon transformer secondary
current and voltage at the time of breakdown.
6.2.2 It is desirable for the reading of the
maximum applied test voltage to be retained
on the voltmeter after breakdown so that the
breakdown voltage can be accurately read and
recorded.
6.3 Electrodes-For a given specimen configuration,
the dielectric breakdown voltage
may vary considerably, depending upon the
geometry and placement of the test electrodes.
For this reason it is important that the electrodes
to be used be described when specifying
this method, and that they be described in the
report.
6.3.1 One of the electrodes listed in Table 1
should be specified by the document referring
this method. If no electrodes have been specified
select an applicable one from Table 1, or
use other electrodes mutually acceptable to the
parties concerned when the standard electrodes
cannot be used due to the nature or configuration
of the material being tested. See references
in Appendix X2 for examples of some
special electrodes. In any event the electrodes
must be described in the report.
6.3.2 The electrodes should be in contact
with the test specimen over the entire area of
the electrode, except for such obvious areas as
46

D 149
the rounded edges of Types 1, 2, 3, and 6 of
Table 1.
6.3.3 Keep the electrode surfaces clean and
smooth, and free from projecting irregularities
resulting from previous tests. If asperities have
developed, they must be removed.
6.3.4 Whenever the electrodes are dissimilar
in size or shape, the one at which the lowest
concentration of stress exists, usually the larger
in size and with the largest radius, should be at
ground potential.
6.3.5 In some special cases liquid metal electrodes,
foil electrodes, metal shot, water, or
conductive coating electrodes are used. It must
be recognized that these may give results differing
widely from those obtained with other
types of electrodes.
6.3.6 Because of the effect of the electrodes
on the test results, it is frequently possible to
obtain additional information as to the dielectric
properties of a material (or a group of
materials) by running tests with more than one
type of electrodes. This technique is of particular
value for research testing.
6.4 Surrounding Medium-The document
calling for this method should specify the surrounding
medium and the test temperature, if
tests are not to be made in air at ambient
temperature and humidity. It is normally preferable
to test materials in the medium in which
they are to be used. When conditions of use are
not well-defined, materials should be tested in
air, unless the breakdown voltage is so high as
to require excessively large specimens, or to
cause heavy surface discharges and burning
prior to failure. Flashover must be avoided,
and the effects of partial discharges prior to
failure minimized, even on short-time tests. The
material of the seals or shrouds around the
electrodes may influence the breakdown values.
For specimens having a high breakdown
voltage it is frequently preferable or even necessary
to make tests in insulating oil. Breakdown
values obtained in insulating oil may not
be comparable with those obtained in air. In
many cases, particularly for research or qualification
purposes, it is desirable to test at the
expected temperature of operation.
6.4.1 When tests are made in insulating oil,
an oil bath of adequate size shall be provided.
The use of glass containers is not recommended
for tests at voltages above about 10 kV, because
the energy released at breakdown may be sufficient
to shatter the container. Metal baths
must be grounded. It is recommended that
mineral oil meeting the requirements of Specification
D 3487, Type I or 11, be used. It should
have a dielectric breakdown voltage as determined
by Method D877 of at least 26 kV.
Other dielectric fluids may be used as surrounding
mediums if specified. These include,
but are not limited to, silicone fluids and other
liquids intended for use in transformers, circuit
breakers, capacitors, or cables.
6.4.1.1 Breakdown values obtained using
liquids having different electrical properties
may not be comparable. See X1.4.7. If tests are
to be made at other than room temperature,
the bath must be provided with a means for
heating or cooling the liquid, and with a means
to ensure uniform temperature. Small baths
can in some cases be placed in an oven (see
6.4.2) in order to provide temperature control.
If forced circulation of the fluid is provided,
care must be taken to prevent bubbles from
being whipped into the fluid. The temperature
shall be maintained within & 5°C of the specified
test temperature at the electrodes, unless
otherwise specified. In many cases it is specified
that specimens to be tested in insulating oil are
to be previously impregnated with the oil and
not removed from the oil before testing (see
Method D 2413). For such materials, the bath
must be of such design that it will not be
necessary to expose the specimens to air before
testing.
6.4.2 If tests in air are to be made at other
than ambient temperature or humidity, an oven
or controlled humidity chamber must be provided
for the tests. Ovens meeting the requirements
of Specification D2436 and provided
with means for introducing the test voltage will
be suitable for use when only temperature is to
be controlled.
6.4.3 Tests in gasses other than air will generally
require the use of chambers that can be
evacuated and filled with the test gas, usually
under some controlled pressure. The design of
such chambers will be determined by the nature
of the test program to be undertaken.
6.5 Test Chamber-The test chamber or area
in which the tests are to be made shall be of
sufficient size to hold the test equipment, and
shall be provided with interlocks to prevent
47

D 149
accidental contact with any electrically energized
parts. A number of different physical
arrangements of voltage source, measuring
equipment, baths or ovens, and electrodes are
possible, but it is essential that (I) all gates or
doors providing access to spaces in which there
are electrically energized parts be interlocked
to shut off the voltage source when opened; (2)
clearances are sumciently large that the field in
the area of the electrodes and specimen are not
distorted and that flashovers and partial discharges
(corona) do not occur except between
the test electrodes; and (3) insertion and replacement
of specimens between tests be as
simple and convenient as possible. Visual observation
of the electrodes and test specimen
during the test is frequently desirable.
7. Safety Precautions
7.1 Lethal voltages are present during every
dielectric breakdown test. It is essential that the
test apparatus and all associated equipment
that may be electrically connected to it be
designed, installed, and operated so that it is
not possible for any person to make contact
with energized conductors.
7.2 Solidly ground all metal parts that any
person might come into contact with during the
test.
7.3 Thoroughly instruct all operators in the
proper way to conduct the tests safely.
7.4 When making tests at high voltage with
large area electrodes, particularly in compressed
gas or in oil, the energy released at
breakdown may be sufficient to result in fire,
explosion, or rupture of the test chamber. Design
of test equipment, test chambers, and test
specimens should be such as to minimize the
possibility of such occurrences, and to eliminate
the possibility of personal injury.
8. Sampling
8.1 The detailed sampling procedure for the
material being tested should be defined in the
specification for that material
8.2 Sampling procedures for quality control
purposes should provide for gathering of sufficient
samples to estimate both the average
quality and the variability of the lot being
examined; and for proper protection of the
samples from the time they are taken until the
preparation of the test specimens in the labo-
ratory or other test area is begun.
8.3 For the purposes of most tests it is desirable
to take samples from areas that are not
immediately adjacent to obvious defects or discontinuities
in the material. The outer few layers
of roll material, the top sheets of a package
of sheets, or material immediately next to an
edge of a sheet or roll should be avoided, unless
the presence or proximity of defects or discontinuities
is of interest in the investigation of the
material.
8.4 The sample should be large enough to
permit making as many individual tests as may
be requiied for the particular material (see
12.3).
9. Test Specimen
9.1 Preparation and Handling:
9.1.1 Prepare specimens from samples collected
in accordance with Section 8.
9.1.2 When flat-faced electrodes are to be
used, the surfaces of the specimens which will
be in contact with the electrodes shall be
smooth parallel planes, insofar as possible without
actual surface machining.
9.1.3 The specimens shall be of sufficient
size to prevent flashover under the conditions
of test. For thin materials it may be convenient
to use specimens large enough to permit making
more than one test on a single piece.
9.1.4 For thicker materials (usually more
than 2 mm thick) the breakdown strength may
be high enough that flashover or intense surface
partial discharges (corona) may occur prior to
breakdown. Techniques that may be used to
prevent flashover, or to reduce partial discharge
(corona) include:
9.1.4.1 Immerse the specimen in insulating
oil during the test. See X 1.4.7 for the surrounding
medium factors influencing breakdown.
This may be necessary for specimens that have
not been dried and impregnated with oil, as
well as for those which have been prepared in
accordance with Method D 2413, for example.
(See 6.4.)
9.1.4.2 Machine a recess or drill a flat-bottom
hole in one or both surfaces of the specimen
to reduce the test thickness. If dissimilar
electrodes are used (such as Type 6 of Table 1)
and only one surface is to be machined, the
larger of the two electrodes should be in contact
with the machined surface. Care must be taken
48

D 149
in machining specimens not to contaminate or
mechanically damage them.
9.1.4.3 Apply seals or shrouds around the
electrodes, in contact with the specimen to reduce
the tendency to flashover.
9.1.5 Materials that are not in flat sheet form
shall be tested using specimens (and electrodes)
appropriate to the material and the geometry
of the sample. It is essential that for these
materials both the specimen and the electrodes
be defined in the specification for the material.
9.1.6. Whatever the form of the material, if
tests of other than surface-to-surface puncture
strength are to be made, define the specimens
and the electrodes in the specification for the
material.
9.2 In nearly all cases the actual thickness of
the test specimen is important. Unless otherwise
specified, measure the thickness after the test
in the immediate vicinity of the area of breakdown.
Measurements shall be made at room
temperature (25 f 5"C), using the appropriate
procedure of Method D 374.
10. Calibration
10.1 In making calibration measurements,
take care that the values of voltage at the
electrodes can be determined within the accuracy
given in 6.2, with the test specimens in the
circuit.
10.2 Use an independently calibrated voltmeter
attached to the output of the test voltage
source to verify the accuracy of the measuring
device. Electrostatic voltmeters, voltage dividers,
or potential transformers having comparable
accuracy may be used for calibration measurement.
10.3 At voltages above about 12 kV rms
(16.9 kV peak) a sphere gap may be used to
calibrate the readings of the voltage-measuring
device. Follow procedures as specified in ANSI
C68.1 in such calibration.
11. Conditioning
11.1 The dielectric strength of most solid
insulating materials is influenced by temperature
and moisture content. Materials so affected
should be brought to equilibrium with an atmosphere
of controlled temperature and relative
humidity before testing. For such materials,
the conditioning should be included in
the specification referencing this method.
1 I .2 Unless otherwise specified, follow the
procedures in Method D 6 18.
11.3 For many materials the moisture content
has more effect on dielectric strength than
does temperature. Conditioning times for these
materials should be sufficiently long to permit
the specimens to reach moisture equilibrium as
well as temperature equilibrium.
1 1.4 If the conditioning atmposphere is such
that condensation occurs on the surface of the
specimens, it may be desirable to wipe the
surfaces of the specimens immediately before
testing. This will usually reduce the probability
of surface flashover.
12. Procedure
12.1 Methods of Voltage Application:
12.1.1 Method A, Short-Time Test-Apply
voltage uniformly to the test electrodes from
zero at one of the rates shown in Fig. 1A until
breakdown occurs. Use the short-time test unless
othwise specified.
12.1.1.1 When establishing a rate initially in
order for it to be included in a new specification,
select a rate that, for a given set of specimens,
will give an average time to breakdown
of between 10 and 20 s. It may be necessary to
run one or two preliminary tests in order to
determine the most suitable rate-of-rise. For
many materials a rate of 500 V/s is used.
12.1.1.2 If the document referencing this
method specified a rate-of-rise it shall be used
consistently in spite of occasional average time
to breakdown falling outside the range of 10 to
20 s. In this case, the times to failures shall be
made a part of the report.
12.1.1.3 In running a series of tests comparing
different material, the same rate-of-rise
shall be used with preference given to a rate
that allows the average time to be between 10
and 20 s. If the time to breakdown cannot be
adhered to, the time shall be made a part of the
report.
12.1.2 Method B, Step-by-Step Test-Apply
voltage to the test electrodes at the preferred
starting voltage and in steps and duration as
shown in Fig. IB until breakdown occurs.
12.1.2.1 From the list in Fig. 1B select the
initial voltage to be the one closest to 50 96 of
the experimentally determined or expected
breakdown voltage under the short time test.
12.1.2.2 If an initial voltage other than one
of the preferred values listed in Fig. 1B is
selected, it is recommended that the voltage
49

D 149
steps be 10% of the preferred initial voltage
immediately below the selected value.
12.1.2.3 Apply the initial voltage by increasing
the voltage from zero as rapidly as can be
accomplished without introducing a transient
voltage or overshoot beyond that permitted in
6.1.3. Similar requirements shall apply to the
procedure used to increase the voltage between
successive steps. After the initial step, the time
required to raise the voltage to the succeeding
step shall be counted as part of the time at the
succeeding step.
12.1.2.4 If breakdown occurs while the voltage
is being increased to the next step, it shall
be recorded as having occurred at the next
lower step and the actual breakdown voltage
also reported.
12.1.2.5 It is desirable that breakdown occur
in four to ten steps, but in not less than 120 s.
If failure occurs at the third step or less, or in
less than 120 s, whichever is greater, on more
than one specimen in a group, the tests should
be repeated with a lower initial voltage. If
failure does not occur before the twelfth step
or greater than 720 s, increase the initial voltage.
12.1.2.6 Record the initial voltage, the voltage
steps, the breakdown voltage, and the
length of time that the breakdown voltage was
held. If failure occurred while the voltage was
being increased to the starting voltage the failure
time shall be zero.
12.1.2.7 Other time lengths for the voltage
steps may be specified, depending upon the
purpose of the test. Commonly used lengths are
20 s and 300 s (5 min). For research purposes,
it may be of value to conduct tests using more
than one time interval on a given material.
12.1.3 Method C, Slow Rate-of-Rise Test-
Apply voltage to the test electrodes, from the
starting voltage and at the rate shown in Fig.
IC until breakdown occurs.
12.1.3.1 Select the initial voltage from shorttime
tests made as specified in 12.1.1. The
initial voltage shall be reached as specified in
12.1.2.3.
12.1.3.2 Use the rate-of-voltage rise from the
initial value specified in the document calling
for this method. Ordinarily the rate is selected
to approximate the average rate for a step-bystep
test.
12.1.3.3 If more than one specimen of a
group of specimens breaks down in less than
120 s, reduce either the initial voltage or the
rate-of-rise, or both.
12.1.3.4 If more than one specimen of a
group of specimens breaks down at less than
1.5 times the initial voltage, reduce the initial
value. If breakdown repeatedly occurs at a
value greater than 2.5 times the initial value
(and at a time of over 120 s), increase the initial
voltage.
12.2 Criteria of Breakdown-Dielectric failure
or dielectric breakdown (as defined in Definitions
D 171 1) consists of an increase in conductance,
limiting the electric field that can be
sustained. This phenomenon is most commonly
evidenced during the test by abrupt rupture
through the thickness of the specimen, which
can be seen and heard, and which results in a
visible puncture and decomposition of the specimen
in the breakdown area. This form of
breakdown is generally irreversible. Repeated
applications of voltage level (sometimes unmeasurably
low), usually with additional damage
at the breakdown area. Such repeated applications
of voltage may be used to give positive
evidence of breakdown and to make the
breakdown path more visible.
12.2.1 A rapid rise in leakage current may
result in tripping of the voltage source without
visible decomposition of the specimen. This
type of failure, usually associated with slowrise
tests at elevated temperatures, may in some
cases be reversible, that is, recovery of the
dielectric strength may occur if the specimen is
allowed to cool to its original test temperature
bcfore reapplying voltage. The voltage source
must trip rapidly at relatively low current for
this type of failure to occur.
12.2.2 Tripping of the voltage source may
occur due to flashover, to partial discharge
current, to reactive current in a high capacitance
specimen, or to malfunctioning of the
breaker. Such interruptions of the test do not
constitute breakdown (except for flashover
tests) and should not be considered as a satisfactory
test.
12.2.3 If the breaker is set for too high a
current, or if the breaker malfunctions, excessive
burning of the specimen will occur.
12.3 Number of Tests-Make five breakdowns
unless otherwise specified for the particular
material.
50

13. Calculations
13.1 Calculate for each test the dielectric
strength in kV/mm or V/mil at breakdown,
and for step-by-step tests, the gradient at the
highest voltage step at which breakdown did
not occur.
13.2 Calculate the average dielectric
strength and the standard deviation, or other
measure of variability.
14. Report
14.1 The report shall include the following:
14.1.1 Identification of the test sample.
14.1.2 For Each Specimen:
14.1.2.1 Measured thickness,
14.1.2.2 Maximum voltage withstood (for
step-by-step tests),
14.1.2.3 Dielectric breakdown voltage,
14.1.2.4 Dielectric strength (for step-by-step
tests),
14.1.2.5 Dielectric breakdown stength, and
14.1.2.6 Location of failure (center of electrode,
edge, or outside).
14.1.3 For Each Sample:
14.1.3.1 Average dielectric withstand
strength,
14.1.3.2 Average dielectric breakdown
strength,
14.1.3.3 Indication of variability, preferably
the standard deviation and coefficient of variation,
14.1.3.4 Description of test specimens,
14.1.3.5 Conditioning and specimen preparation,
14.1.3.6 Ambient atmosphere temperature
and relative humidity,
4Slb D 149
14.1.3.7 Surrounding medium,
14.1.3.8 Test temperature,
14.1.3.9 Description of electrodes,
14.1.3.10 Method of voltage application, and
14.1.3.1 1 Date of test.
15. Precision and Accuracy
15.1 Single- Operator Precision-Depending
upon the variability of the material being
tested, the specimen thickness, method of voltage
application, and the extent to which transient
voltage surges are controlled or suppressed,
the coefficient of variation (standard
deviation divided by the mean) may vary from
a low 1 or 2% to as high as 20% or more.
When making duplicate tests on five specimens
from the same sample, the coefficient of variation
will usually be less than 7 %.
15.2 Multilaboratory Precision-The precision
of tests made in different laboratories (or
of tests made using different equipment in the
same laboratory) may be quite variable. If identical
types of equipment are used, with specimen
preparation, electrodes, and testing procedures
closely controlled, the single-operator
precision may be closely approached. When
direct comparison of results from two or more
laboratories is to be made, it is recommended
that the precision between the laboratories involved
be evaluated.
15.3 Accuracy-This method does not determine
the intrinsic dielectric strength. The test
values are dependent upon specimen geometry,
electrodes, and other variable factors, in addition
to the properties of the sample, so that it
is not possible to make a statement of accuracy.
51

sub D 149
TABLE I
Electrode
Description of
Tvpe
Opposing cylinders 51 mm (2 in.) in diameter, 25 mm
(1 in.) thick with edges rounded to 6.4 mm (0.25 in.)
radius
Opposing cylinders 25 mm ( I in.) in diameter, 25 mm
(1 in.) thick with edges rounded to 3.2 mm (0.125 in.)
radius
Opposing cylindrical rods 6.4 mm (0.25 in.) in diameter
with edges rounded to 0.8 mm (0.0313 in.) radius”
Typical Electrodes for Dielectric Strength Testing of Various Types of Insulating MaterialsA
Flat plates 6.4 mm (0.25 in.) wide and 108 mm (4.25
in.) long with edges square and ends rounded to 3.2
mm (0.125 in.) radius
Hemispherical electrodes 12.7 mm (0.5 in.) in diamete4‘
Opposing cylinders; the lower one 75 mm (3 in.) in
diameter, 15 mm (0.60 in.) thick the upper one 25
mm (I in.) in diameter, 25 mm thick; with edges of
both rounded to 3 mm (0.12 in.) radius’
Insulating Materials
flat sheets of paper, films, fabrics, rubber, molded plastics,
laminates, boards, glass, mica, and ceramic
same as for Type 1, particularly for glass, mica, plastic.
and ceramic
same as for Type I, particularly for varnish, plastic, and
other thin film and tapes: where small specimens
necessitate the use of smaller electrodes, or where
testing of a small area is desired
same as for Type I, particularly for rubber tapes and
other narrow widths of thin materials
filling and treating compounds, gels and semisolid compounds
and greases, embedding, potting, and encapsulating
materials
same as for Types 1 and 2
A These electrodes are those most commonly specified or referenced in ASTM standards. With the exception of Type 5
electrodes, no attempt has been made to suggest electrode systems for other than flat surface material. Other electrodes may
be used as specified in ASTM standards or as agreed upon between seller and purchaser where none of these electrodes in the
table is suitable for proper evaluation of the material being tested.
Electrodes are normally made from either brass or stainless steel. Reference should be made to the standard governing
the material to be tested to determine which, if either, material is preferable:
The electrodes surfaces should be polished and free from irregularities resulting from previous testing.
” Refer to the appropriate standard for the load force applied by the upper electrode assembly. Unless otherwise specified
the upper electrodes shall be 50 -t 2 g.
E Refer to the appropriate standard for the proper gap settings.
The Type 6 electrodes are those given in IEC Publication 243 for testing of flat sheet materials. They are less critical as
to concentricity of the electrodes than are the Types I and 2 electrodes.
FIG. 1A
Rates
(V/S) t 20 41,
IO0
200
500
IO00
2000
5000
Voltage Profile of Short-Time Test
52

Start
Step Voltage
Voltages when Increment Constraints
(kV) V. V. (kV)A is (kV)
0.25 5 or less 0.25 (ti - to) = (I?- ti) = (1.3 - tr) = 60 & 5 S
0.50 over 5 to 10 0.50
I over 10 to 25 I
2 over 25 to 50 2
5 over 50 to 100 5 120 5 t~ 5 720 s
10 over 100 10
20
50 step is used.)
100
(IM will usually exceed 720 s if 300 s time
A V. = 0.5 (V, for Short-Time Test), unless constraints cannot be met.
FIG. 1B Voltage Profile of Stepby-Step Test
Rates (V/s) f 20 %
tbd
Constraints
I
Ihd > 120 s
2
5
10
Yh,, = > 1.5 v,
12.5
20
25
50
100
FIG. 1C Voltage Profile of Slow Rated-Rise Test
53

APPENDIXES
XI. SIGNIFICANCE OF THE DIELECTRIC STRENGTH TEST
X1.l Introduction
XI. 1.1 A brief review of three postulated mechanisms
of breakdown, namely: (1) the discharge or
corona mechanism, (2) the thermal mechanism, and
(3) the intrinsic mechanism, as well as a discussion of
the principal factors affecting tests on practical dielectrics,
are given here to aid in interpreting the data.
The breakdown mechanisms usually operate in combination
rather than singly. The following discussion
applies only to solid and semisolid materials.
X1.2 Postulated Mechanisms of Dielectric Breakdown
XI .2.1 Breakdown Caused by Electrical Discharges-In
many tests on commercial materials,
breakdown is caused by electrical discharges, which
produce high local fields. With solid materials the
discharges usually occur in the surrounding medium,
thus increasing the test area and producing failure at
or beyond the electrode edge. Discharges may occur
in any internal voids or bubbles that are present or
may develop. These may cause local erosion or chemical
decomposition. These processes may continue
until a complete failure path is formed between the
electrodes.
XI .2.2 Thermal Breakdown-Cumulative heating
develops in local paths within many materials when
they are subjected to high electric field intensities,
causing dielectric and ionic conduction losses which
generate heat more rapidly than can be dissipated.
Breakdown may then occur because of thermal instability
of the material.
XI .2.3 Intrinsic Breakdown-If electric discharges
or thermal instability do not cause failure, breakdown
will still occur when the field intensity becomes sufficient
to accelerate electrons through the material.
This critical field intensity is called the intrinsic dielectric
strength. It cannot be determined by this test
method, although the mechanism itself may be involved.
X1.3 Nature of Electrical Insulating Materials
X1.3. I Solid commerical electrical insulating materials
are generally nonhomogeneous and may contain
dielectric defects of various kinds. Dielectric
breakdown often occurs in an area of the test specimen
other than that where the field intensity is
greatest and sometimes in an area remote from the
material directly between the electrodes. Weak spots
within the volume under stress sometimes determine
the test results.
X1.4 Influence of Test and Specimen Conditions
X 1.4.1 Electrodes-In general, the breakdown
voltage will tend to decrease with increasing electrode
area, this area effect being more pronounced with
thin test specimens. Test results are also affected by
the electrode geometry. Results may be affected also
by the material from which the electrodes are constructed,
since the thermal and discharge mechanism
may be influenced by the thermal conductivity and
the work function, respectively, of the electrode material.
Generally speaking, the effect of the electrode
material is difficult to establish because of the scatter
of experimental data.
XI .4.2 Specimen Thickness-The dielectric
strength of solid commerical electrical insulating materials
is greatly dependent upon the specimen thickness.
Experience has shown that for solid and semisolid
materials, the dielectric strength varies inversely
as a fractional power of the specimen thickness, and
there is a substantial amount of evidence that for
relatively homogeneous solids, the dielectric strength
varies approximately as the reciprocal of the square
root of the thickness. In the case of solids that can be
melted and poured to solidify between fixed electrodes,
the effect of electrode separation is less clearly
defined. Since the electrode separation can be fixed
at will in such cases, it is customary to perform
dielectric strength tests on liquids and usually on
fusible solids, with electrodes having a standardized
fixed spacing. Since the dielectric strength is so dependent
upon thickness it is meaningless to report
dielectric strength data for a material without stating
the thickness of the test specimens used.
X 1.4.3 Temperature-The temperature of the test
specimen and its surrounding medium influence the
dielectric strength, although for most materials small
variations of ambient temperature may have a negligible
effect. In general, the dielectric strength will
decrease with increasing temperatures, but the extent
to which this is true depends upon the material under
test. When it is known that a material will be required
to function at other than normal room temperature,
it is essential that the dielectric strength-temperature
relationship for the material be determined over the
range of expected operating temperatures.
X1.4.4 Time-Test results will be influenced by
the rate of voltage application. In general, the breakdown
voltage will tend to increase with increasing
rate of voltage application. This is to be expected
because the thermal breakdown mechanism is timedependent
and the discharge mechanism is usually
time-dependent, although in some cases the latter
mechanism may cause rapid failure by producing
critically high local field intensitives.
XI .4.5 Wave Form-In general, the dielectric
strength is influenced by the wave form of the applied
voltage. Within the limits specified in this method
the influence of wave form is not significant.
X 1.4.6 Frequency-The dielectric strength is not
54

D 149
significantly influenced by frequency variations
within the range of commerical power frequencies
provided for in this method. However, inferences
concerning dielectric strength behavior at other than
commerical power frequencies (50 to 60 Hz) must
not be made from results obtained by this method.
X I .4.7 Surrounding Medium-Solid insulating
materials having a high breakdown voltage are usually
tested by immersing the test specimens in a liquid
dielectric such as tranformer oil, silicone oil, or chlorofluorocarbons,
in order to minimize the effects of
surface discharges prior to breakdown. It has been
shown by S. Whitehead5 that in order to avoid discharges
in the surrounding medium prior to reaching
the breakdown voltage of the solid test specimen, in
alternating voltage tests it is necessary that
Emelm >
If the liquid immersion medium is a low loss material,
the criterion simplifies to
and if the liquid immersion medium is a semiconducting
material the criterion becomes
Emam 27f~r~0Es
where:
E = electric strength,
f = frequency,
E and E' = permittivity,
D = dissipation factor, and
U = conductivity (S/m).
Subscripts:
m refers to immersion medium,
r refers to relative,
0 refers to free space,
(EO = 8.854 X IO-'' F/m) and
s refers to solid dielectric.
X1.4.7. I Whitehead points out that it is therefore
desirable to increase E, and em, or um, if surface
discharges are to be avoided. He also mentions (p.
261) that the use of moist semiconducting oil can
effect an appreciable reduction in edge discharges.
Unless the breakdown path between the electrodes is
solely within the solid, results in one medium cannot
be compared with those in a different medium. It
should also be noted that if the solid is porous or
capable of being permeated by the immersion medium,
the breakdown strength of the solid is directly
affected by the electrical properties of immersion
medium.
XI .4.8 Relative Humidity-The realtive humidity
influences the dielectric strength to the extent that
moisture absorbed by, or on the surface of, the material
under test affects the dielectric loss and surface
conductivity. Hence, its importance will depend to a
large extent upon the nature of the material being
tested. However, even materials that absorb little or
no moisture may be affected because of greatly increased
chemical effects of discharge in the presence
of moisture. Except in cases where the effect of
exposure on dielectric strength is being investigated,
it is customary to control or limit the relative humidity
effects by standard conditioning procedures.
X1.5 Evaluation
X1.5.1 A fundamental requirement of the insulation
in electrical apparatus is that it withstand the
voltage imposed on it in service. Therefore there is a
great need for a test to evaluate the performance of
particular materials at high voltage stress. The dielectric
breakdown voltage test represents a convenient
preliminary test to determine whether a material
merits further consideration, but it falls short of a
complete evaluation in two important respects. First,
the condition of a material as installed in apparatus
is much different from its condition in this test,
particularly with regard to the configuration of the
electric field and the area of material exposed to it,
corona, mechanical stress, ambient medium, and association
with other materials. Second, in service
there are deteriorating influences, heat, mechanical
stress, corona and its products, contaminants, etc.,
which may reduce the breakdown voltage far below
its value as originally installed. Some of these effects
can be incorporated in laboratory tests, and a better
estimate of the material will result, but the final
consideration must always be that of the performance
of the material in actual service.
X1.5.2 The dielectric breakdown test may be used
as a material inspection or quality control test, as a
means of inferring other conditions such as variability,
or to indicate deteriorating processes such as
thermal aging. In these uses of the test it is the relative
value of the breakdown voltage that is important
rather than the absolute value.
' Whitehead, S., Dielectric Breakdown of Solids, Oxford
University Press, 195 I.
X2. STANDARDS REFERRING TO METHOD D 149
X2.1 Introduction
~2.1.1 It is not expected that the documents listed
in this appendix comprise a complete list of ASTM
standards referring to Method D 149. This listing is
included herein for the purpose of providing reference
to a broad spectrum of documents concerned
with dielectric strength at power frequencies. In some
cases the manner in which the reference is made to
this method is not in conformance with the requirements
of 4.4. Do not use another document, such as
those given in this as a model for providing
reference to this method, unless there is conformity
with 4.4.
55

ASTM
Designation
Subject
Fabric, Fiber, Paper, Tape, Film, Flexible
Composites, and Coated Fabrics:
D 69
D 119
D 202
D 295
D 373
D 619
D 902
D IO00
D 1373
D 1389
D 1458
D 1459
D 1830
D 1930
D 2305
D 2381
D 2413
D 3391
Friction Tape
Rubber Tape
Insulating Paper
Varnished Cotton Fabric
Tape
Black Bias-Cut Varnished
Cloth and Tape
Vulcanized Fiber
Resin-Coated Glass Fabrics
and Tapes
Pressure-Sensitive Adhesive-Coated
Tapes
Ozone-Resistant Rubber
Tape
Thin Solid Electric Insulating
Material
Silicone Rubber-Coated
Glass Fabric and Tapes
Silicone Varnished Glass
Cloth and Tape
Coated Fabirc
Kraft Dielectric Tissue
Polymeric Film
Flexible Composite
Impregnated Paper
Rubber Tape
Molding and Embedding Compounds:
D700 Phenolic Molding Compounds
D 704 Melamine-Formaldehyde
Molding Compounds
D 705 Urea-Formaldehyde Molding
Compounds
D 729 Vinylidene Chloride Molding
Compounds
451r D 149
X2.2 ASTM Standards Referring to Method D 149
ASTM
Desig-
Subject
nation
D 1430 Polychlorotrifuoroethylene
(PCTFE) Plastic
D 1636 Allyl Molding Compounds
D 1674 Polymerizable Embedding
Compounds
Mica, Glass, and Porcelain:
D I16 Vitrified Ceramic Materials
D 352 Pasted Mica
D 748 Natural Block Mica
D 1039 Glass-Bonded Mica
D 1677 Untreated Mica Paper
D 2442 Alumina Ceramics
Sleeving, Tubes, Sheets, and Rods.
D 229 Rigid Sheet and Plate Materials
D 348
D 349
D 350
Laminated Tubes
Laminated Round Rods
Flexible Treated Sleeving
D 709 Laminated
Materials
Thermosetting
D 876 Nonrigid Vinyl Chloride
Polymer Tubing
D 1202 Cellulose Acetate Sheet and
D 1675
D 1710
D 2671
D 3394
Film
TFE-Fluorocarbon Tubing
TFE-Fluorocarbon Rod
Heat-Shrinkable Tubing
Insulating Board
Varnishes, Solvents, and Coatings:
D I I5 Varnishes
D I346 Silicone Insulating Varnishes
D 1932 Thermal Endurances of
Flexible Electrical Insulating
Varnishes
~~
ASTM
Desig-
Subject
nation
_________
D 2250 Halogenated Organic Solvents
D 3214 Coating Powders
Rubber and Rubber Products:
D 120 Rubber Insulating Gloves
D 178 Rubber Matting
D 530 Hard Rubber
D 1048 Rubber Insulating Blankets
D 1049 Rubber Insulator Hoods
D I050 Rubber Insulating Line
Hose
D 1051 Rubber Insulating Sleeves
D 3391 Rubber Tape
Filling Compounds:
D 176 Solid Filling and Treating
Compounds
Adhesives:
D 1304 Adhesives Relative to Use
as Electrical Insulation
Wire and Cable:
D 470 Thermosetting Insulated
and Jacketed Wire and
Cable
D 1676 Film-Insulated Magnet
Wire
D 2307 Film-Insulated Magnet
Wire
D 2633 Thermoplastic Insulated
and Jacketed Wire and
Cable
D 3032 Hookup Wire Insulation
D 3353 Fibrous Insulated Magnet
Wire
General:
D 2304
Thermal Evaluation
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in
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56

Wb
Designation: D 150 - 81"'
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Methods for
A-C LOSS CHARACTERISTICS AND PERMITTIVITY
(DIELECTRIC CONSTANT) OF SOLID ELECTRICAL
INSULATING MATERIALS'
This standard is issued under the fixed designation D 150; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
These methods have been approved for use by agencies of the Department of Defense to replace Method 4021 of Federal Test
Method Standard 406 and for listing in the DoD Index of Specifications and Standards.
" Nom-Editorial changes were made throughout in October 1981.
1. scope
1.1 These methods cover the determination
of relative permittivity, dissipation factor, loss
index, power factor, phase angle, and loss angle
of specimens of solid electrical insulating materials
when the standards used are lumped
impedances. The frequency range that can be
covered extends from less than 1 Hz to several
hundred megahertz.
NOTE 1-In common usage, the word relative is
frequently dropped.
1.2 The methods are presented in the following
sequence:
Section
Terminology 3
Significance 4
General Measurement Considerations 5
Electrode Systems 6
Choice of Apparatus and Method for Measuring
Capacitance and A-C Loss 7
Sampling 8
Procedure 9
Report 10
References
Appendix X I-Corrections for Series Inductance and Resistance
and Stray Capacitances
Appendix X2-Effective Area of Guarded Electrode
Appendix X3-Factors Affecting Permittivity and Loss
Characteristics
Appendix XI-Circuit Diagrams of Typical Measuring Circuits
1.3 Since some materials require special
treatment, reference should also be made to the
ASTM methods applicable to the material to
be tested.
2. Applicable Documents
2.1 ASTM Standards:
D 374 Test for Thickness of Solid Electrical
In~ulation~'~
D 1082 Test for Power Factor and Dielectric
Constant of Natural Mica4
D 137 1 Recommended Practice for Cleaning
Plastic Specimens for Insulation Resistance,
Surface Resistance, and Volume Resistivity
Testing3
D 1531 Test for Dielectric Constant and Dissipation
Factor of Polyethylene by Liquid
Displacement Procedure''
D 1711 Definitions of Terms Relating to
Electrical Ins~lation"~
3. Terminology
3.1 capacitance, C-that property of a system
of conductors and dielectrics which permits
the storage of electrically separated charges
when potential differences exist between the
conductors. It is the ratio of a quantity, Q, of
electricity to a potential difference, V. A capacitance
value is always positive. The units are
These methods are under the jurisdiction of ASTM
Committee D-9 on Electrical Insulating Materials and are
the direct responsibility of Subcommittee D09.12 on Electrical
Tests.
Current edition approved Feb. 27, 1981. Published April
1981. Originally published as D 150- 22 T. Last previous
edition D 150 - 80.
' 1983 Annual Book of ASTM Standards, Vol08.01.
1983 Annual Book ofASTM Standards, Vol 10.02.
' 1983 Annual Book ofASTM Standards, Vol 10.01.
57

D 150
farads when the charge is expressed in coulombs
and the potential in volts:
C=Q/V (1)
3.2 dissipation factor (tan 6) (loss tangent),
D-the ratio of the loss index to its relative
permittivity or
D = K”/K!
(2)
It is also the tangent of its loss angle, 6 or the
cotangent of its phase angle, 8.
NOTE a:
D = tan S = cot 0 = XJR,
= G/oC, = I/wC,R, (3)
where:
G = equivalent a-c conductance,
X, = parallel reactance,
R, = equivalent a-c parallel resistance,
C, = parallel capacitance, and
o = 2nrf(sinusoidal wave shape assumed).
The reciprocal of the dissipation factor is the quality
factor, Q, sometimes called the storage factor. The
dissipation factor, D, of the capacitor is the same for
both the series and parallel representations as follows:
D = wR,C, = I/wR,C, (4)
The relationships between series and parallel components
are as follows:
C, = CJ( I + D2) (5)
RJR, = (I + D2)/D2 = 1 + (1/D2) = I + Q’ (6)
NOTE b: Series Representation-While the parallel
representation of an insulating material having a
dielectric loss (Fig. I) is usually the proper representation,
it is always possible and occasionally desirable
to represent a capacitor at a single frequency by a
capacitance, C,, in series with a resistance, R, (Figs.
3 and 4).
3.3 loss angle (phase defect angle), &the
angle whose tangent is the dissipation factor or
arctan K”/K’. It is also the difference between
90” and the phase angle.
NOTE a-The relation of phase angle and loss
angle is shown in Figs. 3 and 4. Loss angle is sometimes
called the phase defect angle.
3.4 loss index, K” (€,”)-the magnitude of
the imaginary part of the relative complex permittivity.
It is the product of the relative permittivity
and dissipation factor.
NOTE a-It
may be expressed as
K” = K’ D
= power loss (E2 X 277 f X E,,-’ (7)
When the units are watts, volts per centimetre,
hertz, and cubic centimetres, eo has the value 8.8542
x 10-l~.
NOTE b-Loss index is the term agreed upon
internationally. In the U.S.A. K” was formerly called
the loss factor.
3.5 phase angle, &the angle whose cotangent
is the dissipation factor, arccot K”/K’. It is
also the angular difference in the phase between
the sinusoidal alternating voltage applied
to a dielectric and the component of the resulting
current having the same frequency as the
voltage.
NOTE-The relation of phase angle and loss angle
is shown in Figs. 2 and 4. Loss angle is sometimes
called the phase defect angle.
3.6 power factor, PF-the ratio of the power
in watts, W, dissipated in a material to the
product of the effective sinusoidal voltage, V,
and current, I, in volt-amperes. It may be expressed
as the cosine of the phase angle t9 (or
the sine of the loss angle 8).
PF = W/ VI = G/ JG2 + (o C,)’
= sin S = cos 0
When the dissipation factor is less than 0.1, the
power factor differs from the dissipation factor
by less than 0.5 %. Their exact relationship may
be found from the following:
PF = D/-]
D = PF/JI - ( PF)~
(9)
3.7 relative permittivity (relative dielectric
constant) (SIC) K’(E,)-the real part of the relative
complex permittivity. It is also the ratio
of the equivalent parallel capacitance, C,, of a
given configuration of electrodes with a material
as a dielectric to the capacitance, C,, of the
same configuration of electrodes with vacuum
(or air for most practical purposes) as the dielectric:
K’ = cp/cL, (iOj
NOTE a-In common usage the word “relative” is
frequently dropped.
NOTE b-Experimentally, vacuum must be replaced
by the material at all points where it makes a
significant change in capacitance. The equivalent
circuit of the dielectric is assumed to consist of C,, a
capacitance in parallel with conductance.
NOTE c-C, is taken to be C, the equivalent
parallel capacitance as shown in Fig. 1.
NOTE d-The series capacitance is larger than the
parallel capacitance by less than 1 % for a dissipation
(8)
58

factor of 0.1, and by less than 0. I % for a dissipation
factor of 0.03. If a measuring circuit yields results in
terms of series components, the parallel capacitance
must be calculated from Eq 5 before the corrections
and permittivity are calculated.
NOTE e-The permittivity of dry air at 23°C and
standard pressure at 101.3 kPa is 1.000536 Its
divergence from unity, K' - 1, is inversely proportional
to absolute temperature and directly proportional
to atmospheric pressure. The increase in permittivity
when the space is saturated with water vapor
at 23°C is 0.00025 (2, 3), and vanes approximately
linearly with temperature expressed in degrees Celsius,
from 10 to 27°C. For partial saturation the
increase is proportional to the relative humidity.
factor, power factor, phase angle, or loss angle.
Factors affecting a-c loss are discussed in Appendix
X3.
4.3 Correlation- When adequate correlating
data are available, dissipation factor or power
factor may be used to indicate the characteristics
of a material in other respects such as
dielectric breakdown, moisture content, degree
of cure, and deterioration from any cause.
However, deterioration due to thermal aging
may not affect dissipation factor unless the
material is subsequently exposed to moisture.
While the initial value of dissipation factor is
3.8 Other definitions may be found in Def- important, the change in dissipation factor with
initions D 17 1 1.
aging may be much more significant.
4. Significance
4.1 Permittivity-Insulating materials are
used in general in two distinct ways, (1) to
support and insulate components of an electrical
network from each other and from ground,
and (2) to function as the dielectric of a capacitor.
For the first use, it is generally desirable to
have the capacitance of the support as small as
possible, consistent with acceptable mechanical,
chemical, and heat-resisting properties. A
low value of permittivity is thus desirable. For
the second use, it is desirable to have a high
value of permittivity, so that the capacitor may
be physically as small as possible. Intermediate
values of permittivity are sometimes used for
grading stresses at the edge or end of a conductor
to minimize a-c corona. Factors affecting
permittivity are discussed in Appendix X3.
4.2 A-C Loss-For both cases (as electrical
insulation and as capacitor dielectric) the a-c
loss generally should be small, both in order to
reduce the heating of the material and to minimize
its effect on the rest of the network. In
high frequency applications, a low value of loss
index is particularly desirable, since for a given
value of loss index, the dielectric loss increases
directly with frequency. In certain dielectric
configurations such as are used in terminating
bushings and cables for test, an increased loss,
usually obtained from increased conductivity,
is sometimes introduced to control the voltage
gradient. In comparisons of materials having
approximately the same permittivity or in the
use of any material under such conditions that
its permittivity remains essentially constant, the
quantity considered may also be dissipation
5. General Measurement Considerations
5.1 Fringing and Stray Capacitance-These
methods are based upon placing a specimen of
material in an electrode system with a vacuum
capacitance that can be either calculated accurately
or determined by a calibration in the
absence of the solid material. The problem of
determining the two capacitance values that are
required, directly or indirectly, to determine K:
is best illustrated by reference to Figs. 5 and 6,
showing two parallel plate electrodes between
which the unknown material is to be placed for
measurement. In addition to the desired direct
interelectrode capacitance, C,f the system as
seen at terminals a-a' includes the following:
C, = fringing or edge capacitance,
C, = capacitance to ground of the outside
face of each electrode,
CL = capacitance between connecting leads,
CL, = capacitance of the leads to ground, and
CL= = capacitance between the leads and the
electrodes.
Only the desired capacitance, Cv, is independent
of the outside environment, all the others
being dependent to 2 degree on the proximity
of other objects. It becomes immediately necessary
to distinguish between two possible measuring
conditions in order to discuss the effects
of the undesired capacitances. If one measuring
electrode is grounded, as is often the case, all
of the capacitances described, except the
ground capacitance of the grounded electrode
The boldface numbers in parentheses refer to the list of
references appended to these methods.
59

D 150
and its lead, are in parallel with the desired C,.
If a guarded test cell is used the capacitance to
ground no longer appears and the capacitance
seen at a-a’ includes C,, Ce, and the lead
capacitances only. The lead capacitance can
usually be made negligibly small. The edge
capacitance, Ce, in air, can be calculated with
reasonable accuracy, but in the presence of the
dielectric the value changes. Empirical corrections
have been derived for various conditions,
and these are given in Table 1 (for the case of
thin electrodes such as. foil). In routine work,
where best accuracy is not required it may be
convenient to use unshielded, two-electrode
systems and make the approximate corrections.
However, for exacting measurements it is necessary
to use guarded electrodes.
5.2 Guarded Electrodes-The fringing and
stray capacitance at the edge of the guarded
electrode is practically eliminated by the addition
of a guard electrode as shown in Fig. 7. If
the test specimen and guard electrode extend
beyond the guarded electrode by at least twice
the thickness of the specimen and the guard
gap is very small, the field distribution in the
guarded area will be identical with that existing
when vacuum is the dielectric, and the ratio of
these two direct capacitances is the permittivity.
Furthermore, the field between the active electrodes
is defined and the vacuum capacitance
can be calculated with the accuracy limited
only by the accuracy with which the dimensions
are known. For these reasons the guarded electrode
(three-terminal) method is to be used as
the referee method unless otherwise agreed
upon. Figure 8 shows a schematic representation
of a completely guarded and shielded electrode
system. Although the guard is commonly
grounded, the arrangement shown permits
grounding either measuring electrode or none
of the electrodes to accommodate the particular
three-terminal measuring system being used. If
the guard is connected to ground, or to a guard
terminal on the measuring circuit, the measured
capacitance is the direct capacitance between
the two measuring electrodes. If, however, one
of the measuring electrodes is grounded, the
capacitance to ground of the ungrounded electrode
and leads is in parallel with the desired
direct capacitance. To eliminate this source of
error, the ungrounded electrode should be surrounded
by a shield connected to guard as
shown in Fig. 8. In addition to guarded meth-
ods, which are not always convenient or practical
and which are limited to frequencies less
than a few megahertz, techniques using special
cells and procedures have been devised that
yield, with two-terminal measurements, accuracies
comparable to those obtained with
guarded measurements. Such methods described
here include shielded micrometer electrodes
(6.3.2) and fluid displacement methods
(6.3.3).
5.3 Geometry of Specimens-For determining
the permittivity and dissipation factor of a
material, sheet specimens are preferable. Cylindrical
specimens can also be used, but generally
with lesser accuracy. The source of the greatest
uncertainty in permittivity is in the determination
of the dimensions of the specimen, and
particularly that of its thickness which should,
therefore, be large enough to allow its measurement
with the required accuracy. The chosen
thickness will depend on the method of producing
the specimen and the likely variation
from point to point. For 1 % accuracy a thickness
of 1.5 mm (0.06 in.) is usually sufficient,
although for greater accuracy it nay be desirable
to use a thicker specimen. Another source
of error, when foil or rigid electrodes are used,
is in the unavoidable gap between the electrodes
and the specimen. For thin specimens
the error in permittivity can be as much as 25
%. A similar error occurs in dissipation factor,
although when foil electrodes are applied with
a grease, the two errors may not have the same
magnitude. For the most accurate measurements
on thin specimens, the fluid displacement
method should be used (6.3.3). This
method reduces or completely eliminates the
need for electrodes on the specimen. The thickness
must be determined by measurements distributed
systematically over the area of the
specimen that is used in the electrical measurement
and should be uniform within +-i % of
the average thickness. If the whole area of the
specimen will be covered by the electrodes, and
if the density of the material is known, the
average thickness can be determined by weighing.
The diameter chosen for the specimen
should be such as to provide a specimen capacitance
that can be measured to the desired
accuracy. With well guarded and screened apparatus
there need be no difficulty in measuring
specimens having capacitances of 10 pF to a
resolution of 1 part in 1000. A thick specimen
60

D 150
of low permittivity may necessitate a diameter
of 100 mm or more to obtain the desired capacitance
accuracy. In the measurement of
small values of dissipation factor, the essential
points are that no appreciable dissipation factor
shall be contributed by the series resistance of
the electrodes and that in the measuring network
no large capacitance shall be connected
in parallel with that of the specimen. The first
of these points favors thick specimens; the second
suggests thin specimens of large area. Micrometex
electrode methods (6.3.2) can be used
to eliminate the effects of series resistance. A
guarded specimen holder (Fig. 8) can be used
to minimize extraneous capacitances.
5.4 Calculation of Vacuum Capacitance-
The practical shapes for which capacitance can
be most accurately calculated are flat parallel
plates and coaxial cylinders, the equations for
which are given in Table 1. These equations
are based on a uniform field between the measuring
electrodes, with no fringing at the edges.
Capacitance calculated on this basis is known
as the direct interelectrode capacitance.
5.5 Edge, Ground, and Gap Corrections-
The equations for calculating edge capacitance,
given in Table 1, are empirical, based on published
work (4) (see 7.5). They are expressed in
terms of picofarads per centimetre of perimeter
and are thus independent of the shape of the
electrodes. It is recognized that they are dimensionally
incorrect, but they are found to give
better approximations to the true edge capacitance
than any other equations that have been
proposed. Ground capacitance cannot be calculated
by any equations presently known.
When measurements must be made that include
capacitance to ground, it is recommended
that the value be determined experimentally
for the particular setup used. This can be done
using a dielectric sample holder or a threeelectrode
method. The difference between the
capacitance measured in the two-terminal arrangement
and the capacitance calculated from
the permittivity and the dimensions of the specimen
is the ground capacitance plus the edge
capacitance. The edge capacitance can be calculated
using one of the equations of Table l.
As long as the same physical arrangement of
leads and electrodes is maintained, the ground
capacitance will remain constant, and the experimentally
determined value can be used as
a correction to subsequently measured values
of capacitance. The effective area of a guarded
electrode is greater than its actual area by
approximately half the area of the guard gap
(5, 6, 18). Thus, the diameter of a circular
electrode, each dimension of a rectangular electrode,
or the length of a cylindrical electrode is
increased by the width of this gap. When the
ratio of gap width, g, to specimen thickness, t,
is appreciable, the increase in the effective dimension
of the guarded electrode is somewhat
less than the gap width. Details of computation
€or this case are given in Appendix X2.
6. Electrode Systems
6.1 Contacting Electrodes-A specimen may
be provided with its own electrodes, of one of
the materials listed below. For two-terminal
measurements the electrodes may extend either
to the edge of the specimen or may be smaller
than the specimen. In the latter case the two
electrodes may be equal or unequal in size. If
equal in size and smaller than the specimen,
the edge of the specimen must extend beyond
the electrodes by at least twice the specimen
thickness. The choice between these three sizes
of electrodes will depend on convenience of
application of the electrodes, and on the type
of measurement adopted. The edge correction
(see Table 1) is smallest for the case of electrodes
extending to the edge of the specimen
and largest for unequal electrodes. When the
electrodes extend to the edge of the specimen,
these edges must be sharp. Such electrodes
must be used, if attached electrodes are used at
all, when a micrometer electrode system is employed.
When equal-size electrodes smaller
than the specimen are used, it is difficult to
center them unless the specimen is translucent
or an aligning fixture is employed. For threeterminal
measurements, the width of the guard
electrode shall be at least twice the thickness of
the specimen (tij 7). The gap width shall be as
small as practical (0.5 mm is possible). For
measurement of dissipation factor at the higher
frequencies, electrodes of this type may be unsatisfactory
because of their series resistance.
Micrometer electrodes should be used for the
measurements.
6.2 Electrod? Materials:
6.2.1 Metal Foil-Lead or tin foil from
0.0075 to 0.025 mm thick applied with a minimum
quantity of refined petrolatum, silicone
grease, silicone oil, or other suitable low-loss
61

D 150
adhesive is generally used as the electrode material.
Aluminum foil has also been used, but
it is not recommended because of its stiffness
and the probability of high contact resistance
due to the oxidized surface. Lead foil also may
give trouble because of its stiffness. Such electrodes
should be applied under a smoothing
pressure sufficient to eliminate all wrinkles and
to work excess adhesive toward the edge of the
foil. One very effective method is to use a
narrow roller, and to roll outward on the surface
until do visible imprint can be made on
the foil. With care the adhesive film can be
reduced to 0.0025 mm. As this film is in series
with the specimen, it will always cause the
measured permittivity to be too low and probably
the dissipation factor to be too high. These
errors usually become excessive for specimens
of thickness less than 0.125 mm. The error in
dissipation factor is negligible for such thin
specimens only when the dissipation factor of
the film is nearly the same as that of the
specimen. When the electrode is to extend to
the edge, it should be made larger than the
specimen and then cut to the edge with a small,
finely ground blade. A guarded and guard
electrode can be made from an electrode that
covers the entire surface, by cutting out a narrow
strip (0.5 mm is possible) by means of a
compass equipped with a narrow cutting edge.
6.2.2 Conducting Paint-Certain types of
high-conductivity silver paints, either airdrying
or low-temperature-baking varieties, are
commercially available for use as electrode material.
They are sufficiently porous to permit
diffusion of moisture through them and thereby
allow the test specimen to condition after application
of the electrodes. This is particularly
useful in studying humidity effects. The paint
has the disadvantage of not being ready for use
immediately after application. It usually requires
an overnight air-drying or iow-temperature
baking to remove all traces of solvent,
which otherwise may increase both permittivity
and dissipation factor. It also may not be easy
to obtain sharply defined electrode areas when
the paint is brushed on, but this limitation
usually can be overcome by spraying the paint
and employing either clamp-on or pressuresensitive
masks. The conductivity of silver paint
electrodes may be low enough to give trouble
at the higher frequencies. It is essential that the
solvent of the paint does not affect the specimen
permanently.
6.2.3 Fired- On Silver- Fired-on silver electrodes
are suitable only for glass and other
ceramics that can withstand, without change, a
firing temperature of about 350°C. Its high
conductivity makes such an electrode material
satisfactory for use on low-loss materials such
as fused silica, even at the highest frequencies,
and its ability to conform to a rough surface
makes it satisfactory for use with high-permittivity
materials, such as the titanates.
6.2.4 Sprayed Metal-A low-melting-point
metal applied with a spray gun provides a
spongy film for use as electrode material which,
because of its grainy structure, has roughly the
same electrical conductivity and the same moisture
porosity as conducting paints. Suitable
masks must be used to obtain sharp edges. It
conforms readily to a rough surface, such as
cloth, but does not penetrate very small holes
in a thin film and produce short circuits. Its
adhesion to some surfaces is poor, especially
after exposure to high humidity or water immersion.
Advantages over conducting paint are
freedom from effects of solvents, and readiness
for use immediately after application.
6.2.5 Evaporated Metal-Evaporated metal
used as an electrode material may have inadequate
conductivity because of its extreme thinness,
and must be backed with electroplated
copper or sheet metal. Its adhesion is adequate,
and by itself it is sufficiently porous to moisture.
The necessity for using a vacuum system in
evaporating the metal is a disadvantage.
6.2.6 Liquid Metal-Mercury electrodes
may be used by floating the specimen on a pool
of mercury and using confining rings with
sharp edges for retaining the mercury for the
guarded and guard electrodes, as shown in Fig.
9. A more convenient arrangement, when a
considerable number of specimens must be
tested, is the test fiiture shown in Fig. I of
Method D 1082. There is some health hazard
present due to the toxicity of mercury vapor,
especially at elevated temperatures, and suitable
precautions should be taken during use. In
measuring low-loss materials in the form of
thin films such as mica splittings, contamination
of the mercury may introduce considerable
error, and it may be necessary to use clean
mercury for each test. Wood's metal or other
low-melting alloy can be used in a similar
manner with a somewhat reduced health haz-
62

D 150
ard. Mercury metal vapor poisoning has long
been recognized as a hazard in industry. The
boiling point of mercury is 356.6OC. However,
the concentration of mercury vapor over spills
from broken thermometers, barometers, or
other instruments using mercury can easily exceed
the maximum standards as set forth by
the American Conference of Governmental Industrial
Hygienists (ACGIH).' Mercury, being
a liquid and quite heavy, will disintegrate into
small droplets and seep into cracks and crevices
in the floor. The increased area of exposure
adds significantly to the mercury vapor concentration
in air. Mercury vapor concentration is
easily monitored using commercially available
sniffers. Spot checks regularly and thorough
checks should be made after spills and around
operations where mercury is exposed to the
atmosphere. Emergency spill kits are also available
should the airborne concentration exceed
the standard.
6.2.7 Rigid Metal-For smooth, thick, or
slightly compressible specimens, rigid electrodes
under high pressure can sometimes be
used, especially for routine work. Electrodes 10
mm in diameter, under a pressure of 18.0 MPa
have been found useful for measurements on
plastic materials, even those as thin as 0.025
mm. Electrodes 50 mm in diameter, under pressure,
have also been used successfully for
thicker materials. However, it is difficult to
avoid an air film when using solid electrodes,
and the effect of such a film becomes greater as
the permittivity of the material being tested
increases and its thickness decreases. The uncertainty
in the determination of thickness also
increases as the thickness decreases. The dimensions
of a specimen may continue to
change for as long as 24 h after the application
of pressure.
6.2.8 Water-Water can be used as one electrode
€or testing insulated wire and cable when
the measurements are made at low frequency
(up to 1000 Hz, approximately). Care must be
taken to ensure that electrical leakage at the
ends of the specimen is negligible.
6.3 Non- Contacting Electrodes:
6.3.1 Fixed Electrodes-Specimens of sufficiently
low surface conductivity can be measured
without applied electrodes by inserting
them in a prefabricated electrode system, in
which there is an intentional airgap on one or
both sides of the specimen. The electrode sys-
tem should be rigidly assembled and should
preferably include a guard electrode. For the
same accuracy, a more accurate determination
of the electrode spacing and the thickness of
the specimen is required than if direct contact
electrodes are used. However, if the electrode
system is filled with a liquid, these limitations
may be removed (see 6.3.3).
6.3.2 Micrometer Electrodes-The micrometer-electrode
system, as shown in Fig. 10, was
developed (8) to eliminate the errors caused by
the series inductance and resistance of the connecting
leads and of the measuring capacitor at
high frequencies. A built-in vernier capacitor is
also provided for use in the susceptance variation
method. It accomplishes this by maintaining
these inductances and resistances relatively
constant, regardless of whether the test specimen
is in or out of the circuit. The specimen,
which is either the same size as, or smaller than,
the electrodes, is clamped between the electrodes.
Unless the surfaces of the specimen are
lapped or ground very flat, metal foil or its
equivalent must be applied to the specimen
before it is placed in the electrode system. If
electrodes are applied, they also must be
smooth and flat. Upon removal of the specimen,
the electrode system can be made to have
the same capacitance by moving the micrometer
electrodes closer together. When the micrometer-electrode
system is carefully calibrated
for capacitance changes, its use eliminates
the corrections for edge capacitance,
ground capacitance, and connection capacitance.
In this respect it is advantageous to use
it over the entire frequency range. A disadvantage
is that the capacitance calibration is not as
accurate as that of a conventional multiplate
variable capacitor, and also it is not direct
reading. At frequencies below 1 MHz, where
the effect of series inductance and resistance in
the ieads is negligible, the capacitance calibration
of the micrometer electrodes can be replaced
by that of a standard capacitor, either
in parallel with the micrometer-electrode system
or in the adjacent capacitance arm of the
bridge. The change in capacitance with the
specimen in and out is measured in terms of
this capacitor. A source of minor error in
micrometer-electrode system is that the edge
capacitance of the electrodes, which is included
'Bldg. D-5, 6500 Glenway Ave. B, Cincinnati, Ohio
4521 1.
63

D 150
in their calibration, is slightly changed by the
presence of a dielectric having the same diameter
as the electrodes. This error can be practically
eliminated by making the diameter of the
specimen less than that of the electrodes by
twice its thickness (3). When no electrodes are
attached to the specimen, surface conductivity
may cause serious errors in dissipation factor
measurements of low loss material. Unless materials
are to be tested "as received" they should
be cleaned and dried in accordance with Recommended
Practice D 1371 and measured in a
dry atmosphere. When the bridge used for
measurement has a guard circuit, it is advantageous
to use guarded micrometer electrodes.
The effects of fringing, etc., are almost completely
eliminated. When the electrodes and
holder are well made, no capacitance calibration
is necessary as the capacitance can be
calculated from the electrode spacing and the
diameter. The micrometer itself will require
calibration, however. It is not practicable to use
electrodes on the specimen when using guarded
micrometer electrodes unless the specimen is
smaller in diameter than the guarded electrode.
6.3.3 Fluid Displacement Methods-When
the immersion medium is a liquid, and no
guard is used, the parallel-plate system preferably
shall be constructed so that the insulated
high potential plate is supported between, parallel
to, and equidistant from two parallel lowpotential
or grounded plates, the latter being
the opposite inside walls of the test cell designed
to hold the liquid. This construction
makes the electrode system essentially selfshielding,
but normally requires duplicate test
specimens. Provision must be made for precise
temperature measurement of the liquid (9,lO).
Cells should be constructed of brass and gold
plated. The high-potential electrode shall be
removable for cleaning. The faces must be as
nearly optically flat and piane paraiiei as possible.
A suitable liquid cell for measurements
up to 1 MHz is shown in Fig. 1 of Method
D 1531. Changes in the dimensions of this cell
may be made to provide for testing sheet specimens
of various thicknesses or sizes, but, such
changes should not reduce the capacitance of
the cell filled with the standard liquid to less
than 100 pF. For measurements at frequencies
from 1 to about 50 MHz, the cell dimensions
must be greatly reduced, and the leads must be
as short and direct as possible. The capacitance
of the cell with liquid shall not exceed 30 or 40
pF for measurements at 50 MHz. Experience
has shown that a capacitance of 10 pF can be
used up to 100 MHz without loss of accuracy.
Guarded parallel-plate electrodes have the advantage
that single specimens can be measured
with full accuracy. Also a prior knowledge of
the permittivity of the liquid is not required as
it can be measured directly (11). If the cell is
constructed with a micrometer electrode, specimens
having widely different thicknesses can
be measured with high accuracy since the electrodes
can be adjusted to a spacing only slightly
greater than the thickness of the specimen. If
the permittivity of the fluid approximates that
of the specimen the effect of errors in determination
of specimen thicknesses are minimized.
The use of a nearly matching liquid and a
micrometer cell permits high accuracy in measuring
even very thin film.
All necessity for determining specimen thickness
and electrode spacing is eliminated if successive
measurements are made in two fluids of
known permittivity (12,13,18). This method is
not restricted to any frequency range; however,
it is best to limit use of liquid immersion methods
to frequencies for which the dissipation
factor of the liquid is less than 0.01 (preferably
less than O.OOO1 for low-loss specimens).
When using the two-fluid method it is important
that both measurements be made on
the same area of the specimen as the thickness
may not be the same at all points. To ensure
that the same area is tested both times and to
facilitate the handling of thin films, specimen
holders are convenient. The holder can be a U-
shaped piece that will slide into grooves in the
electrode cell. It is also necessary to control the
temperature to at least 0.1OC. The cell may be
provided with cooling coils for this purpose
(13).
7. Choice of Apparatus and Methods for Measuring
Capacitance and A-C Loss
7.1 Frequency Range-Methods for measuring
capacitance and a-c loss can be divided into
three groups: null methods, resonance methods,
and deflection methods. The choice of a
method for any particular case will depend
primarily on the operating frequency. The resistive-
or inductive-ratio-arm capacitance
bridge in its various forms can be used over the
frequency range from less than 1 Hz to a few
64

D 150
megahertz. For frequencies below 1 Hz, special
methods and instruments are required. Parallel-T
networks are used at the higher frequencies
from 500 kHz to 30 MHz, since they partake
of some of the characteristics of resonant
circuits. Resonance methods are used over a
frequency range from 50 kHz to several
hundred megahertz. The deflection method,
using commercial indicating meters, is employed
only at power-line frequencies from 25
to 60 Hz, where the higher voltages required
can easily be obtained.
7.2 Direct and Substitution Methods-In any
direct method, the values of capacitance and a-
c loss are in terms of all the circuit elements
used in the method, and are therefore subject
to all their errors. Much greater accuracy can
be obtained by a substitution method in which
readings are taken with the unknown capacitor
both connected and disconnected. The errors
in those circuit elements that are unchanged
are in general eliminated; however, a connectioil
error remains (Note 2).
7.3 Two- and Three-Terminal Measurements-The
choice between three-terminal and
two-terminal measurements is generally one
between accuracy and convenience. The use of
a guard electrode on the dielectric specimen
nearly eliminates the effect of edge and ground
capacitance, as explained in 5.2. The provision
of a guard terminal eliminates some of the
errors introduced by the circuit elements. On
the other hand, the extra circuit elements and
shielding usually required to provide the guard
terminal add considerably to the size of the
measuring equipment, and the number of adjustments
required to obtain the final result
may be increased many times. Guard circuits
for resistive-ratio-arm capacitance bridges are
rarely used at frequencies above 1 MHz. Inductive-ratio-arm
bridges provide a guard terminai
without requiring extra circuits or adjustments.
Parallel-T networks and resonant
circuits are not provided with guard circuits. In
the deflection method a guard can be provided
merely by extra shielding. The use of a twoterminal
micrometer-electrode system provides
many of the advantages of three-terminal measurements
by nearly eliminating the effect of
edge and ground capacitances but may increase
the number of observations or balancing adjustments.
Its use also eliminates the errors
caused by series inductance and resistance in
the connecting leads at the higher frequencies.
It can be used over the entire frequency range
to several hundred megahertz. When a guard
is used, the possibility exists that the measured
dissipation factor may be less than the true
value. This is caused by resistance in the guard
circuit at points between the guard point of the
measuring circuit and the guard electrode. This
may arise from high contact resistance, lead
resistance, or from high resistance in the guard
electrode itself. In extreme cases the dissipation
factor may appear to be negative. This condition
is most likely to exist when the dissipation
factor without the guard is higher than normal
due to surface leakage. Any point capacitively
coupled to the measuring electrodes and resistively
coupled to the guard point can be a
source of difficulty. The common guard resistance
produces an equivalent negative dissipation
factor proportional to chc&, where ch
and Ct are guard-to-electrode capacitances and
Rg is the guard resistance (14).
7.4 Fluid Displacement Methods-The fluid
displacement method may be employed using
either three-terminal or self-shielded, two-terminal
cells. With the three-terminal cell the
permittivity of the fluids used may be determined
directly. The self-shielded, two-terminal
cell provides many of the advantages of the
three-terminal cell by nearly eliminating the
effects of edge and grcund capacitance, and it
may be used with measuring circuits having no
provision for a gcard. If it is equipped with an
integral micrometer electrode, the effects on the
capacitance of series inductance in the connective
leads at the higher frequencies may be
eliminated.
7.5 Accuracy-The methods outlined in 7.1
contemplate an accuracy in the determination
of permittivity off 1 9% and of dissipation factor
of f (5 '36 + 0.0005). These accuracies depend
upon at ieast three factors: the accuracy of the
observations for capacitance and dissipation
factor, the accuracy of the corrections to these
quantities caused by the electrode arrangement
used, and the accuracy of the calculation of the
direct interelectrode vacuum capacitance. Under
favorable conditions and at the lower fre-
quencies, capacitance can be measured with an
accuracy of f (0.1 5% + 0.02 pF) and dissipation
factor with an accuracy of k (2 % + 0.00005).
At the higher frequencies these limits may increase
for capacitance to k (0.5 % + 0.1 pF)
65

D150
and for dissipation factor to f (2 % + 0.0002).
Measurements of dielectric specimens provided
with a guard electrode are subject only to the
error in capacitance and in the calculation of
the direct interelectrode vacuum capacitance.
The error caused by too wide a gap between
the guarded and the guard electrodes will generally
amount to several tenths percent, and the
correction can be calculated to a few percent.
The error in measuring the thickness of the
specimen can amount to a few tenths percent
for an average thickness of 2 mm, on the assumption
that it can be measured to k0.005
mm. The diameter of a circular specimen can
be measured to an accuracy of kO.l%, but
enters as the square. Combining these errors,
the direct interelectrode vacuum capacitance
can be determined to an accuracy of k0.5 %.
Specimens with contact electrodes, measured
with micrometer electrodes, have no corrections
other than that for direct interelectrode capacitance,
provided they are sufficiently smaller in
diameter than the micrometer electrodes. When
two-terminal specimens are measured in any
other manner, the calculation of edge capacitance
and determination of ground capacitance
will involve considerable error, since each may
be from 2 to 40 % of the specimen capacitance.
With the present knowledge of these capacitances,
there may be a 10 9% error in calculating
the edge capacitance and a 25 9% error in evaluating
the ground capacitance. Hence the total
error involved may be from several tenths to
10 % or more. However, when neither electrode
is grounded, the ground capacitance error is
minimized (5.1). With micrometer electrodes,
it is possible to measure dissipation factor of
the order of 0.03 to within k0.0003 and dissipation
factor of the order of 0.0002 to within
&0.00005, of the true values. The range of
dissipation factor is normally 0.0001 to 0.1 but
may be extended above 0.1. Between 10 and 20
MHz it is possible to detect a dissipation factor
of 0.00002. Permittivity from 2 to 5 may be
determined to k 2 9%. The accuracy is limited by
the accuracy of the measurements required in
the calculation of direct interelectrode vacuum
capacitance and by errors in the micrometerelectrode
system.
8. Sampling
8.1 See materials specifications for instructions
on sampling.
9. Procedure
9.1 Preparation of Specimens:
9.1.1 General-Cut or mold the test specimens
to a suitable shape and thickness determined
by the material specification being followed
or by the accuracy of measurement required,
the test method, and the frequency at
which the measurements are to be made. Measure
the thickness in accordance with the standard
method required by the material being
tested. If there is no standard for a particular
material, then measure thickness in accordance
with Methods D 374. The actual points of measurement
shall be uniformly distributed over
the area to be covered by the measuring electrodes.
Apply suitable measuring electrodes to
the specimens (Section 6) (unless the fluid displacement
method will be used), the choice as
to size and number depending mainly on
whether three-terminal or two-terminal measurements
are to be made and, if the latter,
whether or not a micrometer-electrode system
will be used (6.3). The material chosen for the
specimen electrodes will depend both on convenience
of application and on whether or not
the specimen must be conditioned at high temperature
and high relative humidity (Section
6). Obtain the dimensions of the electrodes (of
the smaller if they are unequal) preferably by
a traveling microscope, or by measuring with
a steel scale graduated to 0.25 mm and a microscope
of sufficient power to allow the scale
to be read to the nearest 0.05 mm. Measure the
diameter of a circular electrode, or the dimensions
of a rectangular electrode, at several
points to obtain an average.
9.1.2 Micrometer Electrodes-The area of
the specimen may be equal to or less than the
area of the electrodes, but no part of the specimen
shall extend beyond the electrode edges.
The edges of the specimens sha!! be rrnooth
and perpendicular to the plane of the sheet and
shall also be sharply defined so that the dimensions
in the plane of the sheet may be determined
to the nearest 0.025 mm. The thickness
may have any value from 0.025 mm or less to
about 6 mm or greater, depending upon the
maximum usable plate spacing of the parallelplate
electrode system. ‘The specimens shall be
as flat and uniform in thickness as possible,
and free of voids, inclusions of foreign matter,
wrinkles, and other defects. It has been found
that very thin specimens may be tested more
66

D 150
conveniently and accurately by using a composite
of several or a large number of thicknesses.
The average thickness of each specimen
shall be determined as nearly as possible to
within k0.0025 mm. In certain cases, notably
for thin films and the like but usually excluding
porous materials, it may be preferable to determine
the average thickness by calculation from
the known or measured density of the material,
the area of the specimen face, and the mass of
the specimen (or specimens, when tested in
multiple thicknesses of the sheet), obtained by
accurate weighing on an analytical balance.
9.1.3 Fluid Displacement-When the immersion
medium is a liquid, the specimen may be
larger than the electrodes if the permittivity of
the standard liquid is within about 1 % of that
of the specimen (see Method D 1531). Also,
duplicate specimens will normally be required
for a cell of the type described in 6.3.3, although
it is possible to test a single specimen at a time
in such cells. In any case, the thickness of the
specimen preferably should not be less than
about 80 % of the electrode spacing, this being
particularly true when the dissipation factor of
the material being tested is less than about
0.00 1.
9.1.4 Cleaning-Since it has been found that
in the case of certain materials when tested
without electrodes the results are affected erratically
by the presence of conducting contaminants
on the surfaces of the specimens, clean
the test specimens by a suitable solvent or other
means (as prescribed in the material specification)
and allow to dry thoroughly before test
(15). This is particularly important when tests
are to be made in air at low frequencies (60 to
10 000 Hz), but is less important for measurements
at radio frequencies. Cleaning of specimens
will also reduce the tendency to contaminate
the immersion medium in the case of tests
performed wing a liquid medium. Use Recommended
Practice D 1371 as a guide to the
choice of suitable cleaning procedures. After
cleaning, handle the specimens only with
tweezers and store in individual envelopes to
preclude further contamination before testing.
9.2 Measurement-Place the test specimen
with its attached electrodes in a suitable measuring
cell, and measure its capacitance and a-
c loss by a method having the required sensitivity
and accuracy. For routine work when the
highest accuracy is not required, or when nei-
ther terminal of the specimen is grounded, it is
not necessary to place the solid specimen in a
test cell.
NOTE 2-The method used to connect the specimen
to the measuring circuit is very important, especially
for two-terminal measurements. The connection
method by critical spacing, formerly recommended
in Methods D 150 for parallel substitution
measurements can cause a negative error of 0.5 pF.
A similar error occurs when two-terminal specimens
are measured in a cell used as a guard. Since no
method for eliminating this error is presently known,
when an error of this magnitude must be avoided, an
alternative method must be used, that is, micrometer
electroaes, fluid immersion cell, or three-terminal
specimen with guarded leads.
NOTE 3-Detailed instructions for making the
measurements needed to obtain capacitance and dissipation
factor and for making any necessary corrections
due to the measuring circuit are given in the
instruction books supplied with commercial equipment.
The following paragraphs are intended to furnish
the additional instruction required.
9.2.1 Fixed Electrodes-Adjust the plate
spacing accurately to a value suitable for the
specimen to be tested. For low-loss materials in
particular, the plate spacing and specimen
thickness should be such that the specimen will
occupy not less than about 80 % of the electrode
gap. For tests in air, plate spacings less than
about 0.1 mm are not recommended. When the
electrode spacing is not adjustable to a suitable
value, specimens of the proper thickness must
be prepared. Measure the capacitance and dissipation
factor of the cell, and then carefully
insert and center the specimen between the
electrodes of the micrometer electrodes or test
cell. Repeat the measurements. For maximum
accuracy determine AC and AD directly, if
possible with the measuring equipment used.
Record the test temperature.
9.2.2 Micrometer Electrodes-Micrometer
electrodes are commonly used with the electrodes
making contact with the specimen or its
attached electrodes. To make a measurement
first clamp the specimen between the micrometer
electrodes, and balance or tune the network
used for measurement. Then remove the specimen,
and reset the electrodes to restore the
total capacitance in the circuit or bridge arm to
its original value by moving the micrometer
electrodes closer together.
9.2.3 Fluid Displacement Methods-When a
single liquid is used, fill the cell and measure
the capacitance and dissipation factor. Carefully
insert the specimen (or specimens if the
67

two-specimen cell is used) and center it. Repeat
the measurements. For maximum accuracy determine
AC and AD directly, if possible with
the measuring equipment used. Record the test
temperature to the nearest 0.0 1 "C. Remove
specimens promptly from the liquid to prevent
swelling, and refill the cell to the proper level
before proceeding to test additional specimens.
Equations for calculation of results are given in
Table 3. Method D 1531 describes in detail the
application of this method to the measurement
of polyethylene. When a guarded cell, preferably
with micrometer electrode, is available,
greater accuracy can be obtained by measuring
the specimen in two fluids. This method also
eliminates the need to know the specimen dimensions.
The procedure is the same as before
except for the use of two fluids having different
permittivities (12, 13, 18). It is convenient to
use air as the first fluid since this avoids the
necessity for cleaning the specimen between
measurements. The use of a guarded cell permits
the determination of the permittivity of
the liquid or liquids used (3.2). When either the
one- or two-fluid method is used, greatest accuracy
is possible when the permittivity of one
liquid most nearly matches that of the specimen.
NOTE &--When the two-fluid method is used, the
dissipation factor can be obtained from either set of
readings (most accurately from the set with the higher
Kr?.
9.3 Calculation of Permittivity, Dissipation
Factor, and Loss Index-The measuring circuits
used will give, for the specimen being
measured at a given frequency, a value of
capacitance and of a-c loss expressed as Q,
dissipation factor, or series or parallel resistance.
When the permittivity is to be calculated
from the observed capacitance values, these
values must be converted to parallel capacitance,
if not so expressed, by the use of Ey 5.
The equations given in Table 2 can be used in
calculating the capacitance of the specimen
when micrometer electrodes are used. The
equations given in Table 3 for the different
electrode systems can be used in calculating
permittivity and dissipation factor. When the
parallel substitution method is used, the dissipation
factor readings must be multiplied by
the ratio of the total circuit capacitance to the
capacitance of the specimen or cell. Q and
series or parallel resistance also require calculation
from the observed values. Permittivity is:
Kx) = cp/ct, (1 1)
Expressions for the vacuum capacitance (5.4)
for flat parallel plates and coaxial cylinders are
given in Table 1. When the a-c loss is expressed
as series resistance or parallel resistance or
conductance, the dissipation factor may be calculated
using the relations given in Eqs 3 and
4. Loss index is the product of dissipation factor
and permittivity 3.4.
9.4 Corrections-The leads used to connect
the specimen to the measuring circuit have both
inductance and resistance which, at high frequencies,
increase the measured capacitance
and dissipation factor. When extra capacitances
have been included in the measurements, such
as edge capacitance, and ground capacitance,
which may occur in two-terminal measurements,
the observed parallel capacitance will
be increased and the observed dissipation factor
will be decreased. Corrections for these effects
are given in Appendix X1 and Table 1.
10. Report
10.1 The report shall include the following:
10.1.1 Description of the material tested,
that is, the name, grade, color, manufacturer,
and other pertinent data,
10.1.2 Shape and dimensions of the test
specimen,
10.1.3 Type and dimensions of the electrodes
and measuring cell,
10.1.4 Conditioning of the specimen, and
test conditions,
10.1.5 Method of measurement and measurement
circuit,
10.1.6 Applied voltage, effective voltage gradient,
and frequency, and
10.1.7 Values of parallel capacitance, dissipation
factor or power factor, permittivity, loss
index, and estimated accuracy.
11. Precision and Accuracy
11.1 The precision and accuracy of this test
method is currently in preparation.
68

REFERENCES
(1) Hector, L. G. and Woernle , D. L., “The Dielectric
Constants of Ei ht dases’*, Physical Review,
PHRVA, Vol69, % ebruary 1964, pp. 101-
105.
(2) Ford, L. H., “The Effect of Humidity on the
Calibration of Precision Air Ca acitors”, Proceedin
s, PIEEA, Institution of I! lectrical En i-
neers [London), Vol 96, Part 111, January 19 9,
(3) E:se!!-I!pand Freome, K. O., “Dielectric Constant
and Refractive Index of Air and Its Princi
a1 Constituents at 24,000 Mc/s”, Nature,
&RWA, Vol 167, March 31,‘~. 512.
(4) Scott, A. H., and Curtis, H. L., Edge Correction
in the Determination of Dielectric Constant,”
Journal of Research, JNBAA, Nat. Bureau
Standards, Vol22, June, 1939, pp. 747-775.
(5) Amey, W. G., and Hambur er, F., Jr., “A
Method for Evaluating the Sur P ace and Volume
Resistance Characteristics of Solid Dielectric
Materials,” Proceedings, ASTEA, Am. SOC.
Testin Mats., Vol 49, 1949, pp. 1079-1091.
(6) Field, e;. F., “Errors Occurring in the Measurement
of Dielectric Constant,” Proceedin s, AS-
TEA, Am. SOC. Testing Mats., Vol54, 1 B 54, pp.
456-478.
(7) Moon, C., and Sparks, C. M., “Standards for
Low Values of Direct Ca acitance,” Journal of
Research, JNBAA, Nat. I! ureau Standards, Vol
41, November, 1948, pp. 497-507.
(8) Hartshorn, L., and Ward, W. H., “The Measurement
of the Permittivity and Power Factor
of Dielectrics at Frequencies from lo4 to 10’
Cycles per Second,” Proceedin s, PIEEA, Institution
of Electrical En ineers ( f ondon), Vol79,
1936, pp. 597-609; or P roceedings of the Wireless
Section, Zbid., Vol 12, March, 1937, p . 6-18.
(9) Coutlee, K. G., “Liquid Dis lacement .1p est Cell
for Dielectric Constant an B Dissipation Factor
to 100 Mc,” presented at Conference on
“P E ectrical Insulation (NRC), October, 1959, and
reviewed in Insulation, INULA, November,
9
1959, p. 26.
(IO) Ma ott, A. A., and Smith, E. R., “Table of
Die 7 ectric Constants of Pure Liquids,” NBS
Circular No. 514, 1951.
(11) Hartshorn, L., Parry, J. V. L., and Essen, L.,
“The Measurement of the Dielectric Constant
of Standard Liquids,” Proceedings, PPSBA,
Physical SOC. (London), Vol 68B, July, 1955,
422-446.
(12) l?. arris, ’ W. P., and Scott, A. H., “Precise Measurement
of the Dielectric Constant by the Twofluid
Technique,” 1962 Annual Report, Conference
on Electrical Insulation, NAS-NAC, 5 1.
(13) Endicott, H. S., and McGowan, E. J., “keasurement
of Permittivity and Dissi ation Factor
Without Attached Electrodes,” P 960 Annual
Report, Conference on Electrical Insulation,
NAS-NAC.
(14) Harris, W. P., “Apparent Negative Im edances
and their Effect on Three-terminal 8 ielectric
Loss Measurements,” 1965 Annual Report,
Conference on Electrical Insulation, NAS-NRC
Publication 1356.
(15) Field, R. F., “The Formation of Ionized Water
Films on Dielectrics Under Conditions of Hi h
Humidity,” Journal Ap lied Physics, JAPIA, ? 01
17, May, 1946, p. 31l325.
(16) Lauritzen, J. l, “The Effective Area of a
Guarded Electrode,” 1963 Annual Re ort, Conference
on Electrical Insulation, 8 AS-NRC
Publication 1141.
tober, 1937, p .493-512.
(18) Endicott, H. K., “Guard Gap Corrections for
Guarded-Electrical Measurements and Exact
Equations for the Two-Fluid Method of Measurin
Permittivit and Loss,” Journal of Testing
and $valuation, fTEVA, Vol 4, No. 3, May
1976, pp. 188-195.
69

:;-
TABLE 1 Calculations of Vacuum Capacitance and Edge Corrections (see 7.5)
Type of Electrode
~ $ :
Correction
~
for
~
Stray Field
~
at an Edge,
~
pF
~ ~
c, = 0
Disk electrodes with guard-ring:
Disk electrodes without guard-ring:
Diameter of the electrodes = diameter
of the specimen:
mi
a
*A
Equal electrodes smaller than the
specimen:
a
Unequal electrodes:
d'
C,. = 0.0069541 -!- t
where a e t, C, = (0.0087 - 0.00252 In t)P
C, = (0.0019 IC: - 0.00252 In t + 0.0068)P
where: IC: = an approximate value
of the specimen permittivity,
and
a cb: t.
Cylindrical electrodes with guard-ring:
1
c,, =
t$m$
I , r
. . .,
0.055632 ([I + B* g)
dz
In -
di
C, = (0.0041 IC: - 0.00334 ln t + 0.0122)P
where: K; = an approximate value
of the specimen permittivity,
and
a t.
c, = 0
Cylindrical electrodes without guard-ring:
t
-L
3m
t Ill
--r
* See Appendix X2 for corrections to guard gap.
Parallel Capacitance
0.055632 I! t I
c,, =
If -

TABLE 3 Calculation of Permittivity and Dissipation Factor, Noncontacting Electrodes
Permittivity Dissipation Factor Definitions of Symbols
Micrometer electrodes in air (with guard ring):
AC = capacitance change when specimen is inserted (+ when capaci-
1
D, = D, +
tance increases),
MK,'AD
C1 = capacitance with specimen in place,
AD = increase in dissipation factor when specimen is inserted,
D, = dissipation factor with specimen in place,
Dr = dissipation factor, fluid,
or, if to is adjusted to a new value, ti, such that
to = parallel-plate spacing,
AC-0
t = average thickness of specimen,
t
M = to/t - 1,
Kr =
t - (to- to')
Cf = K;C" capacitance with fluid alone,
= 0.0088542 (dimensions in nun),
Plane electrodes-fluid displacement:
A = area of the electrodes, mmz (the smaller if the two are unequal),
I Kr'
D,= D,+ADM
K; = permittivity of fluid at test temperature (= 1.00066 for air at
Kr =-
I +
23"C, 50 9% RH),
D:
C, = vacuum capacitance of area considered (e, Alto, pF),
= OD of inner electrode,
dl = IDofspecimen,
d2 = ODofspecimen,and
When the dissipation factor of the specimen is less than about 0.1, the following equations
d3 = ID of outer electrode, a
can be used:
1-
K~C,, + Ac 7
Cylindrical electrodes (with guard rings)-fluid displacement.
Ki
K/ =
I--- AC lOgd31do
CI lOgdz/dl
D,= D,+M~AD
Kf
NOTE 1-C and D in these equations are the values for the cell and may
require calculations from the readings of the measuring circuit (as
when using parallel substitution). Refer to Note 10.
3
0
A
8
Two-fluid method-plane electrodes (with guard ring):
NOTE 2-In the equation for the two-fluid method, subscripts 1 and 2
refer to the first and second fluids, respectively.
NOTE 3-Values of C in the two-fluid equations are the equivalent series
values.
Az = effective area of guarded electrode with specimen in liquid,
= (d + 8,)' 1r/4 (See Appendix X2 for corrections to guard gap).

vwcp
FIG. 1 Parallel Circuit
FIG. 4 Vector Diagram for Parallel Circuit
Rs I
FIG. 2 Series Circuit
FIG. 5 Flux Lines Between Electrodes
FIG. 3 Vector Diagram for Series Circuit
GUARDED
GUARD ELECTRODE
ELECTRODE
Guar
Elect
FIG. 6 Stray Capacitances
Guarded
Electrode
UNGUARDED
ELECTRODE
FIG. 7 Guarded PardleCPlate Electrode System
Unguarded
Electrode
FIG. 8 Three-Terminal Cell for Solids
FIG. 9 Guarded Specimen with Mercury Electrodes
72

icrometer Screw
Grounded Terminals
FIG. 10 Micrometer-Electrode System
APPENDIXES
XI. CORRECTIONS FOR SERIES INDUCTANCE AND RESISTANCE AND STRAY
CAPACITANCES
XI.l The increase in ca acitance due to the inductance
of the leads and o P dissipation factor due to
the resistance of the leads is calculated as follows:
AC = w2L,C2
AD = RwC, (12)
I
where:
C, = true capacitance of the capacitor being measured,
L, = series inductance of the leads,
R, = series resistance of the leads, and
w = 2n times the frequency, Hz.
NOTE XI-L and R can be calculated for the leads
used, from measurements of a physically small capacitor,
made both at the measuring equipment terminals
and at the far end of the leads. C is the
ca acitance measured at the terminals, AC is the
di R erence between the two capacitance readings, and
R is calculated from the measured values of C and
D.
X1.2 While it is desirable to have these leads as
short as ossible, it is difficult to reduce their inductance
an B resistance below 0.1 pH and 0.05 at 1
MHz. The high-frequency resistance increases with
the s uare root of the frequency. Hence these correc-
tions 5 ewme increasingly important above 1 MHz.
When extra capacitances have been included in the
measurements, such as ed e capacitance, C,, and
ground capacitance. Cg, w &1 ich may occur in twoterminal
measurements. the observed parallel capac-
itance will be increased and the observed dissipation
factor will be decreased. Designating these observed
quantities by the subscript, m, the corrected values
are calculated as follows:
Cp = C m - (Ce + Cs)
D = CmDm/Cp
= CmDm/ [Cm - (ce + Cg)]
Xl.3 The expression for dissipation factor assumes
that the extra ca acitances are free from loss.
This is essentially true P or ground capacitance except
at low fre uencies, and also for edge capacitance
when the e 9 ectrodes extend to the edge of the specimen,
since nearly all of the flux lines are in air. The
permittivity and loss index are calculated as follows:
K'
Cp/Cu = [C, - (Ce + Cg)]/Cu
K" = CmDm/Cu
X1.4 When one or both of the electrodes are
smaller than the s ecimen, the edge capacitance has
two components. %e capacitance associated with the
flux lines that pass through the surrounding dielectric
has a dissipation factor which, for isotro ic materials,
is the same as that of the body of the die P ectric. There
is no loss in the capacitance associated with the flux
lines through the air. Since it is not practicable to
separate the capacitances, the usual practice is to
consider the measured dissipation factor to be the
true dissipation factor.
X2. EFFECTIVE AREA OF GUARDED ELECTRODE
X2.1 The effective area of a guarded electrode is
greater than its actual area b approximately half the
area of the guarded gap. 6 enerally, therefore, the
diameter of a circular electrode, each dimension of a
rectangular electrode, or the len th of a cylindrical
electrode is increased by the widt fl of the guard gap.
73

However, when the ratio of gap width, g, to electrode
separation, I (usually approximately the specimen
thickness), is appreciable, the increase in the efFective
dimension of the guarded electrode is less than the
gap width by a quantity, 28, called the guard-gap
correction, .which is a function of: (a) the ratio /r,
(b) the ratio of the permittivity of the medium %etween
the electrodes, K', to the ermittivity of the
medium in the gap, upg, and (cy the ratio of the
thickness of the electrodes, a, to the gap width.
x2.2 Exact equations for calculating 28/g for certah
ratios Of K1/Ki and a/g (16) are Shown in Ep. 15
to 17.
X2.3 The fraction of the guard gap to be added to
the overall electrode dimension before calculating the
effective electrode area is B = 1 - 2Wg. Taking into
accmt (b) and (c) above (16), R may be calculated
from the empirical equation in E4. 18.
A is a function of the ratio a/g. When a/g = 0 (thin
electrodes), A= 1. When a/g is one or greater than
one (thick electrodes), A approaches the limit 0.8106
(exactly 8/7r2). Intermediate values of A can be read
from Fi . X2.
X2.4 %'he ratio of In B from Eq 16 to In B Eq 15
is very nearly 1.23 for g/t 5 10. Therefore, the
necessity for evaluating Eq 16 can be eliminated by
writing Eq 18 as shown in Eq 19.
X2.5 VaIues of B calculated from Eq 19 will differ
from the exact values by a maximum of 0.0 1. For a
0.25-mm guard gap this maximum error would give
a 0.0025-mm error in electrode diameter or electrode
dimension. For a 25" electrode this would be an
error of 0.02 % in area.
where:
-=- 2s
g
4t In oosh (z)
rg
K'>>
~g), a/g any value
K'
X3. FACTORS AFFECTING PERMITTIVITY AND LOSS CHARACTERISTICS
X3.1 Frequency
X3.1.1 Insulating materials are used over the entire
electromagnetic spectrum, from direct current to
radar frequencies of at least 3 X IO"' Hz. There are
only a very few materials, such as polystyrene, polyethylene,
and fused silica, whose permittivity and loss
index are even approximately constant over this frequency
range. It is necessary either to measure permittivity
and loss index at the frequency at which the
material will be used or to measure them at several
frequencies suitably placed, if the material is to be
used over a fre uency range.
X3.1.2 The Langes in permittivity and loss index
with frequency are produced by the dielectric polarizations
which exist in the material. The two most
important are dipole polarization due to olar molecules
and interfacial polarization caused ! y inhomogeneities
in the material. Permittivity and loss index
vary with frequenc in the manner shown in Fig. X 1
(17). Starting at t K e highest frequency where the
permittivity is determined by an atomic or electronic
polarization, each succeeding polarization, dipole or
interfacial, adds its contribution to permittivity with
the result that the permittivity has its maximum value
at zero frequency. Each polarization furnishes a maximum
of both loss index and dissipation factor. The
frequency at which loss index is a maximum is called
the relaxation frequency for that polarization. It is
also the frequency at which the permittivity is increasing
at the greatest rate and at which half its
change for that polarization has occurred. A knowledge
of the effects of these polarizations will frequently
help to determine the frequencies at which
measurements should be made.
X3. I .3 Any d-c conductance in the dielectric
caused b free ions or electrons, while having no
direct ef ? ect on permittivity, will produce a dissipation
factor that varies inverse1 with frequency, and
that becomes infinite at zero r requency (dotted line
in Fig. Xl).
74

D 150
X3.2 Temperature
X3.2.1 The major electrical effect of tem erature
on an insulating material is to increase the re P axation
frequencies of its polarizations. They increase ex o-
nentially with temperature at rates such that a ten P old
increase in relaxation frequency may be produced by
temperature increments ranging from 6 to 50°C. The
temperature coefficient of permittivity at the lower
frequencies would always be sitive except for the
fact that the temperature coe fFO icients of permittivity
resulting from many atomic and electronic polarizations
are negative. The temperature coefficient will
or interfacial polar-
of loss index
and dissipation factor may be either positive or neg-
frequency and
negative for lower fre uencies. Since the relaxation
fre uency of interfacia 4 polarization is usually below
1 I3 z, the corresponding temperature coefficient of
loss index and dissipation factor will be positive at
all usual measuring frequencies. Since the d-c conductance
of a dielectric usually increases ex onentially
with decrease of the reciprocal of a E solute
temperature, the values of loss index and dissipation
factor arising therefrom will increase in a similar
manner and will produce a larger positive temperature
coefficient.
X3.3 Voltage
X3.3.1 All dielectric polarizations except interfacial
are near1 independent of the existing potential
gradient unti r such a value is reached that ionization
occurs in voids in the material or on its surface, or
that breakdown occurs. In interfacial polarization the
number of free ions may increase with voltage and
chan e both the magnitude of the polarization and
its re P axation frequency. The d-c conductance is similarly
affected.
X3.4 Humidity
X3.4.1 The major electrical effect of humidity on
an insulating material is to increase greatly the magnitude
of its interfacial olarization, thus increasing
both its permittivity angloss index and also its d-c
conductance. These effects of humidity are caused by
absorption of water into the volume of the material
and by the formation of an ionized water film on its
surface. The latter forms in a matter of minutes,
while the former may require days and sometimes
months to attain equilibrium, particularly for thick
and relatively impervious materials (15).
X3.5 Water Immersion
X3.5.I The effect of water immersion on an insulating
material ap roximates that of ex osure to
100% relative humigty. Water is absorbe B into the
volume of the material, usually at a greater rate than
occurs under a relative humidity of 100 %. However,
the total amount of water absorbed when equilibrium
is finally established is essentially the same under the
two conditions. If there are water-soluble substances
in the material, they will leach out much faster under
water immersion than under 100 % relative humidity
without condensation. If the water used for immersion
is not pure, its impurities may be carried into
the material. When the material is removed from the
water for measurement, the water film formed on its
surface will be thicker and more conducting than that
produced by a 100 % relative humidity without condensation,
and will require some time to attain equili
brium .
X3.6 Weathering
X3.6.1 Weathering, being a natural phenomenon,
includes the effects of varying temperature and humidity,
of fallin rain, severe winds, impurities in the
atmosphere, ani the ultraviolet light and heat of the
sun. Under such conditions the surface of an insulating
material may be permanently changed, physically
by rou hemg and cracking, and chemically by
the loss of tie more soluble components and by the
reactions of the salts, acids, and other impurities
deposited on the surface. Any water film formed on
the surface will be thicker and more conducting, and
water will penetrate more easily into the volume of
the material.
X3.7 Deterioration
X3.7. I Under operating conditions of voltage and
tem erature, an insulating material may deteriorate
in e P ectric strength because of the absorption of moisture,
physical changes of its surface, chemical changes
in its com osition, and the effects of ionization both
on its sur P ace and on the surfaces of internal voids.
In general, both its permittivity and its dissipation
factor will be increased, and these increases will be
greater the lower the measuring frequency. With a
pro er understandin of the effects outlined in X3.1
to B 3.6, the observe L!changes in any electrical property,
particularly dissipation factor, can be made a
measure of deterioration and hence of decrease in
dielectric strength.
X3.8 Conditioning
X3.8.1 The electrical characteristics of many insulating
materials are so dependent on temperature,
humidity, and water immersion, as indicated in the
paragraphs above, that it is usually necessary to
specify the past history of a specimen and its test
conditions regarding these factors. Unless measurements
are to be made at room temperature (20 to
30°C) and unspecified relative humidity, the specimen
should be conditioned in accordance with
ASTM Methods D 618, Conditioning Plastics and
Electrical Insulating Materials for Te~ting.~ The procedure
chosen should be that which most nearly
matches operating conditions. When data are required
covering a wide range of temperature and
relative humidity, it will be necessary to use intermediate
values and possibly to condition to equilibrium.
X3.8.2 Methods of maintainin specified relative
humidities are described in AS#M Recommended
Practice E 104, Maintaining Constant Relative Humidity
by Means of Aqueous solution^.^
X3.8.3 S ecifications for conditioning units are
given in A !TM Specifications E 197, for Enclosures
and Servicing Units for Tests Above and Below
Room Temperature.
75

X4. CIRCUIT DIAGRAMS OF TYPICAL MEASURING CIRCUITS
X4.1 The sim lified circuits and e uations presented
in Figs. X s to XI0 are for genera? information
only. The instruction book accompanying a particu-
lar piece of equipment should be consulted for the
exact diagram, equations, and method of measurement
to be used.
Polarizations
I Interfacial Dipole
I
L
\.
I 1 1 1 7 1 1 1 I 1 I 1 I I 1 I
-6-5 -4-3-2 -I 0 I 2 3 4 5 6 7 8 9 IO
Log
Frequency, HZ
FIG. XI Typical Polarizations (17)
76

A
FIG. X2 A versus a/g
77

Equations
Method of Balance
C, = (Ri/Rz)C* Vary CI and R2 with SI in posi-
D, = URICI tion M to obtain minimum
deflection in Detector D, Repeat
with SI in position G by
varying CI; and RF. Repeat
the above until the detector
shows no change in balance
by switching SI to M or G.
Nom-This type of bridge is especially useful for high-voltage measurements at power frequencies as almost all of the
applied voltage appears across the standard capacitor, C,, and the specimen, C,. The balancing circuits and detector are very
nearly at ground potential.
FIG. X3 High-Voltage Schering Bridge
Equations
Method of Balance
Cx = (Ri/Rz)Cs Set ratio of RI to R2 (range) and
- Dx = uCIRI vary C, and CI to obtain balante.
FIG. X4 Low-Voltage Schering Bridge, Direct Method
Equations
Method of Balance
C, = ACa
ACA = C,' - C,
Vary CI and C,, without and
with the specimen connected,
D, = (C,'/AC,)ACiwRi to obtain balance. Symbols
ACi = Ci - Ci' used for the initial balance,
with the ungrounded lead to
the unknown disconnected,
- are primed.
FIG. X5 Low-Voltage Schering Bridge, Parallel Substitution Method
78

D 150
FIG. X6 Inductive-Ratio-Arm (Transformer) Circuit
Method of Balance
Set ratio of LI to Lz (range) and
adjust C. and G, to obtain balance.
I
I
I
I
I
I
I
I
I
I
Equations
Method of Balance
' C, = C,' - C, = AC8 Balance without and rebalance
with unknown connected, us-
= AGx
ing C. and C4. Symbols used
- D, = G,/wC, = AGr/wAC8 for the initial balance are
primed.
FIG. X7 Parallel-T Network, Parallel Substitution Method
I L--A
I
I
L _ _________--_-__ _I
FIG. X8
Resonant-Rise (@Meter) Method
Method of Balance
Adjust to resonance, without
and with the specimen, noting
I, maximum V and C,. With
a standard I, V on the VTVM
can be calibrated in terms of
Q, since Q = V/IR. Subscripts
1 and 2 denote first and second
balance respectively.
Equations
Method of Balance
__________-_-- --
-7 C, =Act,
Adjust CI so maximum
I
I AC, = C,,' - C,
resonance V' is just un-
I
i CIIJ
I (C

COS e, = w/ VI
0 D, = COS e/ JI - (cos e)*
known connected.
NoTE-This method is for use at power frequencies. Instrument corrections should be applied and an unusually sensitive
wattmeter is required due to small losses. Errors from stray fields should be eliminated by shielding. Accuracy depends on
combined instrument errors and is best at full scale.
FIG. X10 Voltmeter-Wattmeter-Ammeter Method
-
CX
R
Equations
= CI
I
=_
wc2
Method of Balance
Adjust C1 and C2 to obtain
.lull.
C2
D, =-
CI
Assumption: The amplitudes of VI, V2 and VI are equal.
Nom-This circuit requires a source providing at least two outputs, one in quadrature phase relationship with the others.
A third phase, 180 deg from the reference, if not available directly from the source, can be achieved by means of an inverting,
unity-gain operation amplifier. This circuit is useful from frequencies as low as 0.001 Hz (with proper detector) to as high as
10 kHz (with appropriate corrections for phase errors). Accuracy to within 0.1 % of C, is easily attained using a fully shielded
(three-terminal) system. Shield is not shown.
FIG. X11 Ultra-Low-Frequency Bridge Using Multiphase Source
The American Society for Testin and Materials takes no position res ecting the validity o an atent rights asserted in
connection with any item mentionetin this standard. Users of this standrd are expressb a d vise dYt at determination the
validity of any such patent rights, and the risk of infringement of such rights, is entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five
years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or
for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration
at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received
a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, Pa.
19103, which will schedule a further hearing regarding your comments. Failing satisfaction there, you may appeal to the
ASTM Board of Directors.
80

~~
ab
Designation: D 257 - 78 (Reapproved 1983)"
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Methods for
D-C RESISTANCE OR CONDUCTANCE OF INSULATING
MATERIALS'
This standard is issued under the fixed designation D 257; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (0 indicates an editorial change since the last revision or reapproval.
These methods have been approved for use by agencies of the Department of Definse to replace Method 4041 of Federal Standard
406 andfir listing in the DoD Index of SpeciJcaions and Standards.
NOTE-Paragraph I .3 and editorial changes were made throughout in July 1983.
1. scope
1.1 These test methods cover direct-current
procedures for the determination of d-c insulation
resistance, volume resistance, volume resistivity,
surface resistance, and surface resistivity
of electrical insulating materials, or the corresponding
conductances and conductivities.
1.2 The test methods and procedures appear
in the sections as follows:
Method or Procedure
Applicable Documents
Calculation
Choice of Apparatus and Method
Cleaning Solid Specimens
Conditioning of Specimens
Definitions
Effective Area of Guarded Electrode
Electrode Systems
Factors Affixting Insulation Resistance or
Conductance Measurements
Humidity Control
Liquid Specimens and Cells
Precision and Accuracy
Procedure for the Measurement of Resistance
or Conductance
Report
Sampling
Significance
Specimen Mounting
Summary of Methods
Test Specimens for Insulation, Volume,
and Surface Resistance or Conductance
Determination
Typical Measurement Methods
SeCtion
2
13
7
10.1
11
5
x2
6
XI
11.2
9.4
15
12
14
8
4
10
3
9
x3
1.3 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all ofthe safety problems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health practices
and determine the applicability of regulatory limitations
prior to use. See 6.1.8. I.
2. Applicable Documents
2.1 ASTM Standards:
D374 Test Methods for Thickness of Solid
Electrical Insulation2.3
D 618 Methods of Conditioning Plastics and
Electrical Insulating Materials for Testing2
D 1 169 Test Method for Specific Resistance
(Resistivity) of Electrical Insulating Liquids4
E 104 Recommended Practice for Main&-
ing Constant Relative Humidity by Means
of Aqueous Solutions'
3. Description of Terms Specific to This Standard
3.1 insulation resistance, R,-the insulation
resistance between two electrodes that are in
contact with, or embedded in, a specimen, is the
ratio of the direct voltage applied to the electrodes
to the total current between them. It is dependent
upon both the volume and surface resistances of
the specimen.
3.2 volume resistance, R,-the volume resist-
' These test methods are under the jurisdiction of ASTM
Committee D-9 on Electrical Insulating Materials and are the
direct responsibility of Subcommittee DO9.12 on Electrical
Tests.
Current edition approved July 28, 1978. Published September
1978. Originally issued as D 257-25 T. Last previous edition
D 251 - 16.
Annual Book of ASTM Standards, Vol08.0 I.
'Annual Book ofASTM Standards, Vol 10.02.
'Annual Book ofASTM Standards, Vol 10.03.
Annual Book ofASTM Standards, Vol 14.02.
81

D 257
ance between two electrodes that are in contact
with, or embedded in, a specimen, is the ratio of
the direct voltage applied to the electrodes to that
portion of the current between them that is distributed
through the volume of the specimen.
3.3 surface resistance, Rs-the surface resistance
between two electrodes that are on the
surface of a specimen is the ratio of the direct
voltage applied to the electrodes to that portion
of the current between them which is primarily
in a thin layer of moisture or other semiconducting
material that may be deposited on the surface.
3.4 volume resistivity, p,-the volume resistivity
of a material is the ratio of the potential
gradient parallel to the current in the material to
the current density.
NOTE 1 -In the metric system, volume resistivity of
an electrical insulating material in ohm-cm is numerically
equal to the volume resistance in ohms between
opposite faces of a l-cm cube of the material. (Volume
resistivity in i2.m has a value of 1/100 of the value in
SZ . cm.)
3.5 surface resistivity, ps-the surface resistivity
of a material is the ratio of the potential
gradient parallel to the current along its surface
to the current per unit width of the surface.
NOTE 2-Surface resistivity of a material is numerically
equal to the surface resistance between two electrodes
forming opposite sides of a square. The size of
the square is immaterial.
4. Summary of Methods
4.1 The resistance or conductance of a material
specimen or of a capacitor is determined
from a measurement of current or of voltage
drop under specified conditions. By using the
appropriate electrode systems, surface and volume
resistance or conductance may be measured
separately. The resistivity or conductivity can
then be calculated when the required specimen
and electrode dimensions are known.
5. Significance and Use
5.1 Insulating materials are used to isolate
components of an electrical system from each
other and from ground, as well as to provide
mechanical support for the components. For this
purpose, it is generally desirable to have the
insulation resistance as high as possible, consistent
with acceptable mechanical, chemical, and
heat-resisting properties. Since insulation resistance
or conductance combines both volume and
surface resistance or conductance, its measured
value is most useful when the test specimen and
electrodes have the same form as is required in
actual use. Surface resistance or conductance
changes rapidly with humidity, while volume
resistance or conductance changes slowly although
the final change may eventually be
greater.
5.2 Resistivity or conductivity may be used to
predict, indirectly, the low-frequency dielectric
breakdown and dissipation factor properties of
some materials. Resistivity or conductivity is often
used as an indirect measure of moisture
content, degree of cure, mechanical continuity,
and deterioration of various types. The usefulness
of these indirect measurements is dependent on
the degree of correlation established by supporting
theoretical or experimental investigations. A
decrease of surface resistance may result either
in an increase of the dielectric breakdown voltage
because the electric field intensity is reduced, or
a decrease of the dielectric breakdown voltage
because the area under stress is increased.
5.3 All the dielectric resistances or conductances
depend on the length of time of electrification
and on the value of applied voltage (in
addition to the usual environmental variables).
These must be known to make the measured
value of resistance or conductance meaningful.
5.4 Volume resistivity or conductivity can be
used as an aid in designing an insulator for a
specific application. The change of resistivity or
conductivity with temperature and humidity
may be great (1, 2, 3, 4),6 and must be known
when designing for operating conditions. Volume
resistivity or conductivity determinations are often
used in checking the uniformity of an insulating
material, either with regard to processing
or to detect conductive impurities that affect the
quality of the material and that may not be
readily detectable by other methods.
5.5 Volume resistivities above lo2' O.cm
( a. mj, obtained on specimens under usuai
laboratory conditions, are of doubtful validity,
considering the limitations of commonly used
measuring equipment.
5.6 Surface resistance or conductance cannot
be measured accurately, only approximated, because
more or less volume resistance or conductance
is nearly always involved in the measurement.
The measured value is largely a property
of the contamination that happens to be on the
6The boldface numbers in parentheses refer to the list of
references appended to these methods.
82

D 257
specimen at the time. However, the permittivity
of the specimen influences the deposition of contaminants
and its surface characteristics affect
the conductance of the contaminants. Surface
resistivity or conductivity can be considered to
be related to material properties when contamination
is involved but is not a material property
in the usual sense.
6. Electrode Systems
6.1 The electrodes for insulating materials
should be of a material that is readily applied,
allows intimate contact with the specimen
surface, and introduces no appreciable error
because of electrode resistance or contamination
of the specimen (5). The electrode material
should be corrosion-resistant under the
conditions of test. For tests of fabricated
specimens such as feed-through bushings, cables,
etc., the electrodes employed are a part
of the specimen or its mounting. Measurements
of insulation resistance or conductance,
then, include the contaminating effects of
electrode or mounting materials and are generally
related to the performance of the specimen
in actual use.
6.1 .l Binding- Post and Taper- Pin Electrodes,
Figs. 1 and 3, provide a means of
applying voltage to rigid insulating materials
to permit an evaluation of their resistive or
conductive properties. These electrodes simulate
to some degree the actual conditions of
use, such as binding posts on instrument
panels and terminal strips. In the case of
laminated insulating materials having highresin-content
surfaces, somewhat lower insulation
resistance values may be obtained with
taper-pin than with binding posts, due to
more intimate contact with the body of the
insulating material. Resistance or conductance
values obtained are highly influenced by
the individuai contact between each pin and
the dielectric material, the surface roughness
of the pins, and the smoothness of the hole in
the dielectric material. Reproducibility of results
on different specimens is difficult to
obtain.
6.1.2 Metal Bars in the arrangement of
Fig. 2 were primarily devised to evaluate the
insulation resistance or conductance of flexible
tapes and thin, solid specimens as a fairly
simple and convenient means of electrical
quality control. This arrangement is some-
what more satisfactory for obtaining approximate
values of surface resistance or conductance
when the width of the insulating material
is much greater than its thickness.
6.1.3 Silver Paint, Figs, 4, 6, and 7, is
available commercially with a high conductivity,
either air-drying or low-temperature-baking
varieties, which are sufficiently porous to
permit diffusion of moisture through them
and thereby allow the test specimen to be
conditioned after the application of the electrodes.
This is a particularly useful feature in
studying resistance-humidity effects, as well
as change with temperature. However, before
conductive paint is used as an electrode material,
it should be established that the solvent
in the paint does not attack the material so as
to change its electrical properties. Reasonably
smooth edges of guard electrodes may be
obtained with a fine-bristle brush. However,
for circular electrodes, sharper edges can be
obtained by the use of a ruling compass and
silver paint for drawing the outline circles of
the electrodes and filling in the enclosed areas
by brush. A narrow strip masking tape may
be used, provided the pressure-sensitive adhesive
used does not contaminate the surface
of the specimen. Clamp-on masks also may be
used if the electrode paint is sprayed on.
6.1.4 Sprayed Metal, Figs. 4, 6, and 7,
may be used if satisfactory adhesion to the
test specimen can be obtained. Thin sprayed
electrodes may have certain advantages in
that they are ready for use as soon as applied.
They may be sufficiently porous to allow the
specimen to be conditioned, but this should
be verified. Narrow strips of masking tape or
clamp-on masks must be used to produce a
gap between the guarded and the guard electrodes.
The tape shall be such as not to
contaminate the gap surface.
6.1.5 Evaporated Metal may be used under
the same conditions given in 6.1.4.
6.1.6 Metal Foil, Fig. 4, may be applied to
specimen surfaces as electrodes. The usual
thickness of metal foil used for resistance or
conductance studies of dielectrics ranges from
6 to 80 pm. Lead or tin foil is in most
common use, and is usually attached to the
test specimen by a minimum quantity of petrolatum,
silicone grease, oil, or other suitable
material, as an adhesive. Such electrodes shall
be applied under a smoothing pressure suffi-
83

cient to eliminate all wrinkles, and to work
excess adhesive toward the edge of the foil
where it can be wiped off with a cleansing
tissue. One very effective method is to use a
hard narrow roller (10 to 15 mm wide), and
to roll outward on the surface until no visible
imprint can be made on the foil with the
roller. This technique can be used satisfactorily
only on specimens that have very flat
surfaces. With care, the adhesive film can be
reduced to 2.5 pm. As this film is in series
with the specimen, it will always cause the
measured resistance to be too high. This error
may become excessive for the lower-resistivity
specimens of thickness less than 250 pm.
Also the hard roller can force sharp particles
into or through thin films (50 pm). Foil
electrodes are not porous and will not allow
the test specimen to condition after the electrodes
have been applied. The adhesive may
lose its effectiveness at elevated temperatures
necessitating the use of flat metal back-up
plates under pressure. It is possible, with the
aid of a suitable cutting device, to cut a proper
width strip from one electrode to form a
guarded and guard electrode. Such a threeterminal
specimen normally cannot be used
for surface resistance or conductance measurements
because of the grease remaining on
the gap surface. It may be very difficult to
clean the entire gap surface without disturbing
the adjacent edges of the electfode.
6.1.7 Colloidal Graphite, Fig. 4, dispersed
in water or other suitable vehicle, may be
brushed on nonporous, sheet insulating materials
to form an air-drying electrode. Masking
tapes or clamp-on masks may be used
(6.1.4). This electrode material is recommended
only if all of the following conditions
are met:
6.1.7.1 The material to be tested must
accept a graphite coating that will not flake
before testing,
6.1.7.2 The material being tested must not
absorb water readily, and
6.1.7.3 Conditioning must be in a dry atmosphere
(Procedure B, Methods D 618),
and measurements made in this same atmosphere.
6.1.8 Mercury or other liquid metal electrodes
give satisfactory results. Mercury is not
recommended for continuous use or at elevated
temperatures due to toxic effects. Cau-
tion-see 6.1.8.1. The metal forming the
upper electrodes should be confined by stainless
steel rings, each of which should have its
lower rim reduced to a sharp edge by beveling
on the side away from the liquid metal. Figure
5 shows two electrode arrangements.
6.1.8.1 Caution-Mercury metal vapor poisoning
has long been recognized as a hazard in
industry. The maximum exposure limits are set
by the American Conference of Governmental
Industrial Hygienists7. The concentration of mercury
vapor over spills from broken thermometers,
barometers, or other instruments using mercury
can easily exceed these exposure limits.
Mercury, being a liquid and quite heavy, will
disintegrate into small droplets and seep into
cracks and crevices in the floor. The use of a
commercially available emergency spill kit is recommended
whenever a spill occurs. The increased
area of exposure adds significantly to the
mercury vapor concentration in air. Mercury
vapor concentration is easily monitored using
commercially available sniffers. Spot checks
should be made periodically around operations
where mercury is exposed to the atmosphere.
Thorough checks should be made after spills.
6.1.9 Flat Metal Plates, Fig. 4, (preferably
guarded) may be used for testing flexible and
compressible materials, both at room temperature
and at elevated temperatures. They may
be circular or rectangular (for tapes). To
ensure intimate contact with the specimen,
considerable pressure is usually required.
Pressures of 140 to 700 kPa have been found
satisfactory (see material specifications).
6.1.10 Conducting Rubber has been used
as electrode material, as in Fig. 4, and has the
advantage that it can quickly and easily be
applied and removed from the specimen. As
the electrodes are applied only during the
time of measurement, they do not interfere
with the conditioning of the specimen. The
conductive-rubber material must be backed
by proper plates and be soft enough so that
effective contact with the specimen is obtained
when a reasonable pressure is applied.
NOTE 3-There is evidence that values of conductivity
obtained using conductive-rubber electrodes
are always smaller (20 to 70 YO) than values
obtained with tinfoil electrodes (6). When only
order-of-magnitude accuracies are required, and
’ American Conference of Governmental and Industrial Hygienists,
P.O. 1937, Cincinnati, OH, 4520 1.
84

D 257
these contact errors can be neglected, a properly
designed set of conductive-rubber electrodes can
provide a rapid means for making conductivity and
resistivity determinations.
6.1.1 1 Water is widely employed as one
electrode in testing insulation on wires and
cables. Both ends of the specimen must be
out of the water and of such length that
leakage along the insulation is negligible.
Guard rings may be necessary at each end. It
may be desirable to add a small amount of
sodium chloride to the water to ensure high
conductivity. Measurements may be performed
at temperatures up to about 100°C.
7. Choice of Apparatus and Method
7.1 Power Supply-A source of very
steady direct voltage is required (see X1.7.3).
Batteries or other stable direct voltage supplies
may be used.
7.2 Direct Measurements -The current
through a specimen at a fixed voltage may be
measured using any equipment that has the
required sensitivity and accuracy (210 % is
usually adequate). Current-measuring devices
available include electrometers, d-c amplifiers
with indicating meters, and galvanometers.
Typical methods and circuits are given in
Appendix X3. When the measuring device
scale is calibrated to read ohms directly no
calculations are required.
7.3 Comparison Methods -A Wheatstonebridge
circuit may be used to compare the
resistance of the specimen with that of a
standard resistor (see Appendix X3).
7.4 Precision and Bias Considerations:
7.4.1 General -As a guide in the choice of
apparatus, the pertinent considerations are
summarized in Table 1, but it is not implied
that the examples enumerated are the only
ones applicable. This table is not intended to
indicate the limits of sensitivity and error of
the various methods per se, but rather is
intended to indicate limits that are distinctly
possible with modern apparatus. In any case,
such limits can be achieved or exceeded only
through careful selection and combination of
the apparatus employed. It must be emphasized,
however, that the errors considered are
those of instrumentation only. Errors such as
those discussed in Appendix X1 are an entirely
different matter. In this latter connection,
the last column of Table 1 lists the
resistance that is shunted by the insulation
resistance between the guarded electrode and
the guard system for the various methods. In
general, the lower such resistance, the less
probability of error from undue shunting.
NOTE 4-No matter what measurement method
is employed, the highest precisions are achieved
only with careful evaluation of all sources of error.
It is possible either to set up any of these methods
from the component parts, or to acquire a completely
integrated apparatus. In general, the methods
using high-sensitivity galvanometers require a
more permanent installation than those using indicating
meters or recorders. The methods using
indicating devices such as voltmeters, galvanometers,
d-c amplifiers, and electrometers require the
minimum of manual adjustment and are easy to
read but the operator is required to make the
reading at a particular time. The Wheatstone bridge
(Fig. X4) and the potentiometer method (Fig.
X2(b)) require the undivided attention of the operator
in keeping a balance, but allow the setting at
a particular time to be read at leisure.
7.4.2 Direct Measurements:
7.4.2.1 Galvanometer-Voltmeter -The
maximum percentage error in the measurement
of resistance by the galvanometer-voltmeter
method is the sum of the percentage
errors of galvanometer indication, galvanometer
readability, and voltmeter indication. As
an example: a galvanometer having a sensitivity
of 500 pA/scale division will be deflected
25 divisions with 500 V applied to a resistance
of 40 GLR (conductance of 25 pS). If the
deflection can be read to the nearest 0.5
division, and the calibration error (including
Ayrton Shunt error) is 22 % of the observed
value, the resultant galvanometer error will
not exceed +4 %. If the voltmeter has an error
of +2 % of full scale, this resistance can be measured
with a maximum error of +6 % when the
voltmeter reads full scale, and +lo % when it
reads one third full scale. The desirability of
readings near full scale are readily apparent.
7.4.2.2 Voltmeter-Ammeter -The maximum
percentage error in the computed value
is the sum of the percentage errors in the
voltages, V, and V,, and the resistance, R,.
The errors in V, and R, are generally dependent
more on the characteristics of the apparatus
used than on the particular method. The
most significant factors that determine the
errors in V, are indicator errors, amplifier
zero drift, and amplifier gain stability. With
modern, well-designed amplifiers or electrometers,
gain stability is usually not a matter
85

of concern. With existing techniques, the zero
drift of direct voltage amplifiers or electrometers
cannot be eliminated but it can be made
slow enough to be relatively insignificant for
these measurements. The zero drift is virtually
nonexistent for carefully designed convertertype
amplifiers. Consequently, the null
method of Fig. X 1.2(6) is theoretically less subject
to error than those methods employing an
indicating instrument, provided, however, that
the potentiometer voltage is accurately known.
The error in R, is to some extent dependent on
the amplifier sensitivity. For measurement of a
given current, the higher the amplifier sensitivity,
the greater likelihood that lower valued, highly
precise wire-wound standard resistors can be
used. Such amplifiers can be obtained. Standard
resistances of 100 GR known to +2 %, are available.
If IO-mV input to the amplifier or electrometer
gives full-scale deflection with an error not
greater than 2 % of full scale, with 500 V applied,
a resistance of 5000 TR can be measured with a
maximum error of 6 % when the voltmeter reads
full scale, and 10 % when it reads '/3 scale.
7.4.2.3 Comparison - Galvanometer - The
maximum percentage error in the computed
resistance or conductance is given by the sum
of the percentage errors in R,, the galvanometer
deflections or amplifier readings, and the
assumption that the current sensitivities are
independent of the deflections. The latter
assumption is correct to well within 22 %
over the useful range (above l/10 full-scale
deflection) of a good, modern galvanometer
(probably '/3 scale deflection for a d-c current
amplifier). The error in R, depends on the
type of resistor used, but resistances of 1 MR
with a limit of error as low as 0.1 % are
available. With a galvanometer or d-c current
amplifier having a sensitivity of 10 nA for fullscale
deflection, 500 V applied to a resistance
of 5 TSL will produce a 1 90 deflection. At this
voltage, with the above noted standard resistor,
and with Fy = lo5, d,s would be about half
of full-scale deflection, with a readability error
not more than +1 %. If d, is approximately
*/4 of full-scale deflection, the readability
error would not exceed +.4 %, and a
resistance of the order of 200 GR could be
measured with a maximum error of 25'/2 %.
7.4.2.4 Voltage Rate-of-Change -The accuracy
of the measurement is directly propor-
tional to the accuracy of the measurement of
applied voltage and time rate of change of the
electrometer reading. The length of time that
the electrometer switch is open and the scale
used should be such that the time can be
measured accurately and a full-scale reading
obtained. Under these conditions, the accuracy
will be comparable with that of the other
methods of measuring current.
7.4.2.5 Comparison Bridge - When the
detector has adequate sensitivity, the maximum
percentage error in the computer resistance
is the sum of the percentage errors in the
arms, A, B, and N. With a detector sensitivity
of 1 mV/scale division, 500 V applied to the
bridge, and RN = 1 GR, a resistance of 1000
TO will produce a detector deflection of one
scale division. Assuming negligible errors in
RA and RB, with RN = 1 GR known to within
22 % and with the bridge balanced to one
detector-scale division, a resistance of 100 TR
can be measured with a maximum error of
26 %.
8. Sampling
8.1 Refer to applicable materials specifications
for sampling instructions.
9. Test Specimens
9.1 Insulation Resistance or Conductance
Determination:
9.1.1 The measurement is of greatest value
when the specimen has the form, electrodes,
and mounting required in actual use. Bushings,
cables, and capacitors are typical examples
for which the test electrodes are a part of
the specimen and its normal mounting means.
9.1.2 For solid materials, the test specimen
may be of any practical form. The specimen
forms most commonly used are flat plates,
tapes, rods, and tubes. The electrode arrangements
of Fig. 3 may be used for flat plates,
rods, or rigid tubes whose inner diameter is
about 20 mm or more. The electrode arrangement
of Fig. 2 may be used for strips of sheet
material or for flexible tape. For rigid strip
specimens the metal support may not be required.
The electrode arrangements of Fig. 7
may be used for flat plates, rods, or tubes.
Comparison of materials when using different
electrode arrangements is frequently inconclusive
and should be avoided.
86

9.2 Volume Resistance or Conductance Determination:
9.2.1 The test specimen may have any
practical form that allows the use of a third
electrode, when necessary, to guard against
error from surface effects. Test specimens
may be in the form of flat plates, tapes, or
tubes. Figures 4 and 5 illustrate the application
and arrangement of electrodes for plate
or sheet specimens. Figure 6 is a diametral
cross section of three electrodes applied to a
tubular specimen, in which electrode No. 1 is
the guarded electrode, electrode No. 2 is a
guard electrode consisting of a ring at each
end of electrode No. 1, and electrode No. 3 is
the unguarded electrode (7, 8). For materials
that have negligible surface leakage, the guard
rings may be omitted. Convenient and generally
suitable dimensions applicable to Fig. 4
in the case of test specimens that are 3 mm in
thickness are as follows: D3 = 100 mm, D2 =
88 mm, and D1 = 76 mm, or alternatively, D3
= 50 mm, D2 = 38 mm, and D, = 25 mm.
For a given sensitivity, the larger specimen
allows more accurate measurements on materials
of higher resistivity.
9.2.2 Measure the average thickness of the
specimens in accordance with one of the methods
in Test Methods D 374 pertaining to the material
being tested. The actual points of measurement
shall be uniformly distributed over the area to be
covered by the measuring electrodes.
9.2.3 It is not necessary that the electrodes
have the circular symmetry shown in Fig. 4
although this is generally convenient. The
guarded electrode (No. 1) may be circular,
square, or rectangular, allowing ready computation
of the guarded electrode area for
volume resistivity or conductivity determination
when such is desired. The diameter of a
circular electrode, the side of a square, or the
shortest side of a rectangular electrode,
should be at least four times the specimen
thickness. The gap width should be great
enough so that the surface leakage between
electrodes No. 1 and No. 2 does not cause an
error in the measurement (this is particularly
important for high-input-impedance instruments,
such as electrometers). If the gap is
made equal to twice the specimen thickness,
as suggested in 9.3.3, so that the specimen
can be used also for surface resistance or
conductance determinations, the effective
area of electrode No. 1 can be taken, usually
with sufficient accuracy, as extending to the
center of the gap. If, under special conditions,
it becomes desirable to determine a more
accurate value for the effective area of electrode
No. 1, the correction for the gap width
can be obtained from Appendix X2. Electrode
No. 3 may have any shape provided
that it extends at all points beyond the inner
edge of electrode No. 2 by at least twice the
specimen thickness.
9.2.4 For tubular specimens, electrode No.
1 should encircle the outside of the specimen
and its axial length should be at least four
times the specimen wall thickness. Considerations
regarding the gap width are the same
as those given in 9.2.3. Electrode No. 2 consists
of an encircling electrode at each end of
the tube, the two parts being electrically connected
by external means. The axial length of
each of these parts should be at least twice the
wall thickness of the specimen. Electrode No.
3 must cover the inside surface of the specimen
for an axial length extending beyond the
outside gap edges by at least twice the wall
thickness. The tubular specimen (Fig. 6) may
take the form of an insulated wire or cable. If
the length of electrode is more than 100 times
the thickness of the insulation, the effects of
the ends of the guarded electrode become
negligible, and careful spacing of the guard
electrodes is not required. Thus, the gap
between electrodes No. 1 and No. 2 may be
several centimetres to permit sufficient surface
resistance between these electrodes when
water is used as electrode No. 1. In this case,
no correction is made for the gap width.
9.3 Surface Resistance or Conductance Determination:
9.3.1 The test specimen may be of any
practical form consistent with the particular
objective, such as flat plates, tapes, or tubes.
9.3.2 The arrangements of Figs. 2 and 3
were devised for those cases where the volume
resistance is known to be high relative to
that of the surface (2). However, the combination
of molded and machined surfaces
makes the result obtained generally inconclusive
for rigid strip specimens. The arrangement
of Fig. 2 is somewhat more satisfactory
when applied to specimens for which the
width is much greater than the thickness, the
cut edge effect thus tending to become rela-
87

D 257
tively small. Hence, this arrangement is more
suitable for testing thin specimens such as
tape, than for testing relatively thicker specimens.
The arrangements of Figs. 2 and 3
should never be used for resistance or conductance
determinations without due considerations
of the limitations noted above.
9.3.3 The three electrode arrangements of
Figs. 4, 5, and 6 may be used for purposes of
material comparison. The resistance or conductance
of the surface gap between electrodes
No. 1 and No. 2 is determined directly
by using electrode No. 1 as the guarded electrode,
electrode No. 3 as the guard electrode,
and electrode No. 2 as the unguarded electrode
(7,8). The resistance or conductance so
determined is actually the resultant of the
surface resistance or conductance between
electrodes No. 1 and No. 2 in parallel with
some volume resistance or conductance between
the same two electrodes. For this arrangement
the surface gap width,g, should be
approximately twice the specimen thickness,
t, except for thin specimens, where g may be
much greater than twice the material thickness.
9.3.4 Special techniques and electrode dimensions
may be required for very thin specimens
having such a low volume resistivity
that the resultant low resistance between the
guarded electrode and the guard system
would cause excessive error.
9.4 Liquid Insulation Resistance-The sampling
of liquid insulating materials, the test cells
employed, and the methods of cleaning the cells
shall be in accordance with Test Method D 1 169.
10. Specimen Mounting
10.1 In mounting the specimens for measurements,
it is important that there shall be no
conductive paths between the electrodes or between
the measuring electrodes and ground that
will have a significant effect on the reading of the
measuring instrument (9). Insulating surfaces
should not be handled with bare fingers (acetate
rayon gloves are recommended). For referee tests
of volume resistivity or conductivity, the surfaces
should be cleaned with a suitable solvent before
conditioning. When surface resistance is to be
measured, the surfaces should be cleaned or not
cleaned as specified or agreed upon.
11. Conditioning
11.1 The specimens shall be conditioned in
accordance with Methods D 61 8.
11.2 Circulating-air environmental chambers
or the methods described in Recommended
Practice E 104 may be used for controlling
the relative humidity.
12. Procedure
12.1 Insulation Resistance or Conductance
-Properly mount the specimen in the test
chamber. If the test chamber and the conditioning
chamber are the same (recommended
procedure), the specimens should be mounted
before the conditioning is started. Make the measurement
with a suitable device having the required
sensitivity and accuracy (see Appendix
X3). Unless otherwise specified, the time of electrification
shall be 60 s and the applied direct
voltage shall be 500 f 5 V.
12.2 Volume Resistivity or Conductivity -
Measure the dimensions of the electrodes and
width of guard gap,g. Make the measurement
with a suitable device having the required
sensitivity and accuracy. Unless otherwise
specified, the time of electrification shall be
60 s, and the applied direct voltage shall be
500 +: 5 V.
12.3 Surface Resistance or Conductance:
12.3.1 Measure the electrode dimensions
and the distance between the electrodes, g .
Measure the surface resistance or conductance
between electrodes No. 1 and 2 with a
suitable device having the required sensitivity
and accuracy. Unless otherwise specified, the
time of electrification shall be 60 s, and the
applied direct voltage shall be 500 * 5 V.
12.3.2 When the electrode arrangement of
Fig. 2 is used, P is taken as the perimeter of
the cross section of the specimen. For thin
specimens, such as tapes, this perimeter effectively
reduces to twice the specimen width.
12.3.3 When the electrode arrangements
of Fig. 7 are used (and the volume resistance
is known to be high compared to the surface
resistance), P is taken to be the length of the
electrodes or circumference of the cylinder.
13. Calculation
13.1 Calculate the volume resistivity, p,.,
and the volume conductivity, y,., using the
equations in Table 2.
88

D 257
13.2 Calculate the surface resistivity, ps,
and the surface conductivity, ys, using the
equations in Table 2.
14. Report
14.1 The report shall include at least the
following:
14.1 .l. A description and identification of
the material (name, grade, color, manufacturer,
etc.),
14.1.2 Shape and dimensions of the test
specimen,
14.1.3 Type and dimensions of electrodes,
14.1.4 Conditioning of the specimen
(cleaning, predrying, hours at humidity and
temperature, etc.),
14.1.5 Test conditions (specimen temperature,
relative humidity, etc., at time of measurement),
14.1.6 Method of measurement (see A p
pendix X3),
14.1.7 Applied voltage,
14.1.8 Time of electrification of measurement,
14.1.9 Measured values of the appropriate
resistances in ohms or conductances in siemens,
14.1.10 Computed values when required,
of volume resistivity in ohm-centimetres, volume
conductivity in siemens per centimetre,
surface resistivity in ohms (per square), or
surface conductivity in siemens (per square),
and
14.1.11 Statement as to whether the reported
values are “apparent” or “steadystate.”
15. Precision and Bias
15.1 Precision and bias are inherently affected
by the choice of method, apparatus, and specimen.
For analysis and details see Sections 7 and
9, and particularly 7.4.1 through 7.4.2.5.
REFERENCES
(1) Curtis, H. L., “Insulating Properties of Solid
Dielectric.” Bulletin, Nat. Bureau Standards,
Vol 11, 1915, Scientific Paper No. 234, pp.
369-417.
(2) Field, R. F., “How Humidity Affects Insulation,
Part I, D-C Phenomena,” General Radio
Experimenter, Vol 20, Nos. 2 and 3, July-
August, 1945.
(3) Field, R. F., “The Formation of Ionized Water
Films on Dielectrics Under Conditions of
High Humidity,” Journal of Applied Physics,
Vol5, May, 1946.
(4) Herou, R., and LaCoste, R., “Sur La MCsure
Des Resistivities et L’Etude de Conditionnement
des Isolantes en Feuilles,” Report IEC
15-GT2 (France) 4 April, 1963.
(5) Thompson, B. H., and Mathes, K. N., “Electrolytic
Corrosion - Methods of Evaluating
Materials Used in Tropical Service,” Transactions,
Am. Inst. Electrical Engrs., Vol 64,
June, 1945, p. 287.
(6) Scottj A. H., “Anomalous Conductance Behavior
in Polymers,” Report of the 1965
Conference on Electrical Insulation, NRC-
NAS.
(7) Amey, W. G., and Hamberger, F., Jr., “A
Method for Evaluating the Surface and Volume
Resistance Characteristics of Solid Dielectric
Materials,” Proceedings, Am. SOC.
Testing Mats., Vol49, 1949, pp. 1079-1091.
(8) Witt, R. K., Chapman, J. J., and Raskin, B.
L., “Measuring of Surface and Volume Resistance,”
Modern Plastics, Vol 24, No. 8,
April, 1947, p. 152.
(9) Scott, A. H., “Insulation Resistance Measurements,”
Fourth Electrical Insulation Conference,
Washington, D.C., Feb. 19-22,
1962.
(10) Kline, G. M., Martin, A. R., and Crouse, W.
A., “Sorption of Water by Plastics,” Proceedings,
Am. SOC. Testing Mats., Vol 40, 1940,
pp. 1273-1282.
(11) Greenfield, E. W ., “Insulation Resistance
Measurements,” Electrical Engineering, Vol
66. July, 1947, pp. 698-703.
(12) Cole, K. S., and Cole, R. H., “Dispersion
and Absorption in Dielectrics, I1 Direct Current
Characteristics,” Journal of Chemical
Physics, Vol 10, 1942.
(13) Field, R. F., “Interpretation of Current-Time
Curves as Applied to Insulation Testing,”
AIEE Boston District Meeting, April 19-20,
1944.
(14) Lauritzen, J. I., “The Effective Area of a
Guarded Electrode ,” Annual Report, Conference
on Electrical Insulation. NAS-NRC Publication
1141, 1963.
(15) Turner, E. F., Brancato, E. L., and Price,
W., “The Measurement of Insulation Conductivity.”
NRf, Report 5060, Naval Research
Laboratory, Feb. 25, 1958.
(16) Dorcas, D. S., and Scott, R. N., “Instrumentation
for Measuring the D-C Conductivity of
Very High Resistivity Materials,” Review of
Scientific Instruments, Vol 35, No. 9, Sept.
1964.
(17) Endicott, H. S., “Insulation Resistance, Absorption,
and Their Measurement,” Annual
Report, Conference on Electrical Insulation,
NAS-NRC Publication, 1958.
(18) Occhini, E. and Maschio, G., “Electrical
Characteristics of Oil-Im regnated Pa er as
Insulation for HV-DC cagles,’? IEEE Runsactions
on Power Apparatus and Systems, Vol
PAS-86, No. 3- March 1967.
(19) Endicott, H. S., “Guard-Gap Correction for
89

~ ~ ~ ~~ ~~~~ ~~
Guarded-Electrode Measurements and Exact Testing and Evaluation, JTEVA, Vol 4, No.
Equations for the Two-Fluid Method of 3, May 1976, pp. 188-195.
Measuring Permittivity and Loss," Journal of
TABLE 1 Apparatus and Conditions for Use
Reference
Ohms Shunted
Maximum Maximum by Insulation
Ohms Ohms Type of
Method
Resistance from
Detectable to
Section Figure
Measurement Guard to
at 500 V
Guarded
500 V
Electrode
Voltmeter-ammeter (gal- X3.1 XI 10" 10" deflection 10 to I O
vanometer)
Comparison (galvanom- x3.4 x3
IO" 10" deflection IO to 105
eter)
Voltmeter-ammeter (d-c
amplification,
trometer)
elec-
Comparison (Wheatstone
bridge)
Voltage rate-of-change
Megohmmeter (typical)
X3.2 X2(4
(Position I)
ma)
(Position 2)
X2(@
XW)
x3.5 x4
x3.3 x5
commercial instruments
lol:l
deflection
10'8 deflection
10'5 deflection
1015 null
1014 null
ioi4
deflection
direct-reading
io2 to io9
102 to lo:'
Io:' to IO"
0 (effective)
lo5 to 106
unguarded
io4 to ioi0
TABLE 2
Calculation of Resistivity or Conductivity'
Type of Electrodes or
Specimen
Volume Resistivity, 0-cm
Volume Conductivity, SI
cm
t
7. = - G,
A
Circular (Fig. 4)
Rectangular
Square
Tubes (Fig. 6)
Cables
2rrLR.,
A = (a + g) (b + g)
A = (a + g)'
A = mDo(L + g)
Dz
In- Dl
yr = -
~TLR,.
Surface Resistivity, 0
Surface Conductivity, S
(per square)
(per square)
P
g
Pa = -R,
7s = -Gs
g
P
Circular (Fig. 4)
P = WDO
Rectangular
P = 2(a b + 2g)
Square
P = 4(a + g)
Tubes (Figs. 6 and 7)
P=2nDZ
Nomenclature:
A = the effective area of the measuring electrode for the particular arrangement employed,
P = the effective perimeter of the guarded electrode for the particular arrangement employed,
R, = measured volume resistance in ohms,
G, = measured volume conductance in siemens,
R, = measured surface resistance in ohms,
G, = measured surface conductance in siemens,
t = average thickness of the specimen,
Do, D1, Dp, g, L = dimensions indicated in Figs. 4 and 6 (see Appendix X2 for correction tog ),
a, b, = lengths of the sides of rectangular electrodes, and
In = natural logarithm.
All dimensions are in centimetres.
90

1
64"
Metd Support
and Guard.
Side View
Brass, Copper, or
Stainless Steel
Electrodes
II
!! ! I
1 .
I :
II
..
Methacrylate
End View
FIG. 2 Strip Electrodes for Tapes md Flat, Solid Specimens
91

-+--
I
I
-+--
25mm min.
I
--
-25mm mln.
- c
E
E
0
N
E
-
Y
0
N I
c
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E
- 1 0
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I
A. Plate Specimen
25mmmh-1-25*1 --
mm-, 25mm min.
I
I.D. 20mm min.
.-
8. Tube Specimen
O.D. 20mm min.
C. Rod Specimen
Use Pratt 8 Whitney No.3 Taper Pins
FIG. 3 Taper-PinElectmdes
92

FIG. 4
Electrode
Volume Resistivity g Z 21 Surface Resistivity
Fht Specimen for Measuring Volume and Surface Resistances or Conductances
\ r..
Specimen
ttrr.
Detoil
NOTE: Gution--See 6. I .8
FIG. SA Mercury Electrodes for Flat, Solid Specimens
93

Cell Material: Polystyrene.
TFE-Fluorocarbon, or/
, I Poly(nethy1 methacrylate)
I I I
22" 122 mm - Drill for 6-32
1
Flat-head Screws
/- 7 I" drill
SPecimen
I
I
NOTE: C.utiolc--see 6. I .8
FIG. 5B Mercury Cell for Thin Sheet Matdl
Electrode N&- D 2 --I L t
= (Dl + 9)/2 L > 41 g S 2t Volume Resistivity g h 2t Surface Resistivity
FIG. 6 Tubular Specimen for Measuring Volume and Surface Resistances or Conductances
94

D 257
.i
25mmmin. - lOO* I mm - 25mmmin.
A-Plate
Specimen
B-Tube
or Rod Specimen
FIG. 7 Conducting-Paint Electrodes
APPENDIXES
(Nonmandatory Information)
X1. FACLORS AFFECTING INSULATION RESISTANCE OR CONDUCTANCE
MEASUREMENTS
X1.l Inherent Variation in Materials -Because
of the variability of the resistance of a given specimen
under similar test conditions and the nonuniformity
of the same material from specimen to
specimen, determinations are usually not reproducible
to closer than 10 % and often are even more
widely divergent (a range of values of 10 to 1 may
be obtained under apparently identical conditionsj.
X1.2 Temperature -The resistance of electrical
insulating materials is known to change with temperature,
and the variation often can be represented
by a function of the form: (18)
R = BemlT
(XI 1
where:
R = resistance (or resistivity) of an insulating material
or system,
B = proportionality constant,
m = activation constant, and
T = absolute temperature in kelvin (K).
This equation is a simplified form of the Arrhenius
equation relating the activation energy of a chemical
reaction to the absolute temperature; and the
Boltzmann principle, a general law dealing with the
statistical distribution of energy among large numbers
of minute particles subject to thermal agitation.
The activation constant, m, has a value that is
characteristic of a particular energy absorption
process. Several such processes may exist within the
material, each with a different effective temperature
range, so that several values of m would be
needed to fully characterize the material. These
values of m can be determined experimentally by
plotting the natural logarithm of resistance against
the reciprocal of the absolute temperature. The
desired values of m are obtained from such a plot
by measuring the slopes of the straight-line sections
of the plot. This derives from Eq (l), for its follows
that by taking the natural logarithm of both sides:
1
In R = In B + m T -
The change in resistance (or resistivity) corresponding
to a change in absolute temperature from TI to
T2, based on Eq 1, and expressed in logarithmic
form, is:
95

(X3)
These e uations are valid over a temperature range
In (R2/R1) = m (; - 4) (s)
= m
only if t B e material does not undergo a transition
within this temperature range. Extrapolations are
seldom safe since transitions are seldom obvious or
predictable. As a corollary, deviation of a plot of
the logarithm of R against 1/T from a straight line is
evidence that a transition is occurring. Furthermore,
in making comparisons between materials, it
is essential that measurements be made over the
entire range of interest for all materials.
NOTE X1 -The resistance of an electrical insulating
material may be affected by the time of
temperature exposure. Therefore, equivalent temperature
conditioning periods are essentially for
comparative measurements.
NOTE X2 -If the insulating material shows signs
of deterioration after conditioning at elevated temperature
conditioning periods are essential for comparative
measurements.
X1.3 Temperature and Humidity -The insulation
resistance of solid dielectric materials decreases
both with increasing temperature as described in
X1.2 and with increasing humidity (1, 2, 3, 4).
Volume resistance is particularly sensitive to temperature
changes, while surface resistance changes
widely and very rapidly with humidity changes (2,
3). In both cases the change is exponential. For
some materials a change from 25 to 100°C may
change insulation resistance or conductance by a
factor of 100 000, often due to the combined
effects of temperature and moisture content
chan e; the effect of temperature change alone is
usua f ly much smaller. A change from 25 to 90 %
relative humidity may change insulation resistance
or conductance by as much as a factor of 1 000 000
or more. Insulation resistance or conductance is a
function of both the volume and surface resistance
or conductance of the specimen, and surface resistance
changes almost instantaneously with change of
relative humidity. It is, therefore, absolutely essential
to maintain both temperature and relative humidity
within close limits during the conditioning
period and to make the insulation resistance or
conductance measurements in the specified conditioning
environment. Another point not to be overlooked
is that at relative humidities above 90 %,
surface condensation may result from inadvertant
fluctuations in humidity or temperature produced
by the conditioning system. This problem can be
avoided by the use of equivalent absolute humidity
at a slightly higher temperature, as equilibrium
moisture content remains nearly the same for a
small temperature change. In determining the effect
of humidity on volume resistance or conductance,
extended periods of conditioning are required, since
the absorption of water into the body of the dielectric
is a relatively slow process (10). Some specimens
require months to come to equilibrium. When
such long periods of conditioning are prohibitive,
use of thinner specimens or comparative measurements
near equilibrium may be reasonable alternatives,
but the details must be included in the test
report.
X1.4 Time of Electrification -Measurement of a
dielectric material is not fundamentally different
from that of a conductor except that an additional
96
D 257
parameter, time of electrification, (and in some
cases the voltage gradient) is involved. The relationship
between the applied voltage and the current
is involved in both cases. For dielectric materials,
the standard resistance placed in series with
the unknown resistance must have a relatively low
value, so that essentially full voltage will be applied
across the unknown resistance. When a potential
difference is applied to a specimen, the current
through it generally decreases asymptotically toward
a limiting value which may be less than 0.01
of the current observed at the end of 1 min (9,ll).
This decrease of current with time is due to dielectric
absorption (interfacial polarization, volume
charge, etc.) and the sweep of mobile ions to the
electrodes. In general, the relation of current and
time is of the form I(t) = after the initial
charge is completed and until the true leakage
current becomes a significant factor (12, 13). In
this relation A is a constant, numerically the current
at unit time, and m usually, but not always, has a
value between 0 and 1. Depending upon the characteristics
of the specimen material, the time required
for the current to decrease to within 1 % of
this minimum value may be from a few seconds to
many hours. Thus, in order to ensure that measurements
on a given material will be com arable, it is
necessary to specify the time of electri P ication. The
conventional arbitrary time of electrification has
been 1 min. For some materials, misleading conclusions
may be drawn from the test results obtained
at this arbitrary time. A resistance-time or conductance-time
curve should be obtained under the conditions
of test for a given material as a basis for
selection of a suitable time of electrification, which
must be specified in the test method for that material,
or such curves should be used for comparative
purposes. Occasionally, a material will be found for
which the current increases with time. In this case
either the time curves must be used or a special
study undertaken, and arbitrary decisions made as
to the time of electrification.
X 1.5 Magnitude of Voltage:
X1.5.1 Both volume and surface resistance or
conductance of a specimen may be voltage-sensitive
(4). In that case, it is necessary that the same
voltage gradient be used if measurements on similar
specimens are to be comparable. Also, the applied
voltage should be within at least 5 % of the specified
voltage. This is a separate requirement from
that given in X1.7.3, which discusses voltage regulation
and stability where appreciable specimen
capacitance is involved.
X1.5.2 Commonly specified test voltages to be
applied to the complete specimen are 100, 250,
500,1000,2500,5000,10 000 and 15 000 V. Of
these, the most frequently used are 100 and 500 V.
The higher voltages are used either to study the
voltage-resistance or voltage-conductance characteristics
of materials (to make tests at or near the
operating voltage gradients), or to increase the
sensitivity of measurement.
X1.5.3 Specimen resistance or conductance of
some materials may, depending upon the moisture
content, be affected by the polarity of the applied
voltage. This effect, caused by electrolysis or ionic
migration, or both, particularly in the presence of
nonuniform fields, may be particularly noticeable in
insulation configurations such as those found in
cables where the test-voltage gradient is greater at

D 257
the inner conductor than at the outer surface.
Where electrolysis or ionic migration does exist in
specimens, the electrical resistance will be lower
when the smaller test electrode is made negative
with respect to the larger. In such cases, the polarity
of the applied voltage shall be specified according
to the requirements of the specimen under test.
X1.6 Contour of Specimen:
X1.6.1 The measured value of the insulation
resistance or conductance of a specimen results
from the composite effect of its volume and surface
resistances or conductances. Since the relative values
of the components vary from material to material,
comparison of different materials by the use of
the electrode systems of Figs. 1, 2, and 3 is generally
inconclusive. There is no assurance that, if
material A has a higher insulation resistance than
material B as measured by the use of one of these
electrode systems, it will also have a higher resistance
than B in the application for which it is
intended.
X1.6.2 It is possible to devise specimen and
electrode configurations suitable for the separate
evaluation of the volume resistance or conductance
and the approximate surface resistance or conductance
of the same specimen. In general, this requires
at least three electrodes so arranged that one may
select electrode pairs for which the resistance or
conductance measured is primarily that of either a
volume current path or a surface current path, not
both (7).
X1.7 Deficiencies in the Measuring Circuit:
X1.7.1 The insulation resistance of many solid
dielectric specimens is extremely high at standard
laboratory conditions, approaching or exceeding
the maximum measurable limits given in Table 1.
Unless extreme care is taken with the insulation of
the measuring circuit, the values obtained are more
a measure of apparatus limitations than of the
material itself. Thus errors in the measurement of
the specimen may arise from undue shunting of the
specimen, reference resistors, or the current-measuring
device, by leakage resistances or conductances
of unknown, and possibly variable, magnitude.
X1.7.2 Electrolytic, contact, or thermal emf's
may exist in the measuring circuit itself; or spurious
emf's may be caused by leakage from external
sources. Thermal emf's are normally insignificant
except in the low resistance circuit of a galvanometer
and shunt. When thermal emf's are present,
random drifts in the galvanometer zero occur. Slow
drifts due to air currents may be troublesome.
Electrolytic emf's are usually associated with moist
specimens and dissimilar metals, but emf's of 20
mV or more can be obtained in the guard circuit of
a high-resistance detector when pieces of the same
metal are in contact with moist specimens. If a
voltage is applied between the guard and the
guarded electrodes a polarization emf may remain
after the voltage is removed. True contact emf's can
be detected only with an electrometer and are not a
source of error. The term "spurious emf'' is sometimes
applied to electrolytic emf's. To ensure the
absence of spurious emf's of whatever origin, the
deflection of the detecting device should be observed
before the application of voltage to the
specimen and after the voltage has been removed.
If the two deflections are the same, or nearly the
same, a correction can be made to the measured
resistance or conductance, provided the correction
is small. If the deflections differ widely, or approach
the deflection of the measurement, it will be necessary
to find and eliminate the source of the spurious
emf (5). Capacitance changes in the connecting
shielded cables can cause serious difficulties.
X1.7.3 Where appreciable specimen capacitance
is involved, both the regulation and transient
stability of the applied voltage should be such that
resistance or conductance measurements can be
made to prescribed accuracy. Short-time transients,
as well as relatively long-time drifts in the applied
voltage may cause spurious capacitive charge and
discharge currents which can significantly affect the
accuracy of measurement. In the case of currentmeasuring
methods particularly, this can be a serious
problem. The current in the measuring instrument
due to a voltage transient is Zo = C,dV/dt.
The amplitude and rate of pointer excursions depend
upon the following factors:
X1.7.3.1 The capacitance of the specimen,
X1.7.3.2 The magnitude of the current being
measured,
X1.7.3.3 The magnitude and duration of the
incoming voltage transient, and its rate of change,
X1.7.3.4 The ability of the stabilizing circuit
used to provide a constant voltage with incoming
transients of various characteristics, and
X1.7.3.5 The time-constant of the complete test
circuit as compared to the period and damping of
the current-measuring instrument.
X1.7.4 Changes of range of a current-measuring
instrument may introduce a current transient. When
R, 4 R, and C, 6 C,, the equation of this transient
is
z = (V~/R,)[Z - e~'/~m',] (X4)
where:
Vo = applied voltage,
R, = apparent resistance of the specimen,
R, = effective input resistance of the measuring
instrument,
C, = capacitance of the specimen at 1000 Hz,
C, = input capacitance of the measuring instrument,
and
t = time after R, is switched into the circuit.
For not more than 5 % error due to this transient,
R,C, 5 tl3 (X5)
Microammeters employing feedback are usually
free of this source of error as the actual input
resistance is divided, effectively, by the amount of
feedback, usuaiiy at least by i000.
X1.8 Residual Charge-In X1.4 it was pointed
out that tlfe current continues for a long time after
the application of a potential difference to the
electrodes. Conversely, current will continue for a
long time after the electrodes of a charged specimen
are connected together. It should be established
that the test specimen is completely discharged
before attempting the first measurement, a repeat
measurement, a measurement of volume resistance
following a measurement of surface resistance, or a
measurement with reversed voltage (9). The time
of discharge before making a measurement should
be at least four times any previous charging time.
The specimen electrodes should be connected together
until the measurement is to be made to
97

D 257
prevent any build-up of charge from the surroundings.
X 1.9 Guarding:
X1.9.1 Guarding depends on interposing, in all
critical insulated paths, guard conductors which
intercept all stray currents that might otherwise
cause errors. The guard conductors are connected
together, constituting the guard system and forming,
with the measuring terminals, a three-terminal
network. When suitable connections are made,
stray currents from spurious external voltages are
shunted away from the measuring circuit by the
guard system.
X 1.9.2 Proper use of the guard system for the methods
involving current measurement is illustrated in
Figs. XI.1 to X1.3, inclusive, where the guard system
is shown connected to the junction of the voltage source
and current-measuring instrument or standard resistor.
In Fig. X1.4 for the Wheatstone-bridge method, the
guard system is shown connected to the junction of the
two lower-valued-resistance arms. In all cases, to be
effective, guarding must be complete, and must include
any controls operated by the observer in making the
measurement. The guard system is generally maintained
at a potential close to that of the guarded ter-
minal, but insulated from it. This is because, among
other things, the resistance of many insulating materials
is voltage-dependent. Otherwise, the direct resistances
or conductances of a three-terminal network are independent
of the electrode potentials. It is usual to ground
the guard system and hence one side of the voltage
source and current-measuring device. This places both
terminals of the specimen above ground. Sometimes,
one terminal of the specimen is permanently grounded.
The current-measuring device usually is then connected
to this terminal, requiring that the voltage source be
well insulated from ground.
X1.9.3 Errors in current measurements may result
from the fact that the current-measuring device
is shunted by the resistance or conductance between
the guarded terminal and the guard system. This
resistance should be at least 10 to 100 times the
input resistance of the current measuring device. In
some bridge techniques, the guard and measuring
terminals are brought to nearly the same potentials,
but a standard resistor in the bridge IS shunted
between the unguarded terminal and the guard
system. This resistance should be at least 1000
times that of the reference resistor.
I
I I Ayrtori Shunt
FIG. X1.1
Voltmeter-Ammeter Method Using
a Galvanometer.
98

I
'/
(a)Normal Use of Amplifier and Indicating Meter
'1
I
Voltmeter
L
(b) Amplifier and Indicating Meter os Null Detector
I I I I
-
I
FIG. X1.3 Comparison Method
Using a Galvanometer
I
FIG. X1.2 Voltmeter-Ammeter Method
Using D-C Amplification
I 1
-
I V X iRN
Detector
FIG. X1.4 Comparison Method Using
a Wheatstone Bridge
X2. EFFECTIVE AREA OF GUARDED ELECTRODE
X2.1 General -Calculation of volume resistivity
from the measured volume resistance involves the
quantity A, the effective area of the guarded electrode.
Depending on the material properties and
the electrode configuration, A differs from the
actual area of the guarded electrode for either, or
both, of the following reasons.
X2.1.1 Fringing of the lines of current in the
region of the electrode edges may effectively increase
the electrode dimensions.
X2.1.2 If plane electrodes are not parallel, or if
tubular electrodes are not coaxial, the current density
in the specimen will not be uniform, and an
error may result. This error is usually small and
may be ignored.
X2.2 Fringing:
X2.2.1 If the specimen material is homogeneous and
isotropic, fringing effectively extends the guarded elec-
trode edge by an amount (14,19):
and g and t are the dimensions indicated in Figs. 4 and
6. The correction may also be written
g[1 - P W I = Bg (X7)
where B is the fraction of the gap width to be added
to the diameter of circular electrodes or to the
dimensions of rectangular or cylindrical electrodes.
X2.2.2 Laminated materials, however, are
somewhat anisotropic after volume absorption of
moisture. Volume resistivity parallel to the laminations
is then lower than that in the perpendicular
direction, and the fringing effect is increased. With
99

D 257
such moist laminates, 6 ap roaches zero, and the
guarded electrode effective! extends to the center
of the gap between guarded and unguarded electrodes
(14).
X2.2.3 The fraction of the gap width g to be
added to the diameter of circular electrodes or to
the electrode dimensions of rectangular or cylindrical
electrodes, B, as determined by above equation
for 6, is as follows:
glt B glt B
0.1 0.96 1.0 0.64
0.2 0.92 1.2 0.59
0.3 0.88 1.5 0.51
0.4 0.85 2.0 0.41
0.5 0.81 2.5 0.34
0.6 0.77 3.0 0.29
0.8 0.71
NOTE X3 -The symbol “In” designates loga-
rithm to the base e = 2.718. . . . When g is
approximately equal to 2t, 6 is determined with
sufficient approximation by the equation:
6 = 0.586t
NOTE X4-For tests on thin films when t

D 257
is connected as shown, to include the potentiometer in
the measuring circuit. When connections are made. in
this manner, no resistance is placed in the measunng
circuit at balance and thus no voltage drop appears
between the measuring electrode and the guard electrode.
However, a steeply increasing fraction of R, is
included in the measuring circuit, as the potentiometer
is moved off balance. Any alternating voltage appearing
across the specimen resistance is amplified by the net
amplifier gain. The amplifier may be either a direct
voltage amplifier or an alternating voltage amplifier
provided with input and output converters. Induced
alternating voltages across the specimen often are sufficiently
troublesome that a resistance-capacitance filter
preceding the amplifier is required. The input resistance
of this filter should be at least 100 times greater than
the effect resistance that is placed in the measurement
circuit by resistance R,.
X3.2.4 The resistance R,, or the conductance, G,, is
calculated as follows:
R, = l/Gx = V,/Ix = (V,/V,)R, (X9)
where:
V, = applied voltage,
I, = specimen current,
R, = standard resistance, and
V, = voltage drop across R,, indicated by the amplifier
output meter, the electrometer or the calibrated
potentiometer.
X3.3 Voltage Rate-of-Change Method:
X3.3. I If the specimen capacitance is relatively
large, or capacitors are to be measured, the apparent
resistant, R,, can be determined from the charging
voltage, Vo, the specimen capacitance value, CO (capacitance
of C, at 1000 Hz), and the rate-of-change of
voltage, dV/dt, using the circuit of Fig. X3.1 (17). To
make a measurement the specimen is charged by closing
Sz,with the electrometer shorting switch SI closed.
When SI is subsequently opened, the voltage across the
specimen will fall because the leakage and absorption
currents must then be supplied by the capacitance Co
rather than by Vo. The drop in voltage across the
specimen will be shown by the electrometer. If a recorder
is connected to the output of the electrometer,
the rate of change of voltage, dV/dt, can be read from
the recorder trace at any desired time after SZ is closed
(60 s usually specified). Alternatively, the voltage, AV,
appearing on the electrometer in a time, At, can be
used. Since this gives an average of the rate-of-change
of voltage during At, the time Al should be centered at
the specified electrification time (time since closing Sz).
X3.3.2 If the input resistance of the electrometer
is greater than the apparent specimen resistance
and the input capacitance is 0.01 or less of that of
the specimen, the apparent resistance at the time ai
which dV/dt or AV/& is determined is
R, = Vo/I, = Vodt/CodV, or, Vo&/C0AV, (X10)
depending on whether or not a recorder is used.
When the electrometer input resistance or capacitance
cannot be ignored or when V , is more than a
small fraction of Vo the complete equation should
be used.
where:
C, = capacitance of C, at 1000 Hz,
R, = input resistance of the electrometer,
C, = input capacitance of the electrometer,
Vo = applied voltage, and
V, = electrometer reading = voltage decrease on
c,
X3.4 Comparison Method Using a Galvanometer
or D-C Amplifier (I):
X3.4.1 A standard resistance, R,, and a galvanometer
or d-c amplifier are connected to the
voltage source and to the test specimen as shown in
Fig. X3. The galvanometer and its associated Ayrton
shunt is the same as described in X3.1.1. An
amplifier of equivalent direct current sensitivity
with an appropriate indicator may be used in place
of the galvanometer. It is convenient, but not
necessary, and not desirable if batteries are used as
the voltage source (unless a high-input resistance
voltmeter is used), to connect a voltmeter across
the source for a continuous check of its voltage.
The switch is provided for shorting the unknown
resistance in the process of measurement. Sometimes
provision is made to short either the unknown
or standard resistance but not both at the same
time.
X3.4.2 In general, it is preferable to leave the
standard resistance in the circuit st all times to
prevent damage to the current measuring instrument
in case of specimen failure. With the shunt set
to the least sensitive position and with the switch
open, the voltage is applied. The Ayrton shunt is
then adjusted to give as near maximum scale reading
as possible. At the end of the electrification
time the deflection, d,, and the shunt ratio, F,, are
noted. The shunt is then set to the least sensitive
position and the switch is closed to short the unknown
resistance. Again the shunt is adjusted to
give as near maximum scale reading as possible and
the galvanometer or meter deflection, d,, and the
shunt ratio, F,, are noted. It is assumed that the
current sensitivities of the galvanometer or amplifier
are equal for nearly equal deflections d, and d,.
X3.4.3 The unknown resistance, R,, or conductance,
G,, is calculated as follows:
R, = l/C, = R,[(d,F,/d,F,) - 13 (X12)
where:
F, and F,= ratios of the total current to the galvanometer
or d-c amplifier with Ri in
the circuit, and shorted, respectively.
X3.4.4 In case R, is shorted when R, is in the
circuit or the ratio of F, to F, is greater than 100,
the value of R, or C, is computed as follows:
R, = 1/G, = R (d,F, /d,F,) (XI31
X3.5 Comparison Methods Using a Wheatstone
-
Bridge (2):
X3.5.1 The test specimen is connected into one arm
of a Wheatstone bridge as shown in Fig. X1.4. The
three known arms shall be of as high resistance as
practicable, limited by the errors inherent in such resistors.
Usually, the lowest resistance, RA, is used for
convenient balance adjustment, with either RB or RN
being changed in decade steps. The detector shall be a
d-c amplifier, with an input resistance high compared
to any of these arms.
X3.5.2 The unknown resistance, R,, or conductance,
G,, is calculated as follows:
R, = I/G, = R&v/RA
(X14)
101

D 257
where RA, RB, and RN are as shown in Fig. XI .4. When
arm A is a rheostat, its dial can be calibrated to read
directly in megohms after multiplying by the factor
RBRN which for convenience, can be varied in decade
steps.
X3.6 Recordings-it is possible to record continuously
against time the values of the unknown resistance
or the corresponding value of current at a known
voltage. Generally, this is accomplished by an adaptation
of the voltmeter-ammeter method, using d-c amplification
(X3.2). The zero drift of direct coupled d-c
amplifiers, while slow enough for the measurements of
X3.2, may be too fast for continuous recording. This
problem can be resolved by periodic checks of the zero,
or by using an a-c amplifier with input and output
converter. The indicating meter of Fig. X 1.2(a) can be
replaced by a recording milliammeter or millivoltmeter
as appropriate for the amplifier used. The recorder may
be either the deflection type or the null-balance type,
the latter usually having a smaller error. Null-balancetype
recorders also can be employed to perform the
function of automatically adjusting the potentiometer
shown in Fig. XI .2(b) and thereby indicating and recording
the quantity under measurement. The characteristics
of amplifier, recorder balancing mechanism,
and potentiometer can be made such as to constitute a
well integrated, stable, electromechanical, feedback sys-
tem of high sensitivity and low error. Such systems also
can be arranged with the potentiometer fed from the
same source of stable voltage as the specimen, thereby
eliminating the voltmeter error, and allowing a sensitivity
and precision comparable with those of the Wheatstone-Bridge
Method (X3.5).
X3.7 Direct-Reading Instruments -There are
available, and in general use, instruments that
indicate resistance directly, by a determination of
the ratio of voltage and current in bridge methods
or related modes. Some units incorporate various
advanced features and refinements such as digital
readout. Most direct reading instruments are selfcontained,
portable, and comprise a stable d-c
power supply with multi-test voltage capability, a
null detector or an indicator, and all relevant auxiliaries.
Measurement accuracies vary somewhat
with type of equipment and range of resistances
covered; for the more elaborate instruments accuracies
are comparable to those obtained with the
voltmeter-ammeter method using a galvanometer
(X3.1). The direct-reading instruments do not necessarily
supplant any of the other typical measurement
methods described in this Appendix, but do
offer simplicity and convenience for both routine
and investigative resistance measurements.
FIG. X3.1 Voltage Rate-of-Chenge Method
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights. and the risk of infiingement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St.. Philadelphia, Pa. 19103.
102

4[Tb Designation: D 332 - 80
An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
TINTING STRENGTH OF WHITE PIGMENTS'
This standard is issued under the fixed designation D 332; the number immediately following the designation indicates the year of
original adoption or, in the case of revision. the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (6) indicates an editorial change since the last revision or reapproval.
This tiiethod hos been opprowdfor use he ugencies of the Deportment of Defense IO replace Method 4222 of Fedrrol Te.st Method
Stundurd No. 141A und for listing in the DoD Index of Specijicotions ond Stondords.
1. scope
I. I This method is intended to be used only
for comparing a sample of the pigment to be
tested with a reference standard of the same
type and grade.
1.2 This method utilizes visual assessment to
evaluate the results. ASTM Method D 2745,
Test for Instrumental Tinting Strength of
White Pigments,' covers a more precise procedure
based on instrumental measurement of
reflectance of tinted pastes.
2. Applicable Document
2.1 ASTM Standard
D262 Specification for Ultramarine Blue
Pigmen t2
3. Apparatus
3. I Balance, laboratory-type, sensitive to 0.1
mg, equipped with a counter- balanced watch
glass.
3.2 Buret, I-mL capacity, stopcock controlled.
graduated in 0. I-ml divisions, or other
suitable dispensing apparatus with a delivery
accurate to 0.05 mL.
3.3 Glass Muller-A weighted glass muller
with beveled edge having a total weight of 15
Ib (6.8 kg) and a grinding face of from 2?'4 to 3
in. (70 to 76 mm) in diameter. The face shall
be free of blowholes and other imperfections
and kept roughened by lightly grinding with
No. 303 optical emery, or its equivalent, and
turpentine.
3.4 Rubbing Suqace- A ground glass plate,
at least 14 by 20 in. (355 by 510 mm), the
surface of which is kept roughened by lightly
grinding with No. 303 optical emery, or its
equivalent, and turpentine.
3.5 Automatic Muller, auto ma ti^,^ equipped
with a weight that exerts a permanent 50-lbf
(220-N) force and an additional weight exerting
a 50-lbf making a total of 100-lbf (445-N). The
two glass plates shall be kept sharp by removing
from the machine and grinding them face-toface
with No. 303 optical emery or equivalent,
and water.
3.6 Spatula-A flexible spatula having a
chromium-plated or plastic blade 3 to 6 in. (75
to 150 mm) long.
3.7 Panels of bright tin, glass, or white-lacquered
cardboard.
3.8 Scraper-A French scraper or stiff scraping
knife having a blade that is about 3 or 4 in.
(75 to 100 mm) wide with a straight edge.
4. Materials
4. I Tinting Material-Ultramarine blue conforming
to Specification D262 or a grade
agreed upon by the purchaser and the seller.
4.2 Oil-Refined linseed oil with an acid
number of approximately 4.
5. Reference Standard
5.1 A standard white pigment of the same
:ype and grade as the sample !o be tested, as
agreed upon by the purchaser and the seller.
' This method is under the jurisdiction of ASTM Committee
D-1 on Paint and Related Coatings and Materials and is the
direct responsibility of Subcommittee W1.26 on Optical Prop
erties.
Current edition approved Aug. 1,1980. Published November
1980. Originally published as D 332 - 3 I T. Last previous edition
D 332-64 (1975).
Annual Book ofASTM Standards, Vol 06.02.
A satisfactory muller is supplied by the Hoover Color Corp.,
I3 Cordier St. Irvington. N.J. 07 I 1 I .
103

6. Procedure A-Glass Muller
6.1 Weigh exactly 2 g of the reference standard
white pigment and the amount of ultramarine
blue listed in Table 1. Transfer the
weighed portions of white and blue pigments
to the ground-glass plate. Add the amount of
oil specified in Table I from the buret (Note).
Be sure to allow the buret to drain to its true
level because variations in the amount of oil
decrease the accuracy of the test. Work the
pigments and oil into a paste with the spatula;
then rub up the paste with the glass muller,
spreading it over an area 3 to 4 in. (75 to 100
mm) wide and from 12 to 15 in. (305 to 380
mm) long. In counting the rubs, one stroke up
and one stroke back is considered one rub.
Allow the muller to travel up one side and back
the other side, twisting it slightly at the top and
bottom of each stroke. After each 25 rubs with
the muller, “pick up” the paste with the spatula
by scraping the face of the muller and gathering
the paste on the slab into a mound. Repeat
until the paste has been given 100 rubs.
NOTE I-Where the resulting paste is too fluid or
too thick for mulling, adjust the quantity of oil to
give a workable paste and prepare a new paste,
mulling as before. Report the amount of oil used.
6.2 Treat 2 g of the sample in exactly the
same manner as prescribed in 6.1 for the reference
standard, using the same amount of
tinting material and oil.
6.3 Spread the pastes of the reference standard
and the sample in parallel contiguous rectangular
areas on the panel, each about I in.
(25 mm) wide and 2 in. (50 mm) long. Use the
scraper to smooth the surface of the pastes
(here called “draw-downs”) by drawing the
scraper lightly over the pastes to give a straight
and even line of contact between them. Keep
the drawn-downs sufficiently thick to obscure
the panel.
6.4 Immediately examine the draw-downs of
the two pastes, on the top side only, for relative
lightness of tint. If the sample is lighter than
the reference standard it has greater tinting
strength. If the sample differs appreciably from
the reference standard in lightness of tint, and
if a numerical rating is desired, prepare other
pastes of the reference standard white pigment
using different amounts of the tinting material.
Make a draw-down of the sample paste with
each standard as described in 6.3. Select the
draw-down in which the standard paste most
closely matches the sample paste in lightness.
Use the weight of tinting material in this
method to calculate the tinting strength of the
sample.
7. Procedure B-Automatic Muller
7.1 In order to minimize the effect of the
difference in grinding of the area near the
center of the plates as compared to the area
sear the periphery of the plates, draw two
concentric circles under the base plate of the
muller in such a way that they show clearly
through the plate. These circles can be drawn
either on a paper inserted under the plate, or
drawn directly on the bottom of the plate. The
inner circle should be 2% in. (63 mm) in diameter
and the outer circle 4% in. (1 15.3 mm)
in diameter.
7.2 Carefully weigh the pigment as described
in 5.1. transferring the pigment to the base plate
of the muller. Add the oil and work the pigment
and oil into a paste with the spatula. Distribute
the paste within the area between the two con-
Fentric circles on the plate, close the muller,
and add a 50-lb (23-kg) weight (to make a total
weight of 100 Ib (45 kg) pressing the plates
together. Mull the paste with three series of
mulls of 50 revolutions each with a pickup of
the paste between each series, spreading the
paste as before between the two concentric
circles before starting the next series.
7.3 Continue the treatment of the paste of
the sample and standard as described in 6.2,
6.3, and 6.4.
8. Calculation
8. I Calculate the tinting strength of the sample
as follows:
Tinting strength of pigment = (B/A) x T
where:
A = weight in grams of tinting material used
with reference standard to give equality of
tint,
B = weight in grams of tinting material used
with sample, and
T = arbitrary tinting strength value given to
the reference standard.
104

TABLE 1 Quantities of Materials for Tinting Strength
Tests
Weight of
Weight of Ultrama- Amount
Pigment Typc Pigment, rine Blue of Oil,
t3 Tinting mL
Pigment, g
-
White lead 2 0.2 0.5
Zinc oxide 2 0.2 0.7
Zinc oxide, leaded 2 0.2 0.5
Lithopone 2 0.2 0.7
Zinc sulfide 2 0.4 0.7
Titanium dioxide
(anatase) 2 0.4 I .o
(rutile) 2 0.4 0.9
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in
connection with any item mentioned in this stundard. Users of this standardare expressly advised that determination of the vaIidity
of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years
and if not revised, either reapproved or withdrawn, Your comments are invited either for revision of this standard or for additional
standards and should be addressed to A STM Headquarters. Your comments will receive carejiul consideration at a meeting of the
responsible technicalcommittee, which you may attend. Ifyou feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., PhiIadelphia, Pa. 19103.
105

Designation: D 387 - 86
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia. Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
COLOR AND STRENGTH OF COLOR PIGMENTS WITH A
MECHANICAL MULLER'
This standard is issued under the fixed designation D 387; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (E) indicates an editorial change since the last revision or reapproval.
This method has been approved for use bv agencies of the Department of Defense to replace Method 4220. I . 4221 of Federal Test
Method Standard No. 141A and for lisring in (he DoD Index of Speci9carions and Standards.
1. scope
1.1 This test method is intended to be used to
compare the color and strength of a pigment
under test with a reference standard of the same
type and grade.
1.2 This test method does not apply to white
pigments.
NOTE I-Test Method D 3022 is similar to this test
method. but it utilizes a miniature sandmill rather than
a mechanical muller, to disperse the color pigment.
NOTE 2-Test Method D332 and Test Method
D2745 are similar to this test method, but they are
intended for use with white pigments, rather than color
pigments.
1.3 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of the user of this standard to establish appropriate
safety and health practices and determine
the applicability of regulatory limitations prior to
use. Specific hazard statements are given in Section
7.
2. Referenced Documents
2.1 ASTM Standards:
D332 Test Method for Tinting Strength of
White Pigments2
D 1729 Practice for Visual Evaluation of Color
Differences of Opaque Materials)
D 2244 Test Method for Instrumental Evaluation
of Color Differences of Opaque Materials)
D 2745 Test Method for Instrumental Tinting
Strength of White Pigments2
D 3022 Test Method for Color and Strength of
Color Pigments by Use of a Miniature Sandmill2
D 3964 Practice for Selection of Coating Specimens
for Appearance Measurements2
E 97 Test Method for Directional Reflectance
Factor. 45-deg, 0-deg of Opaque Specimens
by Broad-Band Filter Reflectometry3
E 308 Practice for Spectrophotometry and Description
of Color in CIE System4
3. Summary of Test Method
3.1 Pigments are dispersed in a suitable vehicle
with a mechanical muller. Test and standard
pigments are treated identically. Opaque drawdowns
are made from the dispersions and compared.
either visually or instrumentally. for color
and strength differences.
4. Significance and Use
4.1 Color and tinting strength are the most
important properties of a color pigment. This test
method provides a means of testing these properties
for quality control.
4.2 This test method is intended as a referee
method so that such matters as the vehicle for
preparing the dispersions and the white for making
tints have been suggested. However, other
This test method is under the jurisdiction of ASTM Committee
D-l on Paint and Related Coatings and Materials and is
the direct responsibility of Subcommittee W1.26 on Optical
Properties.
Current edition approved Aug. 26, 1986. Published October
1986. Originally published as D 387 - 34 T. Last previous edition
D 387 - 8 I .
Annual Bonk of ASTM Standards, Vol06.02.
Annual Book oJASTM Slandords, Vol06.0 1.
'Annual Book oJASTM Standards, Vol 14.02.
106

D 387
vehicles and whites may be suitable for quality
control purposes, and changes in this test method
are allowed by agreement between the parties to
a test.
4.3 It is assumed that the most exact comparison
of mass color and tinting strength occurs
when the pigment is completely dispersed. By
following the procedure described in Annex A I,
the conditions for achieving the maximum practical
degree of dispersion with a mechanical
muller may be determined. Color and strength
tests should be camed out under these conditions.
4.4 The results obtained with a mechanical
muller do not necessarily correlate directly with
an industrial situation where different dispersing
conditions exist. However, dispersion with a mechanical
muller is a quick and inexpensive way
of testing the color and strength of a pigment for
routine quality control.
5. Apparatus
5.1 Balances-(I) A balance sensitive to 10
mg and (2) an analytical balance sensitive to 1 .O
mg.
5.2 Muller, Me~hanical,~ equipped with
ground-glass plates to which a variable but
known force may be added in 50-lbf (220-N)
increments. The driven glass plate shall have a
speed of rotation of between 70 and 120 rpm
and the apparatus shall have an arrangement
for pre-setting the number of revolutions in
multiples of 50.
5.3 Rubbing Surfaces-The rubbing surfaces
of the ground glass plates shall be kept sharp
by removing them from the muller and grinding
them face-to-face with No. 303 optical
emery, or its equivalent, and water.
5.4 Small Glass Slab or other nonabsorbent
material, suitable for weighing and mixing pigment
pastes.
5.5 Spatula-A flexible spatuia having a 3
to 6-in. (75 to 150-mm) blade.
5.6 Paper Charts,b white with a black band
and a surface impervious to paint liquids.
5.7 Film Applicator,' at least 3 in. (75 mm)
wide with a clearance of 4 mils (100 pm) to
produce wet films about 2 mils (50 pm) thick.
5.8 Color-Measuring Instrument, meeting the
requirements of Test Method D 2244.
6. Materials
6.1 Reference Standard-A standard pig-
ment of the same type and grade as the pigment
to be tested, as agreed upon between the purchaser
and the seller.
6.2 Vehicle-A solvent-free vehicle, such as
No. 1 lithographic varnish, with 0.8 9% each of
cobalt and manganese driers (6 % types).
6.3 White Tinting Paste-A white paint compatible
with the dispersion vehicle, such as 57
parts of rutile titanium dioxide dispersed in 43
parts of the vehicle described in 6.2.
NOTE 3-Because the choice of vehicle and white
tinting pigment may affect the results, they should be
agreed upon between the purchaser and the seller.
7. Hazards
7.1 Some pigments may be potentially toxic
and therefore should be handled with care.
Obtain specific precautions from the manufacturer
or supplier.
7.2 Many solvents and paint vehicles present
explosion, fire, and toxicity hazards, and they
should accordingly be handled with care.
Again, obtain specific precautions from the
manufacturer or supplier.
8. Dispersing Conditions
8.1 The conditions for dispersing the pigment
on the mechanical muller should be such
that the maximum tinting strength is developed.
For each pigment and each dispersing
vehicle the development of tinting strength by
the mechanical muller is influenced by the
force applied, the number of revolutions, the
mass of the pigment, and the mass of the vehicle.
The conditions for obtaining the maximum
tinting strength with the mechanical
muller can be determined by following the
procedure in Annex A 1.
8.2 If these conditions are known for a particular
pigment with a particular vehicle, or if
the purchaser and seller agree upon a particular
set of conditions, there is no need to carry out
the procedure in Annex Ai.
9. Dispersion Procedure
9.1 Decide, by agreement or by experimentation,
as discussed in Section 8, the following
A satisfactory muller is supplied by the Hoover Color Corp.,
I3 Cordier St., Irvington, NJ 07 I I 1.
White charts with a black band are preferred for judging
opacity. Satisfactory charts are available from the Morest Co.,
21 1 Centre St., New York, NY 10073, and the Leneta Co., P.O.
Box 576, Ho-Ho-Kus, NJ 07423.
'Satisfactory film applicators are available from Bird and
Son, Walpole, MA 02081 and Precision Gage & Tool Co., 28
Volkenand Ave., Dayton, OH 45410.
107

D 307
dispersing conditions:
9.1.1 Force applied to the muller plates;
9.1.2 Number of revolutions;
9.1.3 Mass of the pigment; and
9.1.4 Mass of the vehicle.
9.2 Applying these decisions, prepare a dispersion
of the reference standard pigment.
Weigh onto a glass slab to within 2 mg, the
appropriate quantities of the standard pigment
and the dispersing vehicle. Mix the pigment
and vehicle together thoroughly with the spatula
and transfer the mixture to the lower plate
of the muller. Spread the mixture in a path
approximately 100 mm wide and halfway between
the center and rim of the lower plate,
and clean the spatula as much as possible by
wiping it on the upper plate of the muller.
Close the plates and carry out the mulling
stages of 50 revolutions; after each stage collect
the paste from both plates with the spatula and
spread it around the 100-mm path on the lower
plate, wiping the spatula on the upper plate as
before. When the mulling has been carried out
for the prescribed number of revolutions, collect
the paste and store it. Clean the glass slab,
the muller plates, and the spatula, and repeat
the procedure with exactly the same quantities
of the test sample and vehicle. Collect the paste
from this sample and store it. Clean the glass
slab, the muller plates, and the spatula.
NOTE &The most common sources of error in
this procedure are inaccurate weighing, incomplete
transfer of the pigment and vehicle mixture, and
contamination of the plates by previous samples.
10. Masstone Color Procedure
10.1 Draw down a portion of the test and
standard pastes in juxtaposition on a paper
chart over a vacuum-drawdown plate or other
suitable plane surface with the film applicator,
Make sure that the coating is opaque.
10.2 immediately compare the colors visually
while still wet, using Practice D 1729, and record
the results. Set the drawdowns aside in a dustfree
area to dry. When dry repeat the visual color
difference evaluation and record the results. See
Practice D 3964.
10.3 If desired, evaluate the color difference
instrumentally using Test Method D 2244, and
report the color difference in units as agreed upon
between the purchaser and seller.
NOTE 5-Wet color difference evaluations may
not agree with dry color difference evaluations because
of such phenomena as flooding and flocculation.
In the case of a difference between the wet and
dry evaluations, the purchaser and the seller should
agree upon which condition is the standard.
NOTE 6-Color difference measurements of wet
paints may require a special adapter to protect the
instrument from fouling. Because color differencemeasuring
instruments differ widely in their design,
the user may have to develop his own adapter.
108
11. Tint Color Procedure
11.1 Determine by calculation the amount
of white pigment paste that must be added to
0.5 g of the color pigment paste so that the
mixture contains 1 part of dry color pigment to
10 parts of dry white pigment. For stronger or
weaker pigments this ratio may be adjusted
accordingly, for example, 1:20 or 1:5, respectively.
1 1.2 Weigh 500 k 2 mg of the standard color
pigment paste onto a glass slab. Then weigh the
amount of white pigment paste determined in
I 1.1, and place it next to the color pigment paste
on the glass slab. Thoroughly mix the two pastes
together with the spatula until a uniform color is
observed.
11.3 Prepare a tint mixture of the test color
pigment paste and the white pigment paste on a
separate glass slab by the procedure described in
11.2.
I I .4 Draw a portion of the test and standard
tint pastes down in juxtaposition on a paper chart
as in 10.1, Evaluate the color difference visually
as in 10.2 and, if desired, instrumentally as in
10.3. Clean the spatula blade and glass slabs.
12. Calculation of Tinting Strength
12. I If the colors of the test tint paste and the
standard tint paste are visually the same, the
tinting strength of the test pigment is equal to
that of the standard pigment, and the relative
tinting strength of the test pigment is 100%.
However, if the test and standard colors are not
the same, the difference may be due to tinting
strength or hue (shade).
12.2 To determine the relative tinting strength
of the test pigment, repeat the operations of
Section 11, but this time use an amount of the
test pigment paste that is estimated to give the
closest color match to the * standard pigment
paste. Repeat this procedure until satisfied that
the closest color match has been obtained. At
this point any residual color difference between
the test and the standard pigments is attributed
to a shade difference, rather than a strength difference.
Note and record this shade difference.
_

D 387
12.3 Calculate the relative tinting strength of
the test pigment by dividing the mass of the
standard paste by the mass of the test paste used
to obtain the closest color match; multiply by
100 to express the result in percent.
12.4 If desired, the relative tinting strength of
the sample pigment can be calculated from instrumental
measurements (see Test Method E 97
or Practice E 308) using the following equation:
TS = [( 1 - R,)’/2Rm]u/[( 1 - Rm)2/2Rm]s (T)
where:
TS = tinting strength of test pigment,
R, = measured reflectant factor (as a decimal),
T = assigned tinting strength of standard,
usually 100 %, and subscripts “u” and
“s” refer to the test and standard pigments,
respectively.
12.4.1 For R, use the lowest reflectance value
measured in the range 420 to 680 nm with a
spectrophotometer or abridged spectrophotometer.
This method of calculation is not valid when
any tristimulus value or filter colorimeter reading
is substituted for R, unless it can be demonstrated
that with such a substitution the function
(1 - Rm)*/2R, still varies linearly with concentration
for the pigments being tested over the
range of concentrations of interest. Because the
use of different parameters may give significantly
different results for the tinting strength, the
choice of the parameter to be used as R, shall be
agreed on between the purchaser and the seller.
NOTE 7-This method is not applicable to metameric
specimens, or to specimens exhibiting large
shade differences, or to specimens differing in
strength by more than about 30 %.
13. Report
13. I Report the following information:
13.1.1 Type and identification of the test pigment,
reference standard pigment, white tinting
pigment, and dispersing vehicle.
13.1.2 Mass ratio of pigment to vehicle, and
for tints mass ratio of color pigment mass to
white pigment.
13.1.3 Manufacturer and model number of
the mechanical muller employed.
13.1.4 Total force applied to the muller plates
and total number of revolutions.
13.1.5 Results of the visual evaluation of the
color difference (masstone and tint) in accordance
with Practice D 1729.
13.1.6 If an instrument was used to evaluate
the color difference, the results of the instrumental
evaluation in accordance with Test Method
D 2244.
13.1.7 Relative tinting strength and method
by which it was determined (visual or instrumental).
Also, for the instrumental method, the parameter
used as the measure of R,.
13.1.8 Any deviation, by agreement or otherwise,
from the test procedure described above.
14. Precision
14.1 The precision of this test method depends
on several factors such as the type of
pigment. the level of tinting, and the magnitude
and direction of the color difference. This point
is illustrated by the results in Table I(& which
contains the between-laboratories standard deviations
obtained in an interlaboratory study involving
five different laboratories and four different
pigments. The dispersing conditions used to
obtain these results are listed in Table 2.
14.2 Table l(b) lists the maximum acceptable
differences, calculated at the 95 % confidence
level from the results in Table l(a).
ANNEX
(Mandatory Information)
Al. DISPERSING CONDITIONS FOR MAXIMUM TINTING STRENGTH
A1.I The following describes a test method for determining
the conditions for achieving the maximum
level of tinting strength with the mechanical muller.
A I .2 Determine the appr6priate ratio of color pigment
to dispersing vehicle by performing the following
operations: Tare off the weight of a lass slab on
a balance. Weigh 1.00 f 0.01 g of t a e standard
pigment on to the glass slab. Add dispersing vehicle
to the pigment in small amounts and mix them
together with the spatula. Keep adding the vehicle
and mixing the paste until the pigment is completely
wetted and a workable paste is obtained. At this point
the consistency of the paste should be such that a dab
of the paste will drop from the spatula when it is
gently tapped with the finger. Weigh the paste, and
subtract the mass of the pigment to determine the
109

mass of the vehicle. Calculate the pigment to vehicle
mass ratio. Repeat the operations described above
for the test pigment.
A1.3 Determine the appropriate amount of pigment
to use by estimating, to within 0.2 mL, the
volume of that paste prepared in A 1.2 that has the
smallest pigment-to-vehicle mass ratio. Calculate the
masses of pigment and vehicle needed to give a paste
having a volume of about 2.0 mL. Round the amount
of pigment down and the amount of vehicle up to
the nearest 0.1 g.
A 1.4 Apply 100 Ibf (440 N) to the muller plates and
prepare a tint of the standard pigment in accordance
with the procedure in Sections 9 and 11. Use the
amounts of the color pigment and dispersing vehicle
determined in A 1.3 and mull the paste for 100 revolutions
in two stages of 50 revolutions each.
A 1.5 Prepare three more specimens from the same
sample following the procedure described in A 1.4,
but mull these specimens, in stages of 50 revolutions,
for 200,300, and 400 revolutions, respectively.
A1.6 Compare each of the four specimens, one to
the other, for tinting strength using one of the methods
described in Section 12, and determine the minimum
number of revolutions necessary to achieve full tinting
strength. If the tinting strength is still developing after
400 revolutions, repeat A1.4 to A1.6 with 50 lbf (220
N) more force on the mechanical muller plates.
A1.7 Record the appropriate amounts of pigment
and vehicle (by Al.3), the force applied to the mechanical
muller plates and the minimum number of revolutions
required for maximum tinting strength.
A 1.8 Table 2 lists, as examples, the dispersing conditions
used in the interlaboratory study that established
the precision given in Tables l(a) and l(h). The vehicle
used was No. 1 lithographic varnish with 0.8 % each of
cobalt and manganese driers (6 % types).
TABLE I(a)
Pigment Type
Between-Laboratories Standard Deviations for Various Color Difference" and Tinting Strength' Parameters
Masstone Color Tint Color Tinting Strength
____
Pa Ab AL AE Aa Ab AL AE Y T R V
Yellow Iron Oxide 0.10 0.46 0.22 0.42 0.13 0.20 0.19 0.08 2.0 2.2 3.0 0.7
BON Red 0.12 0.37 0.20 0.28 0.29 0.31 0.07 0.24 0.7 1.8 1.1 2.5
Molybdate Orange 0.09 0.14 0.06 0.1 I 0.11 0.12 0.05 0.14 0.5 0.8 0.6 1.0
PhthalocyanineGreenC 0.29 0.65 1.43 0.51 0.25 0.07 0.13 0.21 1.6 1.8 2.6 1.8
TABLE I(b) Maximum Acceptable Differences for Various Color DifferenceA and Tinting Strength' Parameters
Pigment Type
Masstone Color Tint Color Tinting Strength
--_________ ~
Aa Ab AL AE Aa Ab AI, AE Y T R V
~
Yellow Iron Oxide 0.28 1.30 0.62 1.19 0.37 0.57 0.54 0.23 5.7 6.2 8.5 2.0
BON Red 0.34 1.05 0.57 0.79 0.82 0.88 0.20 0.68 2.0 5.1 3.1 7.1
Molybdate Orange 0.25 0.40 0.17 0.31 0.31 0.34 0.14 0.40 1.4 2.3 1.7 2.8
Pthalocyanine Green'' 0.82 1.84 4.04 1.44 0.71 0.20 0.37 0.59 4.5 5.1 7.4 5.1
" Color difference values were calculated with the CIE 1976 L*a*b* (CIELAB) equation.
'Tinting strengths were calculated four different ways with the equation in 12.2: Y, based on Y tristimulus value; T, based on
lowest tristimulus value: R. based on lowest reflectance factor between 420 nm and 680 nm; and I.'. based on visual observation.
'Severe bronzing occurred with the masstone of this pigment (more in the batch than the standard), which probably affected the
color difference measurements made with different types of instruments.
Pigment type
TABLE 2 Dispersing Conditions Used in Interlaboratory Study
Pthalocyanine Yellow Iron BON Red Molybdate
Green Oxide Oranee - - ___
0-
Force applied to the muller plates, Ib (N) 100 (440) loo (440) loo (440) 100 (440)
Total number of revolutions 400 (8 x 50) 100 (2 x 50) 200 (4 x 50) 100 (2 x 50)
Mass of color pigment, g 0.15 I .o 0.6 2.0
Mass of dispersing vehicle, g I .8 I .7 I .4 1 .o
The American Societyfor Testing and Materials takes no position respecting the validity of any patent rights asserted in
conneetior: with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity
of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you fie1 that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards. 1916 Race St.. Philadelphia, PA 19103.
110

Designation: D 522 - 85
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appeaf in the next edition.
Standard Test Method for
ELONGATION OF ATTACHED ORGANIC COATINGS WITH
CONICAL MANDREL APPARATUS'
This standard is issued under the fixed designation D 522: the number immediately following the designation indicates the year of
original adoption or, in the case of revision. the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
T1ii.s iesi tnethod has been approvedjiw 11.~1~ by agencies of the Depariment of Defense to replace Method 6222 of Federul Tesi Meihod
Siuttdard No. 141.4 and,/i,r listing in the DoD Index of Specjficurions and Standards.
1. Scope
1.1 This test method covers the determination
by the conical mandrel test apparatus of the
elongation of attached coatings when applied to
flat sheet metal of uniform surface texture.
2. Applicable Documents
2.1 ASTM Standards:
A 109 Specification for Steel, Carbon, Cold-
Rolled Strip'
D823 Methods of Producing Films of Uniform
Thickness of Paint, Varnish, Lacquer,
and Related Products on Test Panels3
D 1 186 Method for Nondestructive Measurement
of Dry Film Thickness of Nonmagnetic
Coatings Applied to a Ferrous Base3
3. Summary of Method
3.1 The materials under test are applied at
uniform thickness to flat sheet metal panels.
After drying or curing, the panels are bent over
a conical mandrel. The elongation is determined
from the position of the first visible cracking
relative to the small end of the mandrel.
4. Significance and Use
4.1 Coatings attached to substrates are elongated
when the substrates are bent during the
manufacture of articles or when the articles are
abused in service. This test method has been
found useful in rating attached coatings for their
ability to resist cracking when elongated.
5. Apparatus
5.1 Conical Mandrel Te~ter,~ consisting of a
metal cone, a rotating panel bending arm, and
panel clamps, all mounted on a metal base as
illustrated in Fig. 1.
5.1.1 Cone, smooth steel, 8 in. (3.2 mm) in
length, with a diameter of I/s in. at one end and
a diameter of 11/2 in. (38 mm) at the other end.
6. Test Specimens
6.1 The base metal (Note 1) of the specimen
upon which the coating is applied shall be coldrolled
carbon steel strip '/3z in. (0.8 mm) thick
temper No. 5, edge No. 5, finish No. 2. The steel
used shall conform to the dimensional requirements
of Specification A 109. The dimensions of
the base metal shall be 4% in. (114 mm) in width,
with a maximum length Of 7% in. (177 mm) and
a maximum thickness of 1/32 in. (0.8 mm). The
surface preparation of the base metal shall be
agreed upon by the purchaser and the seller. Prior
to application of the finish Ehose edges of the
specimen that will be bent in the test shall be
rounded slightly to remove burrs in order to
eliminate anomalous effects associated with
cracking of a sharp metallic edge when bent over
the small end of the mandrel.
'This test method is under the jurisdiction of the ASTM
Committee D-l on Paint and Related Coatings and Materials
and is the direct responsibility of Subcommittee W1.23 on
Physical Properties of Applied Paint Films.
Current edition approved Sept. 27, 1985. Published November
1985. Originally published as D 522 - 39. Last previous
edition D 522 - 60 (I 979).
.4nniral Bmk 0/'.4STM Standards. Vol 0 I .03.
.Jnnital Book o/..ISTM Siandards. Vol 06.01.
'Suitable apparatus is available from Gardner/Neotec. Division
of Pacific Scientific Co.. I 100 East-West Highway, Silver
Spring. MD 20910 and from Paul N. Gardner Co.. 316 Northeast
First St., Pompano Beach, FL 33061-6688.
111

D 522
NOTE I-Other suitable materials for the test specimen
may be employed. The apparatus is designed for
testing metal panels having a maximum thickness of
'/32 in. (0.8 mm). The method for calculating the elongation
of coatings applied to base materials other than
the steel specified in Section 6 is contained in the
Appendix.
6.2 The coating under test shall be applied to
the clean base metal in accordance with Methods
D 823. The time between the application of the
coating and the testing of the specimen, as well
as the temperature and humidity environment
used for maturing the coating film during this
period, shall be agreed upon by the purchaser
and the seller.
7. Conditioning and Number of Tests
7.1 At least three replicate specimens shall be
tested under conditions of temperature and humidity
mutually agreed upon by the purchaser
and the seller. If it is desirable to check elongation
values at another time or place, the film thickness
and the temperature and humidity conditions at
the time of test shall be the same as those at
which the original determinations were made.
Unless otherwise specified by the purchaser and
the seller, elongation measurements shall be
made at 73.5 k 3.5"F (23 & 2°C) and 50 f 5 %
relative humidity after equilibrating the test specimens
to these conditions for at least 24 h.
8. Procedure
8. I With the operating lever of the apparatus
in a horizontal position, slip the test specimen
between the mandrel and the drawbar with the
finish side towards the drawbar and rigidly clamp
in a vertical position adjacent to the mandrel by
placing the long edge behind the clamping bar in
such a manner that the panel is always set up to
the narrow end of the mandrel. Slip two sheets
of No. 1 brown kraft wrapping paper, substance
30, thoroughly lubricated on each side with talc,
between the specimen and the drawbar and hold
in position only by the pressure of the drawbar
against the paper.
8.2 Move the lever through about 180" at
uniform velocity to bend the specimen approximately
135" in about 15 s (Note 2). Take care at
the end of the stroke so as not to unnecessarily
deform the specimen.
NOTE 2-To simulate some use conditions, it may
be desirable to bend the specimen approximately 135"
in I to 1.5 s. However, when this rapid rate of bending
is used, something other than elongation as defined in
this test method is being measured.
8.3 Examine the bent surface of the specimen
immediately with the unaided eye for cracking.
Having determined and suitably marked the end
of the crack farthest from the small end of the
mandrel, which shall be considered as the end
point, bring the drawbar to the starting position
and remove the panel from the mandrel. Measure
the distance from the farthest end of the
crack to the small end of the mandrel. If it is
desired to compare results with cylindrical mandrel
results, determine the mandrel diameter at
which cracking ceased.
8.4 Perform a minimum of three determinations
of the thickness of the coating on each of
the specimens in accordance with Method
D 1186. The mean value is used in calculating
elongation.
9. Calculation
9.1 Determine the elongation of the finish
from the plotted curve in Fig. 2. This curve
represents the relation between the percent of
elongation and the diameter of the conical mandrel
for a 1.0 mil coating thickness. The relation
between the distance along the conical mandrel
and the corresponding diameter has also been
plotted on this curve.
9.2 Adjust the percent elongation value obtained
from Fig. 2 for coating thickness by adding
the correction obtained from Fig. 3.
NOTE 3: Example-Suppose a visual examination
of the finish on the bent cold-rolled steel specimens %z
in. (0.8 mm) in thickness shows that the end of the first
crack in the coating is at a distance of 3 in. (75 mm)
from the small end of the cone. From Fig. 2 determine
the percent elongation of the film from the measured
crack distance, in this example 5.2 %. To correct for
coating thickness add the value obtained from Fig. 3.
At a crack distance of 3 in. the correction per mil (25
pm) of coating thickness is 0.3 %. If the film thickness
in the example IS 2 mils, the actual percent elongation
is 5.2 + (2 x 0.3) = 5.8 %.
10. Report
10.1 Report the following information:
10.1.1 Mean and range of coating elongation
values for each specimen.
10.1.3 Meart and range of coating film thickness
for each specimen.
10.1.3 Specimen preparation procedure used.
10.1.4 'fcst conditions.
112

(1m D522
10.1.5 Mean and range of elongation and film the precision of this test method. Plans are being
thickness for the replicate specimens.
made to obtain such results. This test method
has been in use for many years and is considered
11. Precision
acceptable for evaluating the crack resistance of
1 1.1 Results are not available to determine attached coatings.
FIG. 1 Conical Mandrel Test Apparatus
6
ELONOATION IN PER CENT
FIG. 2 Distance Along Cone and Corresponding Mandrel Size versus Percent Elongation for Specimens on Cold-Rolled Steel %z
in. (0.8 mm) in Thickness
113

0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 09 1.0 1.1 1.2 1.3 1.4 1.5 1.6
CORRECTION TO BE ADDED TO PER-CENT ELONOATION
FIG. 3 Correction for Thickness of Film
APPENDIX
(Nonmandatory Information)
X1. CALCULATION FROM MANDREL SIZE
X 1.1 Assuming elastic conditions of the base material
(which, of course, is not the case but is useful in
establishing a limiting condition), the theoretical elongation
for each mandrel size can be calculated. Under
this assumption the moduli of elasticity for tension and
compression are equal in magnitude and the neutral
plane (that is, the plane where the bent metal is neither
elongated nor compressed) is at the centroidal axis of
the specimen. In a strip having a thickness, I, bent
around a mandrel of radius, r, the neutral plane would
be located at a distance t/2 from the surface of the
metal, and the perimeter of the bent section along the
neutral axis, assuming the specimen to be bent through
I go", is equal to r(r + t/2). At the upper surface of the
metal, the perimeter would be equal to r(r + I), and
the elongation of its surface would be:
Elongation = r(r + t) - r(r + t/2)
Elongation = 7r(t/2)
and the percent elongation at the surface would be:
Elongation, % = [(rt/2) X 100]/7r(~ + t/2)
Elongation, % = [f/(2r +.!)I x !OO
X 1.2 Using this equation, the theoretical elongation
(under elastic conditions) at the surface of the specimen
can be calculated for any thickness of specimen and
mandrel size, resulting in the following values for three
specimen thicknesses and six mandrel sizes:
Elongation, %
Mandrel Size = 2r
Specimen 1 in. 3/4 in. V2 in. 3/n in. V4 in. '/a in.
Thickness. (25.4 (19 (12.7 (9.5 (6.4 (3.2
in. mm) mm) mm) mm) mm) mm)
f = 1/w(0.4 mm) 1.5 2.0 3.0 4.0 5.9 11.1
t = %2(0.8 mm) 3.0 4.0 5.9 7.7 11.1 20.0
r=%6(1.6mm) 5.9 7.7 11.1 14.3 20.0 33.3
X 1.3 Actually the specimens are elongated considerably
past their elastic limit, so that the elongations
obtained with the mandrel test are considerably higher
than the values calculated above. Since it is impossible
to calculate the position of the neutral plane when the
elastic limit has been exceeded, a special jig should be
used to measure the elongation directly.
X1.4 This jig (Fig. X1.1) consists of two forks for
holding the mandrel and specimen in position and a
roller with which the specimen is tightly wrapped
around and held against the mandrel.
X 1.5 Method of Measuring Elongation with Jig-
Two parallel gage scratches shall be made with a sharp
stylus on the edge of the specimen and so located that
when it is wrapped around the mandrel the included
angle between the scratches will be approximately 180".
In locating the scratches, it is necessary to make sure
that they will be within the section of the specimen
which after bending is tightly wrapped against the mandrel.
Having located the scratches, the linear distance
between them shall be measured to within 2 pm.5 The
specimen shall then be clamped in the jig and the roller
brought down tight against it. The roller shall then be
drawn around causing the specimen to be tightly
wrapped and secured against the surface ofthe mandrel.
In order to hold the jig in this position the forks shall
be held together with a C-clamp. The clamp jig shall
then be rigidly mounted on the table of the measuring
machine.' Each of the gage scratches shall then be made
to coincide with the vertical cross hair of the measuring
eyepiece while the horizontal cross hair is tangent to
the curvature ofthr upper surface of the specimen. The
angle reading shall be taken at each of these points. The
difference between the two angle readings is a measure
of the included angle formed by the two gage scratches
__
'A star comparator is suitable for this purpose.
114

D 522
and the radii drawn coincident with the scratches. The
angle readings shall be read in minutes and seconds to
a precision of &5 s. The total diameter of the mandrel
and the bent specimen shall also be determined. From
these data the percent elongation at the surface of the
specimen may be calculated as follows:
L = ar/ 180r
Elongation, ?6 = [(L - d)/dl x 100
where:
a = angle,",
L = arclength,
r = radius of curvature for system (mandrel radius +
1). and
d = original distance between scratches.
FIG. X1.1 Jig for Determining Elongation of Bent Metal Specimens
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any sirch
putent rights, and the risk of injringement of such rights. are entireiv their own responsibility.
This standard is subject 10 revision ut any time by the responsible technical commitree and must be reeiened everyjve years and
If not revised, either reupproved or withdrawn. Yoirr comments are invited either for revision of this standard or for additional
standards and shoitld be addressed to ASTM Heqdqirarters. Your comments nil receive carefitl consideration at a meeting of the
responsible technical committee, nhich voir may attend. If yoir feel that your comments have not received a fair hearing yoii shoitld
make voitr views known to the ASTM Committee on Standards. 1916 Race SI.. Philadelphia, PA 19103.
115

Designation: D 523 - 85"
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
SPECULAR GLOSS'
This standard is issued under the fixed designation D 523; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This fesi method has been approvedfor use by agencies offhe Deparfmenf of Dejhnse andfor lisfing in the DoD Index qfSpectficafions
and Standards.
'' NOTE-Paragraph 6.2. Note 3, and Figs. I and 2 were changed editorially in November 1986.
1. Scope
1.1 This test method covers the measurement
of the specular gloss of nonmetallic specimens
for glossmeter geometries of 60, 20, and 85" (1-
7).*
I .2 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the s&ty problems
associafed with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safity and health practices
and determine the applicability of regulatory limitalions
prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D823 Methods of Producing Films of Uniform
Thickness of Paint, Varnish, and Related
Products on Test Panels3
D 3964 Practice for Selection of Coating Specimens
for Appearance Measurement3
D 3980 Practice for Interlaboratory Testing of
Paints and Related Materials3
D4039 Test Method for Reflectioc Haze of
High-Gloss Surfaces3
E 97 Test Method for Directional Reflectance
Factor, 45-deg, 0-deg of Opaque Specimens
by Broad-Band Filter Reflectometry3
E 430 Method for Measurement of Gloss of
High-Gloss Surfaces by Goni~photometry~
3. Definitions
3.1 gloss, specular-the relative luminous reflectance
factor of a specimen in the mirror direction.
3.2 relative luminous reflectance factor-the
ratio of the luminous flux reflected from a specimen
to the luminous flux reflected from a standard
surface under the same geometric conditions.
For the purpose of measuring specular gloss, the
standard surface is polished glass.
4. Summary of Method
4.1 Measurements are made with 60, 20, or
85" geometry (8,9). The geometry of angles and
apertures is chosen so that these procedures may
be used as follows:
4.1.1 The 60" geometry is used for intercomparing
most specimens and for determining when
the 20" geometry may be more applicable.
4.1.2 The 20" geometry is advantageous for
comparing specimens having 60" gloss higher
than 70.
4.1.3 The 85" geometry is used for comparing
specimens for sheen or near-grazing shininess. It
is most frequently applied when specimens have
60" gloss values lower than IO.
5. Significance and Use
5,l Gloss is associated with the capacity of a
surface to reflect more light in some directions
than in others. The directions associated with
' This test method is under the jurisdiction of ASTM Committee
D- I on Paint and Related Coatings and Materials and is
the direct responsibility of Subcommittee WI .26 on Optical
Properties.
Current edition approved Sept. 27, 1985. Published November
1985. Originally published as D 523 - 39 T. Last previous
edition D 523 - 80.
'The boldface numbers in parentheses rerer to the list of
references at the end of this test method.
Annual Book (?f ASTM Standards. Vol 06.0 I .
' Anntrul Book ofASTM Siandards. Vol 14.02.
116

D 523
mirror (or specular) reflection normally have the
highest reflectances. Measurements by this test
method correlate with visual observations of surface
shininess made at roughly the corresponding
angles.
5.1.1 Measured gloss ratings by this test
method are obtained by comparing the specular
reflectance from the specimen to that from a
black glass standard. Since specular reflectance
depends also on the surface refractive index of
the specimen, the measured gloss ratings change
as the surface refractive index changes. In obtaining
the visual gloss ratings, however, it is customary
to compare the specular reflectances of two
specimens having similar surface refractive indices.
Since the instrumental ratings are affected
more than the visual ratings by changes in surface
refractive index, non-agreement between visual
and instrumental gloss ratings can occur when
high gloss specimen surfaces differing in refractive
index are compared.
5.2 Other visual aspects of surface appearance,
such as distinctness of reflected images, reflection
haze, and texture, are frequently involved in the
assessment of gloss (I), (6), (7). Method E430
includes techniques for the measurement of both
distinctness-of-image gloss and reflection haze.
Test Method D 4039 provides an alternative procedure
for measuring reflection haze.
5.3 Little is known about the relations of numerical-to-perceptual
intervals of specular gloss.
It is probable that, within the middle-scale ranges
(for example, 10 to 60), perceived specular gloss
differences correspond more closely to differences
in ratios of gloss values than to differences
in numerical magnitudes of gloss.
6. Apparatus'
6.1 lnstrumental Components-The apparatus
shall consist of an incandescent light source
furnishing an incident beam. means for locating
the surface of the specimen, and a receptor located
to receive the required pyramid of rays
reflected by the specimen. The receptor shall be
a photosensitive device responding to visible radiation.
6.2 Geometric Conditions-The axis of the
incident beam shall be at one of the specified
angles from the perpendicular to the specimen
surface. The axis of the receptor shall be at the
mirror reflection of the axis of the incident beam.
The axis of the incident beam and the axis of the
receptor shall be within 0.1 O of the nominal value
indicated by the geometry. With a flat piece of
polished black glass or other front-surface mirror
in the specimen position, an image of the source
shall be formed at the center of the receptor field
stop (receptor window). The length of the illuminated
area of the specimen shall be not more
than one third of the distance from the center of
this area to the receptor field stop. The dimensions
and tolerance of the source and receptor
shall be as indicated in Table 1. The angular
dimensions of the receptor field stop are measured
from the receptor lens in a collimatedbeam-type
instrument, as illustrated in Fig. 1,
and from the test surface in a converging-beamtype
instrument, as illustrated in Fig. 2. See Figs.
1 and 2 for a generalized illustration of the dimensions.
The tolerances are chosen so that errors
in the source and receptor apertures do not
produce an error of more than one gloss unit at
any point on the scale. (5).
6.2.1 The important geometric dimensions of
any specular-gloss measurement are:
6.2.1.1 Beam axis angle(s), usually 60, 20, or
85".
6.2.1.2 Accepted angular divergences from
principal rays (degree of spizading or diffusion
of the reflected beam).
NOTE I -The parallel-beam glossmeters possess the
better uniformity of principle-ray angle of reflection,
but the converging-beam glossmeters possess the better
uniformity in extent of angular divergence accepted for
measurement.
NOTE 2--Po/uri~u~ion--An evaluation of the impact
of polarization on gloss measurement has been
reported (10). The magnitude of the polarization error
depends on the difference between the refractive indices
of specimen and standard, the angle of incidence. and
the degree of polarization. Because the specimen and
standard are generally quite similar optically, measured
gloss values are little affected by polarization.
6.3 Vignefting-There shall be no vignetting
of rays that lie within the field angles specified in
Table 1.
6.4 Spectral Conditions-Results should not
differ significantly from those obtained with a
source-filter photocell combination that is spectrally
corrected to yield CIE luminous efficiency
with CIE source C. Since specular reflection is,
in general, spectrally nonselective, spectral cor-
' A list of manufacturerers of glossmeters can be obtained
from ASTM Headquarters.
117

D 523
rections need to be applied only to highly chromatic,
low-gloss specimens upon agreement of
users of this test method.
6.5 Measurement Mechanism-The receptormeasurement
mechanism shall give a numerical
indication that is proportional to the light flux
passing the receptor field stop with +1 % of fullscale
reading.
7. Reference Standards
7.1 Primary Standards-Highly polished,
plane, black glass with a refractive index of 1.567
for the sodium D line shall be assigned a specular
gloss value of 100 for each geometry. The gloss
value for glass of any other refractive index can
be computed from the Fresnel equation (5). For
small differences in refractive index, however,
the gloss value is a linear function of index, but
the rate of change of gloss with index is different
for each geometry. Each 0.001 increment in refractive
index produces a change of 0.27, 0.16,
and 0.0 I6 in the gloss value assigned to a polished
standard for the 20, 60, and 85" geometries,
respectively. For example, glass of index 1.527
would be assigned values of 89.2,93.6, and 99.4,
in order of increasing geometry.
NOTE 3-Polished black glass has been reported to
change in refractive index with time largely due to
chemical contamination (IO). The original values can
be restored by optical polishing with cerium oxide. A
wedge of high-purity quartz provides a more stable
reference standard than glass.
7.2 Working Srandards6-Ceramic tile, depolished
ground opaque glass, emery paper, and
other semigloss materials having hard and uniform
surfaces are suitable when calibrated against
a primary standard on a glossmeter known to
meet the requirements of this test method. Such
standards should be checked periodically for constancy
by comparing with primary standards.
7.3 Store standards in a closed container when
not in use. Keep them clean and away from any
dirt that might scratch or mar their surfaces.
Never place standards face down on a surface
that may be dirty or abrasive. Always hold standards
at the side edges to avoid getting oil from
the skin on the standard surface. Clean the standards
in warm water and a mild detergent solution
brushing gently with a soft nylon brush. (Do not
use soap solutions to clean standards, because
they can leave a film.) Rinse standards in hot
running water (temperature near 150°F (65°C) to
remove detergent solution, followed by a final
rinse in distilled water. Do not wipe standards.
The polished black glass high-gloss standard may
be dabbed gently with a lint-free paper towel or
other lint-free absorbent material. Place the
rinsed standards in a warm oven to dry.
8. Preparation and Selection of Test Specimens
8.1 This test method does not cover preparation
techniques. Whenever a test for gloss requires
the preparation of test specimens, use the
procedures given in Methods D 823.
NOTE 4-To determine the maximum gloss obtainable
from a test material, such as a paint or varnish,
use Methods B or C of Methods D 823.
8.2 Select specimens in accordance with Practice
D 3964.
9. Instrument Calibration
9. I Operate the glossmeter in accordance with
the manufacturer's instructions.
9.2 Verify the instrument zero by placing a
black cavity in the specified position. If the reading
is not within +O. 1 of zero, subtract it algebraically
from subsequent readings or adjust the
instrument to read zero.
9.3 Calibrate the instrument at the start and
completion of every period of glossmeter operation,
and during the operation at sufficiently
frequent intervals to assure that the instrument
response is practically constant. To calibrate, adjust
the instrument to read correctly the gloss of
a highly polished standard, properly positioned
and oriented, and then read the gloss of a working
standard in the mid-gloss range. If the instrument
reading for the second standard does not agree
within one unit of its assigned values, check
cleanliness and repeat. If the instrument reading
for the second standard still does not agree within
one unit of its assigned value, repeat with another
mid-range standard. If the disparity is still more
than one unit, do not use the instrument without
readjustment, preferably by the manufacturer.
10. Procedure
10.1 Position each specimen in turn beneath
(or on) the glossmeter. For specimens with brush
Gloss standards are available from: Gardner/Neotec, Division
of Pacific Scientific Co., 2431 Linden Lane, Silver Spring,
MD 20910 Byk-Chemie USA, Inc., 524 South Cherry St.,
Wallingford. CT 06492; and Hunter Associates Laboratory. Inc.,
I I495 Sunset Hills Road, Reston. VA 22090.
118

I
D 523
marks or similar texture effects, place them in
such a way that the directions of the marks are
parallel to the plane of the axes of the incident
and reflected beams.
10.2 Take at least three readings on a 3 by 6-
in. (75 by 150-mm) area of the test specimen. If
the range is greater than two gloss units, take
additional readings and calculate the mean after
discarding divergent results as in the section on
Test for Outliers of Practice D 3980. For larger
specimens, take a proportionately greater number
of readings.
11. Diffuse Correction
11.1 Apply diffuse corrections only upon
agreement between the producer and the user.
To apply the correction, subtract it from the
glossmeter reading. To measure the correction,
illuminate the specimen perpendicularly and
view at the incident angle with the receiver a p
erture specified in 6.2 for the corresponding geometry.
To compute the correction, multiply the
45', 0" directional reflectance of the specimen,
determined in accordance with Test Method
E97, by the effective fraction of the luminous
flux reflected by the perfect diffuse reflector and
accepted by the receiver aperture. The luminous
flux entering the receiver aperture from the perfect
white diffusor would give the following gloss
indications for each of the geometries:
12 Report
Geometry, *
Gloss of Perfect White Diffuser
60 2.5
20 1.2
85 0.03
12.1 Report the following:
12.1.1 Mean specular gloss readings and the
geometry used.
12.1.2 If uniformity of surface is of interest,
the presence of any specimen that exhibits gloss
readings varying by more than 5 % from their
mean.
12.1.3 Where preparation of the test specimen
has been necessary, a description or identification
of the method of preparation.
12.1.4 Manufacturer's name and model designation
of the glossmeter.
12.1.5 Working standard or standards of gloss
used.
13. Precision
13.1 On the basis of studies of this test method
by several laboratories in which single determinations
were made on different days on several
ceramic tiles and painted panels differing in visually
perceived gloss, the pooled within-laboratory
and between-laboratories standard deviations
were found to be those shown in Table 2.
Based on these standard deviations, the following
criteria should be used for judging the acceptability
of results at the 95 % confidence level:
13.1.1 Repeatability-Two results, each of
which are single determinations obtained on the
same specimen by the same operator, should be
considered suspect if they differ by more than
the maximum acceptable differences given in
Table 3.
13.1.2 Reproducibility-Two results, each the
mean of three determinations, obtained on the
Jame specimen by different laboratories should
be considered suspect if they differ by more than
the maximum acceptable differences given in
Table 3. This does not include variability due to
preparation' of panels in different laboratories.
NOTE 5-For some types of paint, particularly semigloss,
the measured gloss is affected by method of film
preparation and drying conditions so that the reproducibility
of results from such materials may be poorer
than the values given in Table 3.
119

D523
TABLE 1 Angles and Relative Dimensions of Source Image and Receptors
In Plane of
Measurement
Perpendicular to
Plane of Measurement
Relative
Relative
8, tan 8’2 Dimension 8, tan e’2 Dimension
Source image 0.75 0.0131 0.171 2.5 0.0436 0.568
Tolerance * 0.25 0.0044 0.057 0.5 0.0087 0.1 14
60’ receptor 4.4 0.0768 I .000 11.7 0.2049 2.668
Tolerance ? 0.1 0.00 I8 0.023 0.2 0.0035 0.046
20’ receptor 1.8 0.03 14 0.409 3.6 0.0629 0.819
Tolerance +- 0.05 0.0009 0.0 12 0. I 0.0018 0.023
85” receptor 4.0 0.0698 0.909 6.0 0.1048 I .365
Tolerance ? 0.3 0.0052 0.068 0.3 0.0052 0.068
Type of
Gloss, *
TABLE 2 Standard Deviations of Gloss Determinations
No. of
Degrees of Freedom
Standard Deviations
Ceramic Within- Between-
Within-
Between-
Tiles Laboratory Laboratories Laboratory‘ Laboratories’
20 4 40 34 0.4 I .2
60 4 40 34 0.3 I .2
85 2 16 6 0.2 0.6
Type 0.f
Gloss.
No. of
Degrees of Freedom
Standard Deviations
Painted Within- Between- Within- Between-
Panels Laboratory Laboratories Laboratory‘ Laboratories’
20 8 no 72 0.6
60 22 220 I36 0.3
85 6 48 18 0.3
” Single determinations.
’ For means of three determinations
2.2
I .2
2.4
TABLE 3 Maximum Acceptable Differences for Two
Results
Repeatability Reproducibility
Type of
(Within Laboratoriesy
(Between Laboratories)’
Gloss.
Ceramic Painted Ceramic Painted
Tiles Panels Tiles Panels
’0 1.1 I .7 3.5 6.4
60 0.9 0.9 3.4 3.5
85 0.6 0.8 2.0 7.2
A Singie determinations.
*For means of three determinations.
120

D523
TEST
SPECIMEN t- RECEPTOR LEN<
:----A
RECEPTOR FIELD ANGLE
SPECTRAL CORRECTION FILTER
PHOTO DETECTOR
FIG. 1
Diagram of Parallel-Beam Glossmeter Showing Apertures and Source Mirror-Image Position
TEST
CONDENSER
LENS
J-
INCIDENCE ANGLE‘
/”
zniiar
.LE ......._.
-_
\- SOURCE FIELD APERTURE
SOURCE
‘vIENIN ANGLE
SPECTRAL
CORRECTION FILTER
I
PHOTODETECTOR 2
FIG. 2 Diagram of Converging-Beam Glossmeter Showing Apertures and Source Mirror-Image Position
121

@ D523
REFERENCES
(1) Hunter, R. S., “Methods of Determining Gloss,”
Proceedings, ASTM, Vol36, 1936, Part 11, p. 783.
Also, Journal of Research, Nat. Bureau Standards,
Vol 18, No. I, January 1937, p. 19 (Research
Paper RP958). Six somewhat different appearance
attributes are shown to be variously associated
with gloss. Therefore, as many as six different
photometric scales may be required to handle all
gloss measurement problems. (This paper is out
of print).
(2) Hunter, R. S., and Judd, D. B., “Development of
a Method of Classifying Paint According to
Gloss,” ASTM Bulletin, No. 97, March 1939, p.
1 1. A comparison is made of several geometrically
different photometric scales for separating paint
finishes for gloss. The geometric conditions of test
later incorporated in Test Method D 523 are recommended.
(3) Wetlaufer, L. A.. and Scott, W. E., “The Measurement
of Gloss,” Industrial and Engineering
Chemistry, Analytical Edition, Vol 12, November
1940, p. 647. A goniophotometric study of a
number of paint finishes illuminated at 45”; a
study of gloss readings affected by variation of
aperture for 45 and 60” incidence.
(4) Hunter, R. S., “The Gloss Measurement of Paint
Finishes,” ASTM Bulletin, No. 150, January
1948. p. 72. History of Test Method D 523.
(5) Hammond, H. K., 111, and Nimerroff. 1.. “Measurement
of Sixty-Degree Specular Gloss.” Journal
q/Rt.search. Nat. Bureau Standards. A study
of the effect of aperture variation on glossmeter
readings. including definitions of terms used in
connection with specular gloss measurement, the
Fresnel equation in a form readily usable for
computation, and the deviation of diffuse correction
formulas.
(6) Hunter, R. S., “Gloss Evaluation of Materials,”
ASTM Bulletin, No. 186, December 1952, p. 48.
A study of the history of gloss methods in ASTM
and other societies, describing the background in
the choice of geometry of these methods. Contains
photographs depicting gloss characteristics of a
variety of methods.
(7) Hunter, R. S., The Measurment of Appearance,
Wiley-Interscience, New York, 1975, Chapter 6.
“Scales for Gloss and Other Geometric Attributes,”
and Chapter 13, “Instruments for the Geometric
Attributes of Object Appearance.”
(8) Horning. S. C., and Morse, M. P., “Measurement
of the Gloss of Paint Panels,” Oflcial Digest,
Federation of Paint and Varnish Production
Clubs, March 1947, p. 153. A study of the effect
of geometric conditions on results of gloss tests
with special attention to high-gloss panels.
(9) Huey, S.. Hunter, R. S., Schreckendgust. J. G..
and Hammond. H. K.. 111, “Symposium on Gloss
Measurement.” O[/k*ial Digest, Vol 36, No. 47 1.
April 1964. p. 343. Contains discussion of industrial
experience in measurement of 60” specular
gloss (Huey). high-gloss measurement (Hunter),
evaluation of low-gloss finishes with 85” sheen
measurements (Schreckendgust), and gloss standards
and glossmeter standardization (Hammond).
(IO) Budde. W.. “Stability Problems in Gloss Measurements,”
Joirrnul (?/‘Coatings Teclinologv. Vol 52.
June 1980, pp. 44-48.
The American Societyji)r Testing and Materials iaki.s no position respecting the validity ofany paient rights assertc~d in conncwion
with ani‘ item mcwtioned in this standard. U.7er.s qf this standard are evpriwly advised thar determination of the validity of any siich
patent rights. and [he risk of infiingcvnent of such rights. art entirely their ow responsibility.
This standard is siibjiw to rcvision at any lime hy [hi> riqwnsihle technical committee and miist he revitwed ewrj*jivc years and
If nor riviscd. eiihvr reapproved or withdrawn. Your c”wni.7 are invitcd pither .for revision of this standard or ji)r udditional
standards and shoiild hi. addrc.ssi.d to ASTM Heudquarter.s. Your commcnt.7 uill receive cari:/iil consideration ut a tncvting ofthe
re~sponsihlc, technical twnmiircv. which you muj, attend. lf,soii,fivl ihat yoiir commenis have not received a juir hiwring you slioiild
makii j *ow view knoun to the ASTM Committcv on Standards. 1916 Race SI.. Philaddphia. PA 1910-3.
122

ds[b L-9 ANSVASTM D 542 - 50 (Reapproved 1977)c
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Methods for
INDEX OF REFRACTION OF TRANSPARENT
ORGANIC PLASTICS'
This Standard is issued under the fixed designation D 542; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of
last reapproval.
This method has been approved for use by agencies of the Department of Defense to replnce method 3011 of Federal Test
Method Standard 406, and for listing in the DoD Index of Specifications and Standards.
Nom-Sections 1 and 6 were changed editorially in May 1977.
1- scope
1.1 These methods cover the measurement
of the index of refraction of transparent organic
plastic materials.
1.2 Two procedures, refractometric and
microscopical methods, are proposed in order
to cover satisfactorily the maximum range of
indices found in these materials. Both methods
require optically homogeneous specimens
of uniform index for ease of duplicability. The
refractometric method is to be preferred
wherever it is applicable.
NOTE ]-The values stated in SI units are to be
regarded as the standard.
2. Significance
2.1 This test measures a fundamental property
of matter useful for control of purity and
composition, for simple identification purposes
and for optical parts design. It is capable
of much greater precision than ordinarily
required. The refractometric method is accurate
to four significant figures. The microscopical
method, which is dependent upon the operator's
skill in determining f~cus, is usaa!!y
accurate to only three significant figures.
3. Conditioning
3.1 Conditioning-Condition the test specimens
at 23 f 2 C (73.4 f 3.6 F) and 50 f 5
percent relative humidity for not less than 40
h prior to test in accordance with Procedure A
of ASTM Methods D 618, Conditioning Plastics
and Electrical Insulating Materials for
Testing,' for those tests where conditioning is
required. In cases of disagreement, the tolerances
shall be 1 C (1.8 F) and =t2 percent relative
humidity .
3.2 Test Conditions-Conduct tests in the
Standard Laboratory Atmosphere of 23 f
2C (73.4 f 3.6F) and 50 f 5 percent relative
humidity, unless otherwise specified in
the test methods or in this specification. In
cases of disagreements, the tolerances shall be
1 C (1.8 F) and &2 percent relative humidity.
If a material is found to have a high thermal
coefficient of index, the temperature shall be
accurately controlled to 23 C.
REFRACTOMETRIC METHOD
4. Apparatus
4.1 The apparatus for the preferred method
shall consist of an Ab& refractometer (Note
2), a suitable source of white light, and a
small quantity of a suitable contacting liquid
(Notes 3 and 4).
NOTE 2-Other suitable refractometers can be
used with appropriate modification of procedure as
described in Section 6.
NOTE 3-4 satisfactory contacting liquid is one
which will not soften or otherwise attack the surface
of the plastic within a period of 2 h of contact. The
index of refraction of the liquid must be higher, by
not less than one unit in the second decimal place,
than the index of the plastic being measured.
The following liquids are suggested:
'These methods are under the jurisdiction of ASTM
Committee D-20 on Plastics ana are the direct responsibility
of Suocommittee D-20.40 on Optical Properties.
Current edition effective Sept. 30, 1950. Originally issued
1939. Replaces D 542 - 42.
Annual Book o/ ASTM Standards, Part 35.
I23

D 542
Phenol
resin
Plastic
formaldehyde
Cellulose acetate and
cellulose nitrate
Acrylic resins
Vinyl resins"
Styrene resins
Contacting Liquid
a-bromnaphthalene
{
cassia oil
aniseed oil
a-bromnaphthalene
saturated aqueous sohtion
of zinc chloride
made slightly acid
a-monobromnaph thalene
saturated aqueous solution
of potassium mercuric
iodide (Thoulet's or
Sonstadt's solution)'
" No liquid has been found to date which is entirfly
satisfact0r.y for vinyl resins.
Avoid contact of this liquid with the skin or prolonged
contact with the metal parts of the refractometer.
NOTE &In many cases a liquid as suggested
above is not available and a second rapid reading
must be made on a fresh specimen after preliminary
trial.
5. Test Specimen
5.1 The test specimen shall be of a size
such as will conveniently fit on the face of the
fixed half of the refractometer prisms (Note 5).
A specimen measuring 6.3 mm (0.25 in.) by
12.7 mm (0.5 in.) on one face is usually satisfactory.
NOTE %For maximum accuracy in the refractometer
method the surface contacting the prism shall
be quite flat. This surface can be judged for flatness,
provided the specimen has been satisfactorily polished,
by observing the sharpness of the dividing
line between the light and dark field. A sharp,
straight dividing line indicates a satisfactory contact
of the specimen and prism surfaces.
5.2 The surface to be used in contact with
the prism shall be flat and shall have a good
polish. A second edge surface perpendicular
to the first and on one end of the specimen
shall be prepared with a fair polish (Note 6).
The polished surfaces shall intersect without a
beveled or rounded edge.
NoTEGI~ has been found possible to prepare a
satisfactorily polished surface by hand polishing
small specimens on an abrasive material backed by
a piece of plate glass. Fine emery paper (for example,
No. OOO Behr-Manning polishing paper) followed
by a polishing rouge suspended in water on a
piece of parchment paper have been used as the
abrasive.
6. Procedure
6.1 Remove the hinged illuminating prism
from the refractometer, if necessary. Place a
source of diffuse light so that good illumination
is obtained along the plane of the surface
of contact between the specimen and the refractometer
prism. Place a small drop of a
suitable contacting liquid on the polished surface
of the specimen and then place the specimen
in firm contact with the surface of the
prism and with the polished edge of the specimen
toward the source of light. Determine the
index of refraction in the same manner as for
liquids. This shall be done by moving the index
arm of the refractometer until the field
seen through the eyepiece is one-half dark.
Adjust the compensator (Amici prisms) drum
to remove all color from the field. Adjust the
index arm by means of the vernier until the
dividing line between the light and dark portions
of the field exactly coincides with the
intersection of the cross hairs as seen in the
eyepiece. Read the value of the index of refraction
for the sodium D lines. Determine
the dispersion by reading the compensator
drum and applying this figure, along with the
index of refraction, to a chart or table supplied
with the instrument.
NOTE 7-Sodium light from some type of a sodium
burner is of use in increasing the accuracy and
ease of setting of the refractometer.
MICROSCOPICAL METHOD
7. Apparatus
7.1 The apparatus for the auxiliary method
shall consist of a microscope having a magnifying
power of at least 200 diameters. This
microscope shall be equipped with a means of
measuring the longitudinal travel of the lens
tube to within 0.025 mm (0.001 in.).
8. Test Specimens
8.1 The specimen described in Sectinn 5
will be satisfactory for use with the microscopical
method if it is not too thick to permit
focusing the microscope through the polished
surface (having a fair polish). A small specimen
taken from a sheet of the material may
be used if it is about 6.3 mm (0.25 in.) in
thickness.
9. Procedure
9.1 Place a specimen having two parallel
surfaces on the measuring microscope table
124

D 542
with that surface having the best polish placed
nearest to the objective. Focus the microscope
through the specimen and on the bottom surface.
Note the reading of the longitudinal displacement
of the lens tube to the nearest 0.025
mm (0.001 in.) or less. Without moving the
specimen, focus the microscope on the top
surface of the specimen and again note the
reading of the displacement. The difference
between these two readings is the apparent
thickness of the specimen. The index of refraction
is found by dividing the actual thickness
of the specimen by the apparent thickness.
10. Report
10.1 The report shall include the following:
10.1.1 The name of the method used.
10.1.2 The index of refraction to the nearest
significant figure warranted by the accuracy
and duplicability of the measurement. If
the index is specified to more than three significant
figures, the wave length of light for
which the measurement was made shall be
specified.
NOTE 8-In the case of nonisotropic materials,
for example injection and compression molded ma-
terials. the index observed by the AbbC refractometer
method will be the average value for a thin layer
of small area at a point of contact near the center of
the refractometer prism. For a complete and accurate
determination of the variation of the index
throughout the test specimen it is necessary to make
the measurement at more than one point on the surface
and within the body of the material. This can
be done by preparing a contacting surface both perpendicular
and parallel to the molding pressure or
flow. After the test specimen is contacted to the
prism it may be translated carefully for short distances
along the prism surface in the direction of
the light source while the variation of index is followed
with the refractometer. This procedure should
be repeated a sufficient number of times and for a
sufficient number of specimens to determine the
range of indices involved. The average value and
the range of the index readings obtained from these
specimens shall be reported if the range exceeds the
accuracy of the measurement. If the variations in
index are systematic with the orientation of the test
specimen and if these variations exceed those found
between specimens of the same material, the nature
of these variations shall be reported with the average
value.
Care should be taken to work rapidly to avoid
changes in the refractive index of the plastic due to
its absorption of the contacting liquid.
10.1.3 The temperature in degrees Celsius
at which the index was measured.
10.1.4 If available, the dispersion shall be
reported along with the index of refraction.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights awerted
in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination
of the validity of any such patent rights, and the risk of infringement of such rights, is entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five
years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or
for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration
at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not
received a fair hearing you should make your views known to the ASTM Committee on Standards, 1916 Race St.,
Philadelphia, Pa. 19103, which will schedule a further hearing regarding your comments. Failing satisfaction there, you
may appeal to the ASTM Board of Directors.
125

Designation: D 638 - 87a
abAMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
TENSILE PROPERTIES OF PLASTICS'
This standard is issued under the fixed designation D 638: the number immediately following the designation indicates the year of
original adoption or. in the case of revision. the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (6) indicates an editorial change since the last revision or reapproval.
This test mdicxl has been approved fi,r iise by agencies qfthe Department of Definse andfijr listing in the DoD 1nde.v i$S~&ntion.s
and Standards.
1. scope
I. 1 This test method covers the determination
of the tensile properties of plastics in the form of
standard dumbbell-shaped test specimens when
tested under defined conditions of pretreatment,
temperature, humidity, and testing machine
speed.
1.2 This test method can be used for testing
materials of any thickness up to 0.55 in. (14
mm). However, for testing specimens in the form
of thin sheeting, including film less than 0.04 in.
( I .O mm) in thickness, Test Method D 882 is the
preferred test method. Materials with a thickness
greater than 0.55 in. must be reduced by machining.
NOTE I-A complete metric companion to Test
Method D 638 has been developed-D 638 M.
NOTE 2-This test method is not intended to cover
precise physical procedures. It is recognized that the
constant-rate-of-crosshead-movement type of test
leaves much to be desired from a theoretical standpoint,
that wide differences may exist between rate of crosshead
movement and rate of strain between gage marks
on the specimen, and that the testing speeds specified
disguise important effects characteristic of materials in
the plastic state. Further, it is realized that variations in
the thicknesses of test specimens, which are permitted
by these procedures, produce variations in the surfacevolume
ratios of such specimens, and that these variations
may influence the test results. Hence, where directly
comparable results are desired, all samples should
be of equal thickness. Special additional tests should be
used where more precise physical data are needed.
NOTE 3-This test method may be used for testing
phenolic molded resin or laminated materials. However,
where these materials are used as electrical insulation,
such materials should be tested in accordance
with Method D 229 and Test Method D 65 I .
1.3 The values as stated in inch-pound units
are to be regarded as the standard. The values in
parentheses are given for information only.
1.4 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the sakt-v prob
Iems associated with its use. It is the responsibility
of the user ofthis standard to establish appropriate
safety and health practices and determine
the applicability of regulatory limitations prior to
use.
2. Referenced Documents
2. I ASTM Standards:
D229 Method of Testing Rigid Sheet and Plate
Materials Used for Electrical In~ulation~-~
D374 Test Methods for Thickness of Solid
Electrical Insulati~n~*~
D412 Test Methods for Rubber Properties in
Tensi~n~.~
D 6 I8 Methods of Conditioning Plastics and
Electrical Insulating Materials for Testing2
D651 Test Method for Tensile Strength of
Molded Electrical Insulating Materials3
D882 Test Methods for Tensile Properties of
Thin Plastic Sheeting2
D883 Definitions of Terms Relating to
Plastics2
D 1822 Test Method for Tensile-Impact Energy
to Break Plastics and Electrical Insulating
Materials6
' This test method is under the jurisdiction of ASTM Committee
IT20 on Plastics and is the direct responsibility of Subcommittee
D 20. IO on Mechanical Properties.
Current edition approved Oct. 30.1987. Published Duxmber
1987. Originally published as D638 - 41 7. Last pteviouS edition
D 638 - 87.
*Annual Book ofASTM Standards. Vol08.0 I .
' Annual Book of ASTM Standards, Vol 10.0 I.
Annual Book of ASTM Standards, Vol 10.02.
'Annual Book ofASTM Standards. Vol09.01.
Annual Book of ASTM Standards. Vol08.02.
126

D 638
D4066 Specification for Nylon Injection and
Extrusion Materials (PA)'
E 4 Practices for Load Verification of Testing
Machines'.'
E 83 Practice for Verification and Classification
of Extensometers'
E 691 Practice for Conducting an Interlaboratory
Test Program to Determine the Precision
of Test Methods'
3. Definitions
3.1 General-Definitions of terms applying to
this test method appear in Definitions D 883 and
Annex A I.
4. Significance and Use
4.1 This test method is designed to produce
tensile property data for the control and specification
of plastic materials. These data are also
useful for qualitative characterization and for
research and development.
4.2 Tensile properties may vary with specimen
preparation and with speed and environment
of testing. Consequently, where precise
comparative results are desired, these factors
must be carefully controlled.
4.2.1 It is realized that a material cannot be
tested without also testing the method of preparation
of that material. Hence, when comparative
tests of materials per se are desired, the greatest
care must be exercised to ensure that all samples
are prepared in exactly the same way, unless the
test is to include the effects of sample preparation.
Similarly, for referee purposes or comparisons
within any given series of specimens, care
must be taken to secure the maximum degree of
uniformity in details of preparation, treatment,
and handling.
4.3 Tensile properties may provide useful data
for plastics engineering design purposes. However,
because of the high degree of sensitivity
exhibited by many plastics io raie of straining
and environmental conditions, data obtained by
this test method cannot be considered valid for
applications involving load-time scales or environments
widely different from those of this test
method. In cases of such dissimilarity, no reliable
estimation of the limit of usefulness can be made
for most plastics. This sensitivity to rate of straining
and environment necessitates testing over a
broad load-time scale (including impact and
creep) and range of environmental conditions if
tensile properties are to suffice for engineering
design purposes.
NOTE 4-Since the existence of a true elastic limit
in plastics (as in many other organic materials and in
many metals) is debatable, the propriety of applying
the term "elastic modulus" in its quoted generally accepted
definition to describe the "stiffness" or "rigidity"
of a plastic has beem seriously questioned. The exact
stress-strain characteristics of plastic materials are
highly dependent on such factors as rate of application
of stress, temperature, previous history of specimen,
etc. However. stress-strain curves for plastics. determined
as described in this test method, almost always
show a linear region at low stresses, and a straight line
drawn tangent to this portion of the curve permits
calculation of an elastic modulus of the usually defined
type. Such a constant is useful if its arbitrary nature
and dependence on time. temperature, and similar
factors are realized.
5. Apparatus
5. I Testing Machine-A testing machine of
the constan t-rate-of-crosshead-movement type
and comprising essentially the following:
5. I. 1 Fixed Member-A fixed or essentially
stationary member carrying one grip.
5. I .2 Movable Member-A movable member
carrying a second grip.
5. I .3 Grips-Grips for holding the test specimen
between the fixed member and the movable
member. The grips shall be self-aligning, that is,
they shall be attached to the fixed and movable
member, respectively, in such a manner that they
will move freely into alignment as won as any
load is applied, so that the long axis of the test
specimen will coincide with the direction of the
applied pull through the center line of the grip
assembly. The specimens should be aligned as
perfectly as possible with the direction of pull so
that no rotary motion that may induce slippage
will occur in the grips; there is a limit to the
amount of misalignment self-aligning grips will
accommodate.
5. I .3. I The test specimen shall be held in such
a way that slippage relative to the grips is prevented
insofar as possible. Grip surfaces that are
deeply scored or serrated with a pattern similar
to those of a coarse single-cut file, serrations
about 0.09 in. (2.4 mm) apart and about 0.06 in.
( 1.6 mm) deep, have been found satisfactory for
most thermoplastics. Finer serrations have been
'Annual Book oJASTM Standards, Vol08.03.
Annual Book oJASTM Standards. Vol03.0 I .
Annual Book of ASTM Standards, Vol 14.02.
127

D 638
found to be more satisfactory for harder plastics.
such as the thermosetting materials. The serrations
should be kept clean and sharp. Breaking
in the grips may occur at times, even when deep
serrations or abraded specimen surfaces are used:
other techniques must be used in these cases.
Other techniques that have been found useful.
particularly with smooth-faced grips, are abrading
that portion of the surface of the specimen
that will be in the grips. and interposing thin
pieces of abrasive cloth, abrasive paper, or plastic
or rubber-coated fabric, commonly called hospital
sheeting. between the specimen and the grip
surface. No. 80 double-sided abrasive paper has
been found effective in many cases. An openmesh
fabric. in which the threads are coated with
abrasive has also been effective. Reducing the
cross-sectional area of the specimen may also be
effective. The use of special types of grips is
sometimes necessary to eliminate slippage and
breakage in the grips.
5. I .4 Driw Mechanism-A drive mechanism
for imparting to the movable member a uniform.
controlled velocity with respect to the stationary
member, this velocity to be regulated as specified
in Section 9.
5. I .5 Load Indicator-A suitable load-indicating
mechanism capable of showing the total
tensile load carried by the test specimen when
held by the grips. This mechanism shall be essentially
free of inertia lag at the specified rate of
testing and shall indicate the load with an accuracy
of _+I 96 of the indicated value, or better.
The accuracy of the testing machine shall be
verified in accordance with Practices E 4.
NOTE 5-Experience has shown that many testing
machines now in use are incapable of maintaining
accuracy for as long as the periods between inspection
recommended in Practices E4. Hence, it is recommended
that each machine be studied individually and
verified as often as may be found necessary. It frequently
will be necessary to perform this function daily.
5.1.6 The fixed member, movable member,
drive mechanism, and grips shall be constructed
of such materials and in such proportions that
the total elastic longitudinal strain of the system
constituted by these parts does not exceed I %
of the total longitudinal strain between the two
gage marks on the test specimen at any time
during the test and at any load up to the rated
capacity of the machine.
5.2 Extension Indicator-A suitable instru-
ment for determining the distance between two
fixed points located within the gage length of the
test specimen at any time during the test. It is
desirable. but not essential. that this instrument
automatically record this distance (or any change
in it) as a function of the load on the test specimen
or of the elapsed time from the start of the
test. If only the latter is obtained. data on load as
a function of time must also be taken.
5.2. I Low Ewnsion (Modirlirs) Measirrc-
nwnts-For elastic modulus measurements, a
mechanically attached extensometer accurate to
_+I 96 of the measured strain shall be used. The
attachment of the extensometer shall be such as
to cause no damage to the surface of the specimen,
and the weight of the instrument shall not
induce bending strains in the specimen. A noncontacting
extensometer may be used if it can be
shown to be of equivalent sensitivity.
5.2.2 High E.vtcnsion Mcasirrcmennrs- For
strain measurements beyond the Hookean region,
alternative methods of strain measurement
may be used, but they must be accurate to .+I %
of the measured strain.
5.2.3 All extension indicators shall be free of
inertial lag at the specified speed of testing and
shall be calibrated periodically in accordance
with Practice E 83.
NOTI.: 6-Refer to Practice E 83.
5.3 Micro~ncwrs-Suitable micrometers for
measuring the width and thickness of the test
specimen to an incremental discrimination of at
least 0.001 in. (0.025 mm) should be used. All
width and thickness measurements of rigid and
semirigid plastics may be measured with a hand
micrometer with ratchet. A suitable instrument
for measuring the thickness of nonrigid test specimens
shall have: (I) a contact measuring pressure
of 3.6 .+ 0.36 psi (25 .+ 2.5 kPa), (2) a
movable circular contact foot 0.250 .+ 0.001 in.
(6.35 .+ 0.025 mm) in diameter, and (3) a lower
fixed anvil large enough to extend beyond the
contact foot in all directions and being parallel
to the contact foot within 0.0002 (0.005 mm) in.
over the entire foot area. Flatness of foot and
anvil shall conform to the portion of the Calibration
Section of Test Methods D 374, which addresses
“flatness of surfaces of micrometers.”
5.1.3. An optional instrument equipped with a
circular contact foot 0.625 f 0.003 in. (I 5.88 .+
0.08 mm) in diameter is recommended for thickness
measuring of process samples or larger spec-
128

0638
imens at least 0.625 in. (1 5.88 mm) in minimum
width.
6. Test Specimens
6.1 Sheet. Plate, and Molded Plastics:
6. I. I Rigid and Semirigid Plastics-The test
specimen shall conform to the dimensions shown
in Fig. 1. The Type I specimen is the preferred
specimen and shall be used where sufficient material
having a thickness of 0.28 in. (7 mm) or
less is available. The Type I1 specimen may be
used when a material does not break in the
narrow section with the preferred Type I specimen.
The Type V specimen shall be used where
only limited material having a thickness of 0.16
in. (4 mm) or less is available for evaluation, or
where a large number of specimens are to be
exposed in a limited space (thermal and environmental
stability tests, etc.). The Type IV specimen
should be used when direct comparisons are
required between materials in different rigidity
cases (that is, nonrigid and semirigid). The Type
I11 specimen must be used for all materials with
a thickness of greater than 0.28 in. (7 mm) but
not more than 0.55 in. (14 mm).
6.1.2 Nonrigid Plastics-The test specimen
shall conform to the dimensions shown in Fig. 1.
The Type IV specimen shall be used for testing
nonrigid plastics with a thickness of 0.16 in. (4
mm) or less. The Type I11 specimen must be used
for all materials with a thickness greater than
0.28 in. (7 mm) but not more than 0.55 in. (14
mm).
6.1.3 Preparation-Test specimens shall be
prepared by machining operations, or die cutting,
from materials in sheet, plate, slab, or similar
form. Materials thicker than 0.55 in. (14 mm)
must be machined to 0.55 in. (14 mm) for use as
Type I11 specimens. Specimens can also be prepared
by molding the material to be tested.
NOTE 7-Specimens prepared by injection molding
may have different tensile properties than specimens
prepared by machining or diecutting because of the
orientation induced. This effect may be more pronounced
in specimens with narrow sections.
6.2 The test specimen for rigid tubes shall be
as shown in Fig. 2. The length, L, shall be as
shown in the table in Fig. 2. A groove shall be
machined around the outside of the specimen at
the center of its length so that the wall section
after machining shall be 60% of the original
nominal wall thickness. This groove shall consist
of a straight section 2.25 in. (57.2 mm) in length
with a radius of 3 in. (76 mm) at each end joining
it to the outside diameter. Steel or brass plugs
having diameters such that they will fit snugly
inside the tube and having a length equal to the
full jaw length plus 1 in. (25 mm) shall be placed
in the ends of the specimens to prevent crushing.
They can be located conveniently in the tube by
separating and supporting them on a threaded
metal rod. Details of plugs and test assembly are
shown in Fig. 2.
6.3 The test specimen for rigid rods shall be
as shown in Fig. 3. The length, L, shall be as
shown in the table in Fig. 3. A groove shall be
machined around the specimen at the center of
its length so that the diameter of the machined
portion shall be 60% of the original nominal
diameter. This groove shall consist of a straight
section 2.25 in. (57.2 mm) in length with a radius
of 3 in. (76 mm) at each end joining it to the
outside diameter.
6.4 All surfaces of the specimen shall be free
of visible flaws, scratches, or imperfections.
Marks left by coarse machining operations shall
be carefully removed with a fine file or abrasive,
and the filed surfaces shall then be smoothed
with abrasive paper (No. 00 or finer). The finishing
sanding strokes shall be made in a direction
parallel to the long axis of the test specimen. All
flash shall be removed from a molded specimen,
taking great care not to disturb the molded surfaces.
In machining a specimen, undercuts that
would exceed the dimensional tolerances shown
in Fig. 1 shall be scrupulously avoided. Care shall
also be taken to avoid other common machining
errors.
6.5 If it is necessary to place gage marks on
the specimen, this shall be done with a wax
crayon or India ink that will not affect the material
being tested. Gage marks shall not be
scratched, punched, or impressed on the specimen.
6.6 When testing materials that are suspected
of anisotropy, duplicate sets of test specimens
shall be prepared, having their long axes respectively
parallel with, and normal to, the suspected
direction of anisotropy.
7. Conditioning
7.1 Conditioning-Condition the test specimens
at 73.4 f 3.6"F (23 f 2%) and 50 f 5 %
relative humidity for not less than 40 h prior to
129

D 638
test in accordance with Procedure A of Methods
D 6 18, for those tests where conditioning is required.
In cases of disagreement, the tolerances
shall be k I .8"f(+ 1°C) and +2 % relative humidity.
7.1.1 Note that for some hygroscopic materials,
such as nylons, the material specifications
(for example, Specification D 4066) call for testing
"dry as-molded specimens." Such requirements
take precedence over the above routine
preconditioning to 50 % relative humidity and
require sealing the specimens in water vaporimpermeable
containers as won as molded and
not removing them until ready for testing.
7.2 Test Conditions-Conduct tests in the
Standard Laboratory Atmosphere of 73.4 f 3.6"F
(23 f 2'C) and 50 f: 5 % relative humidity, unless
otherwise specified in the test methods. In cases
of disagreements, the tolerances shall be I .8"F
(1°C) and +-2 % relative humidity.
NOTE 8-The tensile properties of some plastics
change rapidly with small changes in temperature.
Since heat may be generated as a result of straining the
specimen at high rates, conduct tests without forced
cooling to ensure uniformity of test conditions. Measure
the temperature in the reduced section of the
specimen and record it for materials where self-heating
is suspected.
8. Number of Test Specimens
8.1 Test at least five specimens for each sample
in the case of isotropic materials.
8.2 Test ten specimens, five normal to, and
five parallel with the principal axis of anisotropy,
for each sample in the case of anisotropic materials.
8.3 Discard specimens that break at some obvious
fortuitous flaw, or that do not break between
the predetermined gage marks, and make
retests, unless such flaws constitute a variable to
be studied.
NOTE 9-Before testing, all transparent specimens
shoufd be inspected in a poianscope. Those which show
atypical or concentrated strain patterns should be rejected,
unless the effects of these residual strains constitute
a variable to be studied.
9. Speed of Testing
9.1 Speed of testing shall be the relative rate
of motion of the grips or test fixtures during the
test. Rate of motion of the driven grip or fixture
when the testing machine is running idle may be
used, if it can be shown that the resulting speed
of testing is within the limits of variation allowed.
9.2 Choose the speed of testing from Table 1.
Determine this chosen speed of testing by the
specification for the material being tested, or by
agreement between those concerned. When the
speed is not specified, use the lowest speed shown
in Table 1 for the specimen geometry being used,
which gives rupture within */2 to 5 min testing
time.
9.3 Modulus determinations may be made at
the speed selected for the other tensile properties
when the recorder response and resolution are
adequate.
10. Procedure
10.1 Measure the width and thickness of rigid
flat specimens (Fig. 1) with a suitable micrometer
to the nearest 0.001 in. (0.025 mm) at several
points along their narrow sections. Measure the
thickness of nonrigid specimens (produced by a
Type IV die) in the same manner with the required
dial micrometer. Take the width of this
specimen as the distance between the cutting
edges of the die in the narrow section. Measure
the diameter of rod specimens, and the inside
and outside diameters of tube specimens, to the
nearest 0.001 in. (0.025 mm) at a minimum of
two points 90" apart; make these measurements
along the groove for specimens so constructed.
Use plugs in testing tube specimens, as shown in
Fig. 2.
10.2 Place the specimen in the grips of the
testing machine, taking care to align the long axis
of the specimen and the grips with an imaginary
line joining the points of attachment of the grips
to the machine. The distance between the ends
of the gripping surfaces, when using flat specimens,
shall be as indicated in Fig. 1. On tube and
rod specimens, the location for the grips shall be
as shown in Figs. 2 and 3. Tighten the grips
evenly and firmly to the degree necessary to
prevent slippage of the specimen during the test,
but not to the point where the specimen would
be crushed.
10.3 Attach the extension indicator. When
modulus is being determined, the extension indicator
must continuously record the distance
the specimen is stretched (elongated) within the
gage length as a function of the load through the
initial (linear) portion of the load-elongation
curve.
NOTE 10-Modulus of materials is determined from
the slope of the linear portion of the stress-strain curve.
I30

D 638
For most plastics, this linear portion if very small,
occurs very rapidly, and must be recorded automatically.
The change in jaw separation is never to be used
for calculating modulus or elongation.
10.4 Set the speed of testing at the proper rate
as required in Section 9, and start the machine.
10.5 Record the load-extension curve of the
specimen.
10.6 Record the load and extension at the
yield point (if one exists) and the load and extension
at the moment of rupture.
NOTE I 1-If it is desired to measure both modulus
and failure properties (yield or break, or both), it may
be necessary, in the case of highly extensible materials
to run two independent tests. The high magnification
extensometer normally used to determine properties up
to the yield point may not be suitable for tests involving
high extensibility. If allowed to remain attached to the
specimen, the extensometer could be permanently
damaged. A broad range incremental extensometer or
hand rule technique may be needed when such materials
are taken to rupture.
11. Calculation
11.1 Tensile Strength-Calculate the tensile
strength by dividing the maximum load in newtons
(or pounds-force) by the original minimum
cross-sectional area of the specimen in square
metres (or square inches). Express the result in
pascals (or pounds-force per square inch) and
report it to three significant figures as "Tensile
Strength at Yield" or "Tensile Strength at Break,"
whichever term is applicable. When a nominal
yield or break load less than the maximum is
present and applicable, it may be desirable also
to calculate, in a similar manner, the corresponding
"Tensile Stress at Yield" or "Tensile Stress at
Break" and report it to three significant figures
(Annex Note A 1.1 ).
I 1.2 Percent Elongation-If the specimen
gives a yield load that is larger than the load at
break, calculate "Percent Elongation at Yield."
Otherwise, calculate "Percent Elongation at
Break." Do this by reading the extension (change
in gage length) at the moment the applicable load
is reached. Divide that extension by the original
gage length and multiply by 100. Report "Percent
Elongation at Yield" or "Percent Elongation at
Break" to two significant figures. When a yield
or breaking load less than the maximum is present
and of interest, it is desirable to calculate and
report both "Percent Elongation at Yield" and
"Percent Elongation at Break" (Annex Note
A 1.2).
1 1.3 Moduhrs of Elasticity-Calculate the
modulus of elasticity by extending the initial
linear portion of the load-extension curve and
dividing the difference in stress corresponding to
any segment of section on this straight line by
the corresponding difference in strain. All elastic
modulus values shall be computed using the
average initial cross-sectional area of the test
specimens in the calculations. The result shall be
expressed in pounds-force per square inch (pascals)
and reported to three significant figures.
11.4 For each series of tests, calculate the
arithmetic mean of all values obtained and report
it as the "average value'' for the particular prop
erty in question.
1 1.5 Calculate the standard deviation (estimated)
as follows and report it to two significant
figures:
s = d(ZX2 - nP)/(n - I)
where:
s = estimated standard deviation,
X = value of single observation,
n = number of observations, and
= arithmetic mean of the set of observations.
1 1.6 See Appendix X 1 for information on toe
compensation.
12. Report
12.1 The report shall include the following
12. I. 1 Complete identifications of the material
tested, including type, source, manufacturer's
code numbers, form, principal dimensions, previous
history, etc.,
12.1.2 Method of preparing test specimens,
12.1.3 Type of test specimen and dimensions,
12.1.4 Conditioning procedure used,
12.1.5 Atmospheric conditions in test room,
12.1.6 Number of specimens tested,
12.1.7 Speed of testing,
12.1.8 Tensile strength at yield or break, average
value, and standard deviation,
12.1.9 Tensile stress at yield or break, if a p
plicable, average value, and standard deviation,
12.1.10 Percentage elongation at yield or
break (or both, as applicable), average value, and
standard deviation,
12.1.1 1 Modulus of elasticity, average value,
and standard deviation, and
12.1.12 Dateoftest.
131

D638
13. Precision and Biasao
13. I Tables 2 through 6 are based on a round
robin conducted in 1984. involving five materials
tested by eight laboratories using the Type I
specimen, all of nominal 0.125-in. thickness.
Each test result was based on five individual
determinations. Each laboratory obtained two
test results for each material.
13.2 In Tables 2 through 6. for the materials
indicated, and for test results that are derived
from testing five specimens:
13.2. I S, is the within-laboratory standard deviation
of the average: fr = 2.83 s,. (See 13.2.3
for application of lr.)
13.2.2 SR is the between-laboratory standard
deviation of the average: IR = 2.83 SR. (See 13.2.4
for application of IR.)
13.2.3 Ri~pcJatahility-In comparing two test
results for the same material. obtained by the
same operator using the same equipment on the
same day, those test results should be judged not
equivalent if they differ by more than the I, value
for that material and condition.
I 3.2.4 Rc~prodircihility-1 n comparing two
test results for the same material. obtained by
different operators using different equipment on
different days. those test results should be judged
not equivalent if they differ by more than the IR
value for that material and condition. (This ap
plies between different laboratories or between
different equipment within the same laboratory.)
13.2.5 Any judgment in accordance with
13.2.3 and 13.2.4 will have an approximate 95 %
(0.95) probability of being correct.
13.2.6 Other formulations may give somewhat
different results.
13.3 For further information on the methodology
used in this section. see Practice E 69 I.
13.4 There are no recognized standards on
which to base an estimate of bias for this test
method.
13.5 The precision of this test method is very
dependent upon the uniformity of specimen
preparation. standard practices for which are covered
in other documents.
lo Supporting data are available from ASTM Headquarters.
Request RR: D20-I 125.
-
TABLE 1
Designations for Speed of Testing"
speed Of
Classification" Specimen Type in./min
(mm/min)
Nominal Strainc
Rate at Start of Test.
in./in. -min
(mm/mm. min)
Rigid and Semirigid I. 11. Ill rods and tubes 0.2 f 25 7% 0.1
2* IO% I
IV
20* 10% IO
0.2 * 25 % 0.15
2* IO% I .5
20* 10% I5
V 0.05 f 25 % 0. I
0.5 * 25 % 1
5*25% IO
Nonrigid 111 2*10%
20* 10%
I
IO
IV
2* IO%
I .5
202 iO-70 ij
A Select the lowest speed that produces rupture in Yz to 5 min for the specimen geometry being used (see 9.2).
"See Definitions D 883 for definitions.
The initial rate of straining cannot be calculated exactly for dumbbell-shaped specimens because of extension, both in the
reduced section outside the gage length and in the fillets. This initial strain rate can be measured from the initial slope of the tcnsik
strai n-versus-time diagram.
132

TABLE 2 Modulus, 18 psi. for Eight LaborntMies. Five Materials
. Mean S, SR I, In
Polypropylene 0.2 IO 0.0089 0.07 I 0.025 0.201
Cellulose Acetate Butyrate 0.246 0.0179 0.035 0.05 I 0.144
Acrylic 0.48 I 0.0 I79 0.063 0.05 1 0.144
General Resin Nylon 1.17 0.0537 0.2 I7 0. I52 0.614
General Resin Polyester I .39 0.0894 0.266 0.253 0.753
TABLE 3 Tensile Stress at Yield, Id psi. for Eight laboratories, Three Materials
Mean S, SR I, IR
Polypropylene 3.63 0.022 0.161 0.062 0.456
Cellulose Acetate Butyrate 5.0I 0.058 0.227 0.164 0.642
Acrylic 10.4 0.067 0.317 0.190 0.897
~-
TABLE 4 Elongation at Yield, W, for Eight laboratories, Three Materials
Mean S, sn 1, 1,
Cellulose Acetate Butyrate 3.65 0.27 0.62 0.76 1.75
Acrylic 4.89 0.2 I 0.55 0.59 1.56
Polypropylene 8.79 0.45 5.86 1.27 16.5
TABLE 5 Tensile Strength at Break, Id psi. for Eight hhtories, Five Materials"
Mean S, sn I, In
Polypropylene 2.97 1.54 I .65 4.37 4.66
Cellulose Acetate Butyrate 4.82 0.058 0.180 0.164 0.m
Acrylic 9.09 0.452 0.75 I I .27 2.13
General Resin Polyester 20.8 0.233 0.437 0.659 I .24
General Resin Nylon 23.6 0.277 0.698 0.784 I .98
A Tensile strength and elongation at break values obtained for unreinforced propylene plastics generally are highly variable due
to inconsistencies in necking or "drawing" of the Center section of the test bar. Since tensile strength and elongation at yield are
more reproducible and relate in most cases to the practical usefulness of a molded part. they are generally recommended for
specification purposes.
TABLE 6 Elomution at Break. 96. for Eight laboratories, Five Materials"
Mean S, SR 1, In
General Resin Polyester 3.68 0.20 2.33 0.570 6.59
General Resin Nylon 3.87 0.10 2.13 0.283 6.03
Acrylic 13.2 2.05 3.65 5.80 10.3
Cellulose Acetate Butyrate 14. I I .87 6.62 5.29 18.7
Polypropylene 293.0 50.9 119.0 144.0 337.0
A Tensile strength and elongation a! break values oWned for unrtinfcmed propylene plastics pnmlly are highly variable due
to inconsistencies in necking or "drawing" of the center section of the test bar. Since tensile stmgth and elongation at yield are
more reproducible and relate in most cases to the practical usefulness of a molded part. they are generally recommended for
specification purposes.
133

@ D638
r
i-.
--.__
- i d
' Z - . c
- LO -
TYPE LP
- -T
Specimen Dimensions for Thickness, T. in. (mmy
0.28 (7) or under
Over 0.28 to
0.55 (7 to 0. I6 (4) or under
Dimensions (see drawings) 14) incl. Tolerances
Type1 TmII TywIII TmIVG
U'-Width of narrow section".' 0.50 (13) 0.25 (6) 0.75 (19) 0.25 (6)
L-Length of narrow section 2.25 (57) 2.25 (57) 2.25 (57) 1.30 (33)
R'O-Width over-all, minE 0.75 ( 19) 0.75 ( 19) I. I3 (29) 0.75 ( 19)
WO-Width over-all, mint ... ... ... ...
LO-Length over-all. minF 6.5 (165) 7.2 (183) 9.7 (246) 4.5 (I IS)
G-Gage lengthr 2.00 (50) 2.00 (50) 2.00 (50) ...
Type VI
0.125 (3.18) M.02 (M.5)G.'
0.375 (9.53) M.02 (M.57
... M.25 (6.4)
0.375 (9.53) M.125 (+3.18)
2.5 (63.5) no max (no max)
0.300 (7.62) M.010 (M.25)'
131
... M.005 (M.
G-Gage lengthC ... ... ... 1.00 (25)
D-Distance-between grips 4.5(115) 5.3(135) 4.5(llS) 2.SH(64) LO(25.4) MO.2(f5) '
R-Radius of fillet 3.00 (76) 3.00 (76) 3.00 (76) 0.56 (14) 0.5 (12.7) M.04 (*I7
RO-Outer radius (Type IV) ... ... ... I.00(25) ... M.04 (*I)
FIG. 1 Tensioa Test Specinmu for Sbeet, Phte, .Id Molded phrtics
"The width at the center W, shall be M.OO0 in., -0.004 in. (M.00 mm. -0. IO mm) compared with width Wat other parts of
the reduced section. Any nduction in W at the center shall be gradual, equally on each side so that no abrupt chaw in dimeasion
result.
' For molded specimens, a draft of not over 0.005 in. (0. I3 mm) may be allowed for either Type I or I1 specimens 0.13 in. (3.2
mm) in thickness, and this should be taken into account when calculating width of the specimen. Thus a typical section ofa molded
Type I specimen, having the maximum allowable draft, could be as follows
Test marks or initial extensometer span.
Thickness, T. shall be 0.13 f 0.02 in. (3.2 f 0.4 mm) for all types of molded specimens and for other Typa I and 11 specimens
where possible. If specimens an machined from sheets or plates, thickness, T, may be the thickness of the sheet or plate provided
this does not ex& the range saated for the intended specimen type. For sheets of nominal thickness greater than 0.55 in. (14 mm)
the specimens shall be machined to 0.55 f 0.02 in. (I4 f 0.4 mm) in thickness, for use with the Type 111 specimen. For sheas of
nominal thickness between 0.55 and 2 in. (14 and 5 I mm) approximately equal amounts shall be machined thm each surkc. For
thicker sheets both surfaces of the specimen shall be machined and the location of the specimen with denma to the original
thickness of the sheet, shall be noted. Tolerances on thickness less than 0.55 in. (14 mm) shall be those stpadprd for the grede of
material tested.
EOverall widths greater than the minimum indicated may be desirable for some materials in order to avoid bmking in the grips.
FOverall lengths greater than the minimum indicated may be desirable either to avoid W n g in the grips or to saw special
test requirements.
For the Type IV specimen, the intend width of the narrow section of the die shall be 0.250 f 0.002 in. (6.00 f 0.05 mm).
The dimensions are essentially those of Die C in Test Method D 412.
"When self-tightening grips are used, for highly extensible poly" the distance bttween grips will dcpcld upon the types of
grips used and may not be critical if maintained uniform once chosen.
134

D638
.......... ......
-- -------
0.505 in., mrx
(12.03 mm)
c ........ 0.500 in. ......-.
(12.70 mm)
‘The Type V specimen shall be machined or die cut to the dimensions shown, or molded in a mold whose cavity has these
dimensions. The dimensions shall bc:
It’ = 0.125 f 0.001 in. (3.18 f 0.03 mm).
L = 0.375 f 0.003 in. (9.53 f 0.08 mm).
G = 0.300 f 0.001 in. (7.62 f 0.02 mm). and
R = 0.500 f 0.003 in. (12.7 f 0.08 mm).
The other tolerances are those in the table.
’Supporting data on the introduction of the L specimen of Test Method D 1822 as the Type V specimen are available from
ASTM Headquarters. Request RRD 20-1038.
FIG. I Continued.
I
--
135

-
Metal Plugs
\
Nominal wall Thickness
1,
DIMENSIONS OF TUBE SPECIMENS
Length of Radial Scr9ions.
2R.S.
in. (mm)
Total Calculated Minimum
Length of Specimen
men Standard be Length. used for L. 3.5-in. of Speci- (89-
mm) Jaw&
V32 (0.79) 0.547 ( I 3.9) 13.80 (350) I5 (381)
v64 (I.2) 0.670 ( 17.0) 13.92 (354) I5 (381)
%s (1.6) 0.773 ( 19.6) 14.02 (356) I5 (381)
J ~ (2.4) Z
0.946 (24.0) 14.20 (361) 15 (381)
Vi (3.2) 1.091 (27.7) 14.34 (364) I5 (381)
'/I6 (4.8) 1.333 (33.9) 14.58 (370) I5 (381)
V4 (6.4) 1.536 (39.0) 14.79 (376) 15.75 (400)
%6 (7.9) 1.714 (43.5) 14.96 (380) 15.75 (400)
w (9.5) I .873 (47.6) 15.12 (384) 15.75 (400)
'116 ( I 1.1) 2,019(51.3) 15.27 (388) 15.75 (400)
95 (12.7) 2.154 (54.7) 15.40 (391) 16.5 ..(4191
. --,
A For other jaws gmter than 3.5 in. (89 mm), the standad length shall be increased by twice the length of the jaws minus 7 in.
(I 78 mm). The standard length permits a slippage of approximately 0.25 to 0.50 in. (6.4 lo 12.7 mm) in each jaw while maintaining
maximum length of jaw grip.
FIG. 2 D&g"i Showing Loation of Tube Tension Test Specimens in Testing Machine
-
136

Machine to
Nominal Diameter
% (3.2)
%6 (4.7)
V4 (6.4)
v8 (9.5)
'h(12.7)
U ( 15.9)
?h( 19.0)
'18 (22.2)
I (25.4)
1%(31.8)
1 'h(38. I )
1% (42.5)
2 (50.8)
DIMENSIONS OF ROD SPECIMENS
Length of Radial
Sections, 2R.S.
0.773 (19.6)
0.946 (24.0)
1.091 (27.7)
1.333 (33.9)
1.536 (39.0)
1.714 (43.5)
1.873 (47.6)
2.019 (51.5)
2. I54 (54.7)
2.398 (60.9)
2.615 (66.4)
2.812 (71.4)
2.993 (76.0)
in. (mm)
Total Calculated Minimum
Length of Specimen
14.02 (356)
14.20 (361)
14.34 (364)
14.58 (370)
14.79 (376)
14.96 (380)
15.12 (384)
15.27 (388)
15.40 (391)
15.65 (398)
15.87 (403)
16.06 (408)
16.24 (412)
Standard Length. L, of Specimen
lo be used for 89-mm
(3Ih-in.) JawsA
I5 (381)
15 (381)
I5 (381)
I5 (381)
15.75 (400)
15.75 (400)
!5.75 (400)
15.75 (400)
16.5 (419)
16.5 (419)
16.5 (419)
16.5 (419)
17 1432)
A For other jaws greater than 3.5 in. (89 mm). the standard length shall be increased by twice the length of the jaws minus 7in.
( I78 mm). The standard length permits a slippage of approximately 0.25 to 0.50 (6.4 to 12.7 mm) in each jaw while maintaining
maximum length of jaw grip.
FIG. 3 Myplm Showing Location of Rod Tension Test Specimen in Testiq Machine
137

@ 0638
ANNEX
(Mandatory Information)
AI. DEFINITIONS OF TERMS AND SYMBOLS RELATING TO TENSION TESTING OF PLASTICS
A 1. I rensile stress (nominal)-the tensile load per
unit area of minimum original cross-section, within the
gage boundaries, camed by the test specimen at any
given moment. It is expressed in force per unit area,
usually pounds-force per square inch (megapascals).
NOTE A I . I-The expression of tensile properties in
terms of the minimum original cross-section is almost
universally used in practice. In the case of materials
exhibiting high extensibility, or "necking". or both,
(A I. I I) nominal stress calculations may not be meaningful
beyond the yield point (A I. IO) due to the extcnsive
reduction in cross-sectional area that ensues. Under
some circumstances it may be desirable to express the
tensile properties per unit of minimum prevailing crosssection.
These properties are called "true" tensile prop
erties (that is. true tensile stress, etc.).
A I .2 tensilestrengrh (nominal)-the maximum tensile
stress (nominal) sustained by the specimen during
a tension test. When the maximum stress occurs at the
yield point (AI.10). it shall be designated Tensile
Strength at Yield. When the maximum stress occurs at
break. it shall be designated Tensile Strength at Break.
A I .3 gage length-the original length of that portion
of the specimen over which strain or change in
length is determined.
A 1.4 elungatiun-the increase in length produced
in the gage length of the test specimen by a tensile load.
It is expressed in units of length, usually inches (millimetres).
(Also known as exrension.)
NOTE A 1.2-Elongation and strain values are valid
only in cases were uniformity of specimen behavior
within the gage length is present. In the case of materials
exhibiting "necking phenomena," such values are only
of qualitative utility after attainment of "yield" point.
This is due to inability to assure that necking will
encompass the entire length between the gage marks
prior to specimen failure.
A I .5 percenrage elungatiun-the elongation of a test
specimen expressed as a percentage of the gage length.
A I .6 percentage elongation at yield and break:
A I .6. I percentage elungation at yield-the percentage
elongation at the moment the yield point (A1.10)
is attained in the test specimen.
A I .6.2 percenrage elongation at break-the percentage
elongation at the moment of rupture of the test
specimen.
A I .7 strain-the ratio of the elongation to the gage
length of the test specimen, that is, the change in length
per unit of original length. It is expressed as a dimensionless
ratio.
A1.8 true strain (see Fig. Al.1) is defined by the
following equation for CT:
where:
dL = the increment of elongation when the distance
between the gage marks is L,
L,, = the original distance between gage marks. and
L = the distance between gage marks at any time.
A I .9 tcwsilc stress-sfrain ciirve-a diagram in which
values of tensile stress are plotted as ordinates against
corresponding values of tensile strain as abscissas.
A1.10 yieldpuinr-the first point on thestress-strain
curve at which an increase in strain occurs without an
increase in stress (Fig. A I .2).
NOTE A I .3-Only materials whose stress-strain
curves exhibit a point of zero slope may be considered
as having a yield point.
NOTE A I .4--Some materials exhibit a distinct
"break" or discontinuity in the stress-strain curve in
the elastic region. This break is not a yield point by
definition. However, this point may prove useful for
material characterization in some cases.
A I. I I necking-the localized reduction in cross-section
which may occur in a material under tensile stress.
A I. 12 yield srrength-the stress at which a material
exhibits a specified limiting deviation from the proportionality
of stress to strain. Unless otherwise specified.
this stress will be the stress at the yield point and when
expressed in relation to the Tensile Strength shall be
designated either Tensile Strength at Yield or Tensile
Stress at Yield as required under A I .2 (Fig. A 1.2). (See
ufier yield srrengrh.)
A I. I3 offset yield stret,gth-the stress at which the
strain exceeds by a specified amount (the offset) an
extension of the initial proportional portion of the
stress-strain curve. It is expressed in force per unit area,
usually pounds-force per square inch (megapaxals).
NOTE AI.5-This measurement is useful for materials
whose stresstrain curve in the yield range is of
gradual curvature. The offset yield strength can be
derived from a stress-strain curve as follows (Fig. A I .3):
On the strain axis lay off OM equal to the specified
offset.
Draw OA tangent to the initial straight-line portion
of the stress-strain curve.
Through M draw a line MN parallel to OA and locate
the intersection of MN with the stress-strain curve.
The stress at the point of intersection r is the "offset
yield strength." The specified value of the offset must
be stated as a percentage of the original gage length in
conjunction with the strength value. Example: 0.1 96
138

0 638
offset yield strength = ... psi (MPa), or yield strength
at 0.1 96 offset ... psi (MPa).
A I. 14 propurtional limit-the greatest stress which
a material is capable ofsustaining without any deviation
from proportionality of stress to strain (Hooke’s law).
It is expressed in force per unit area, usually poundsforce
per square inch (megapascals).
A 1.15 elastic limit-the greatest stress which a material
is capable of sustaining without any permanent
strain remaining upon complete release of the stress. It
is expressed in force per unit area, usually pounds-force
per square inch (megapascals).
NOTE A I .6--Measured values of proportional limit
and elastic limit vary greatly with the sensitivity and
accuracy of the testing equipment, eccentricity of loading,
the scale to which the stress-strain diagram is
plotted, and other factors. Consequently, these values
are usually replaced by yield strength.
A1.16 modulus of elasticity-the ratio of stress
(nominal) to corresponding strain below the proportional
limit of a material. It is expressed in force per
unit area, usually pounds-force per square inch (megapascals)
(Also known as elastic modulus or Young’s
modulus).
NOTE A I .7-The stress-strain relations of many
plastics do not conform to Hooke’s law throughout the
elastic range but deviate therefrom even at stresses well
below the elastic limit. For such materials the slope of
the tangent to the stress-strain curve at a low stress is
usually taken as the modulus of elasticity. Since the
existence of a true proportional limit in plastics is
debatable, the propriety of applying the term “modulus
of elasticity” to describe the stiffness or rigidity of a
plastic has been seriously questioned. The exact stressstrain
characteristics of plastic materials are very dependent
on such factors as rate of stressing, temperature,
previous specimen history, etc. However, such a
value is useful if its arbitrary nature and dependence
on time, temperature, and other factors are realized.
A I. 17 secant modulus-the ratio of stress (nominal)
to corresponding strain at any specified point on the
stress-strain curve. It is expressed in force per unit area,
usually pounds-force per square inch (megapascals),
and reported together with the specified stress or strain.
NOTE A 1.8-This measurement is usually employed
in place of modulus of elasticity in the case of materials
whose stress-strain diagram does not demonstrate proportionality
of stress to strain.
A 1. I8 percentage reduction of area (nominab-the
difference between the original cross-sectional area
measured at the point of rupture after breaking and
after all retraction has ceased, expressed as a percentage
of the original area.
A 1.19 percentage reduction of area (“)-the difference
between the original cross-sectional area of the
test specimen and the minimum cross-sectional area
within the gage boundaries prevailing at the moment
of rupture, expressed as a percentage of the original
area.
A1.20 rate of loading-the change in tensile load
carried by the specimen per unit time. It is expressed
in force per unit time, usually pounds-force (newtons)
per minute. The initial rate of loading can be calculated
h m the initial slope of the load versus time diagram.
A1.21 rate of stressing (nominao-the change in
tensile stress (nominal) per unit time. It is expressed in
force per unit area per unit time, usually pounds-force
per square inch (megapasals) per minute. The initial
rate of stressing can be calculated from the initial slope
of the tensile stress (nominal) versus time diagram.
NOTE A1.9-The initial rate of stressing as determined
in this manner ha5 only limited physical significance.
It does, however, roughly describe the average
rate at which the initial stress (nominal) carried by the
test specimen is applied. It is affected by the elasticity
and flow characteristics of the materials being tested.
At the yield point, the rate of stressing (true) may
continue to have a positive value if the cross-sectional
area is decreasing.
A 1.22 rate of straining-the change in tensile strain
per unit time. It is expressed either as strain per unit
time, usually inches per inch (metres per metre) per
minute, or percentage elongation per unit time, usually
percentage elongation per minute. The initial rate of
straining can be calculated from the initial slope of the
tensile strain versus time diagram.
NOTE A I. IO-The initial rate of straining is synonymous
with the rate of crosshead movement divided by
the initial distance between crossheads only in a machine
with constant-rate-of-crosshead movement and
when the specimen has a uniform original cross-section,
does not “neck down,“ and does not slip in the jaws.
A1.23 Symbols-The following symbols may be
used for the above terms:
SYMBOL
W
AW
L
LO
L.
AL,
A
Ao
AA
A.
AT
t
At
U
Au
UT
VU
=UT
c
AC
CU
%2
Y.P.
E
TERM
Load
Increment of load
Distance between gage marks at any time
Original distance between gage marks
Distance between gage marks at moment of
rupture
Increment of distance between gage marks
= elongation
Minimum cross-sectional area at any time
Original cross-section area
Increment of cross-sectional area
Cross-sectional area at point of rupture measured
after breaking specimen
Cross-sectional area at point of rupture,
measured at the moment of rupture
Time
Increment of time
Tensile stress
Increment of stress
True tensile stress
Tensile strength at break (nominal)
Tensile strength at break (true)
Strain
Increment of strain
Total strain, at break
True strain
Percentage elongation
Yield point
Modulus of elasticity
A1.24 Relations between these various terms may
be defined as follows:
139

~
0638
u = W/Ao
UT = W/A
ut1 = W/Ao (where W is breaking load)
OUT = W/A T (where W is breaking load)
t = AL/Lo= (L - Lo)/Lo
tL1 -- t Lu - LYLO
"= dL/L = In L/Lo
WE/= [(L- Lo)/Lo] X 100 = t x 100
Percentage reduction of area (nominal)
= [(A0 - &)/A01 X 100
Percentage reduction ofarea (true)
= [(A0- AT)/&] X 100
Rate of loading = A W/Af
Rateofstressing(nominal) = Aa/At = (A W/A,,)/At
Rate of straining = &/At = (AL./Lo)Af
For the case where the volume of the test specimen
does not change during the test, the following three
relations hold: ~
UT= a(l + t) = t7L/Lo
041 + tu) = uu L JLo
A= Ao/(l+t)
OUT=
A
/
FIG. A1.2
STRAIN
TensikDes@ations
140

@ D638
I A N
cn
'
cn
L
/ /
/
/ OM=Specified
Off set
0 M
Strain
FIG. A13 Offsct Yield Strength
APPENDIX
(Nonmandatory Information)
X1. TOE COMPENSATION
X I. I In a typical stresstrain curve (Fig. XI, I) there
is a toe region, AC, that does not represent a property
of the material. It is an artifact caused by a takeup of
slack, and alignment or seating of the specimen. In
order to obtain correct values of such parameters as
modulus, strain. and offset yield point, this artifact must
be compensated for to give the corrected zero point on
the strain or extension axis.
X 1.2 In the case of a material exhibiting a region of
Hookean (linear) behavior (Fig. XI. I), a continuation
of the linear (CD) region of the curve is constructed
through the zero-stress axis. This intersection (B) is the
corrected zero-strain point from which all extensions
or strains must be measured, including the yield offset
(BE), if applicable. The elastic modulus can be determined
by dividing the stress at any point along the line
CD (or its extension) by the strain at the same point
(measured from point B, defined as zero-strain).
XI .3 In the case of a material that does not exhibit
any linear region (Fig. Xl.2), the same kind of toe
correction of the zero-strain point can be made by
constructing a tangent to the maximum slope at the
inflection point (H'). This is extended to intersect the
strain axis at point B', the corrected zero-strain point.
Using point B' as zero strain, the stress at any point
(G') on the curve can be divided by the strain at that
point to obtain a secant modulus (slope of line B' G').
For those materials with no linear region, any attempt
to use the tangent through the inflection point as a basis
for determination of an offset yield point may result in
unacceptable error.
141

A B E Strain
Ncm-.%me chart recorders pl01 the mirror image of this
graph.
FIG. X1.l Material with Hookean Region
A B‘ Strain
NOTE-some chart recorders plot the mirror image of this
graph.
FIG. XI.2 Material with No Hookean Region
The American Scniet.r.fi)r Testing and Materials takes no pasition respecting thin validity qlbny patent rights ussserted in connection
with any i:em mentioned in rhis standard. Users ofthis standard are espressly advised that determination ot’tht validity (!/‘any S14C.h
patent rixhts, and the risk of infringement qf such rights. arc entirelr their o w re.vponsihility.
This standard is subject to revision at any timi. by the responsible technical commirtee and must he reviewed iwr~*/iw years and
If ncn revised, either reapproved or nithdrawn. Your comments are invited either Ji)r revision of rhis standard or ,lbr additional
standards and should be addressed to ASTM Headquarters. Your comments will receive carefir1 consideration at a mecting of the
responsible technical committee. which jvnt may attend. If you .feel that your comments haw not received a ,fair hilaring you should
make your views known to the ASTM Committee on Standards. 1916 Race S:., Philadelphia. PA 19/03.
142

AMERICAN NATIONAL
STANDARD
ASTM D 696 - 79
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
COEFFICIENT OF LINEAR THERMAL EXPANSION OF
PLASTICS'
This Standard is issued under the fixed designation D 696; the number immediately following the designation indicates
the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the
year of last reapproval.
NoTE-scction 5.2 was corrected editorially and the designation date was changed May 4. 1979.
_ _ . -
This method hos been approved for use by agenries of the Deparrment of Dejense andlor listing in the Do D Index of Speccifications
ond Standards.
1. scope
1.1 This method covers determination of
the coefficient of linear thermal expansion
for plastics by use of a vitreous silica dilatometer.
At the test temperatures and under the
stresses imposed, the plastic materials shall
have a negligible creep or elastic strain rate
or both, insofar as these properties would
significantly affect the accuracy of the measure
men t s .
NOTE 1 -See also Method E 228.
1.2 The thermal expansion of a plastic is
composed of a reversible component on which
are superimposed changes in length due to
changes in moisture content, curing, loss of
plasticizer or solvents, release of stresses,
phase changes and other factors. This method
of test is intended for determining the coefficient
of linear thermal expansion under the
exclusion of these factors as far as possible.
In general, it will not be possible to exclude
the effect of these factors completely. For
this reason, the method can be expected to
give only an approximation to the true thermal
expansion.
NOTE 2 -The values stated in SI units are to be
regarded as the standard.
2. Applicable Documents
2.1 ASTM Standards:
E 228 Test for Linear Thermal Expansion
of Rigid Solids with a Vitreous Silica
Dilatometer'
D 2236 Test for Dynamic Mechanical Prop
erties of Plastics by Means of a Torsional
Pendulum3
143
D 1898 Recommended Practice for Sampling
of Plastics3
D 618 Conditioning Plastics and Electrical
Insulating Materials for Testing3
3. Significance
3.1 The coefficient of linear thermal expansion,
a, between temperatures T1 and T2 for
a specimen whose length is L,, at the reference
temperature, is given by the following equation:
1~ = (L2 - Ll)/[L,(T, - Tal = ALILOAT
where L, and L, are the specimen lengths at
temperatures T, and T2, respectively. (Y is,
therefore, obtained by dividing the linear
expansion per unit length by the change in
temperature.
3.2 The nature of most plastics and the
construction of the common type of dilatometer
make -30 to +30°C a convenient temperature
range for linear thermal expansion
measurements of plastics. This range covers
the temperatures in which plastics are very
commonly used. When extending the range
when the measurement of a plastic whose
characteristics are not known through the
standard range is being made, particular attention
shall be paid to the factors mentioned
in 1.2 and special preliminary investigations
This method is under the jurisdiction of ASTM Committee
D-20 on Plastics and is the direct responsibility of
Subcommittee D20.30 on Thermal Properties.
Current edition approved May 4. 1979. Published July
1979. Originally published as D 6%-42. Last previous edition
D 6% - 70 (1978).
'Annual Book of ASTM Standards, Parts IO, 17.41, and
44.
a Annuol Book of ASTM Stondards, Part 35.

D 696
by thermo-mechanical analysis, such as that
prescribed in Method D 2236 for the location
of phase changes. may be required to avoid
excessive error. Other ways of locating phase
changes or transition temperatures using the
dilatometer itself may be employed to cover
the range of temperatures in question by
using smaller steps than 30°C or by observing
the rate of expansion during a steady rise in
temperature of the specimen. Once such a
transition point has been located, a separate
coefficient of expansion for a temperature
range below and above the transition point
shall be determined. For specification and
comparison purposes. the range from -30°C
to +30"C (provided it is known that no transition
point exists in this range) shall be used.
4. Summary of Method
4.1 This method is intended to provide a
means of determining the coefficient of linear
thermal expansion of plastics which are not
distorted or indented by the thrust of the
dilatometer on the specimen. The specimen
is placed at the bottom of the outer dilatometer
tube with the inner one resting on it. The
measuring device which is firmly attached to
the outer tube is in contact with the top of
the inner tube and indicates variations in the
length of the specimen with changes in temperature.
Temperature changes are brought
about by immersing the outer tube in a liquid
bath at the desired temperature.
5. Apparatus
5.1 Fused-Quartz- Tube Dilatometer suitable
for this method is illustrated in Fig. I. A
clearance of approximately 1 mm is allowed
hetween the inner and outer tubes.
5.2 Device for measuring the changes in
length (dial gage. LVCT. iii iXe eqiiivaknt)
shall be fixed on the mounting fixture so that
its position may be adjusted to accommodate
specimens of varying length (see 7.2). The
accuracy shall be such that the error of indication
will not exceed f 1.0 pn (4 x in.)
for any length change. The weight of the inner
silica tube plus the measuring device reaction
shall not exert a stress of more than 70 kPa (IO
psi) on the specimen so that the specimen is not
distorted or appreciably indented.
5.3 Scale or Caliper capable of measuring
the initial length of the specimen with an
accuracy of a0.S % .
5.4 Liquid Bath to control the temperature
of the specimen. The bath shall be so arranged
that uniform temperature over the length of
the specimen is assured. Means shall be provided
for stirring the bath and for controlling
its temperature within 50.2"C (0.4"F) at the
time of the temperature and measuring device
readings.
NOTE 3-Jt is preferable and not difficult to
avoid contact between the bath liquid and the test
specimen. If such contact is unavoidable. care must
be taken to select a liquid that will not affect the
physical properties of the material under test.
5.5 Thermometer or Thermocouple -The
bath temperature shall be measured by a
thermometer or thermocouple capable of an
accuracy of +O.I"C (a0.2"F).
6. Sampling
6. I Unless otherwise agreed upon between
interested parties. the material shall be sampled
as described in Sections 8 through 14 of
Recommended Practice D 1898.
7. Test Specimens
7. I The test specimens may be prepared by
machining. molding. or casting operations under
conditions which give a minimum of strain
or anisotropy. If specimens are cut from samples
that are suspected of anisotropy. the
specimens shall be cut along the principal
axes of anisotropy and the coefficient of linear
thermal expansion shall be measured on each
set of specimens.
7.2 The specimen length shall be between
50 mm (2 in.) and 125 mm (5 in.).
NOTE 4 -If specimens shorter than SO mm are
used. a loss in sensitivity results. If specimens
greatly longer than 125 mm are used. the tem
ture gradient along the specimen becomes diK%
to control within the prescribed limits. The length
used will be governed by the sensitivity and range
of the measuring device, the extension expected
and the accuracy desired. Generally speaking, the
longer the specimen and the more sensitive the
measuring device, the more accurate will be the
determination if the temperature is well controlled.
7.3 The cross section of the test specimen
may be round. square. or rectangular and
should fit easily into the outer tube of the
dilatometer without excessive play on the one
144

D 696
hand or friction on the other. The cross
section of the specimen shall be large enough
so that no bending or twisting of the specimen
occurs. Convenient specimen cross sections
are: 12.5 by 6.3 mm (I/? in. by l/4 in.). 12.5
by 3 mm (I/z by I/a in.). 12.5 mm (I/? in.) in
diameter or 6.3 mm (l/4 in.) in diameter. If
excessive play is found with some of the
thinner specimen, guide sections may be cemented
or otherwise attached to the sides of
the specimen to fill out the space.
7.4 The ends of the specimens shall be
reasonably flat and perpendicular to the
length axis of the specimen. The ends shall
be protected against indentation by means of
flat, thin steel plates cemented or otherwise
firmly attached to them before the specimen
is placed in the dilatometer. These plates
shall be 0.3 to 0.5 mm (0.012 to 0.020 in.)
in thickness.
8. Conditioning
8.1 Conditioning -Condition the test specmens
at 23 * 2°C (73.4 & 3.6"F) and 50 *
5 % relative humidity for not less than 40 h
prior to test in accordance with Procedure A
of Methods D 6 18 for those tests where conditioning
is required. In cases of disagreement,
the tolerances shall be kI"C (k1.8"F)
and k 2 9% relative humidity.
8.2 Test Conditions-Conduct tests in the
Standard Laboratory Atmosphere of 23 2
2°C (73.4 * 3.6"F) and 50 2 5 % relative
humidity. unless otherwise specified in the
test methods or in this specification. In cases
of disagreement. the tolerances shall be 2 1 "C
(2 1.8"F) and 22 % relative humidity.
9. Procedure
9.1 Measure the length of the conditioned
specimen at room temperature to the nearest
25 pm (0.0ui in.j with the scale or caiiper
(see 4.3).
9.2 Cement or otherwise attach the steel
plates to the ends of the specimen to prevent
indentation (see 7.4).
9.3 Mount the specimen in the dilatometer.
Carefully install the dilatometer in the
-30°C (-22°F) bath so that the top of the
specimen is at least 50 mm (2 in.) below the
liquid level of the bath. Maintain the temperature
of the bath in the range from -32°C to
28°C (-25 to -18°F) 2 0.2"C (0.4"F) until
the temperature of the specimen reaches the
temperature of the bath as denoted by no
further movement indicated by the measuring
device over a period of 5 to IO min. Record
the actual temperature and the measuring
device reading.
9.4 Without disturbing or jarring the dilatometer.
change to the +3O"C (86°F) bath.
so that the top of the specimen is at least 50
mm (2 in.) below the liquid level of the bath.
Maintain the temperature of the bath in the
range from +32 to +28"C (+82 to 90°F)
+0.2"C (O.4"F) until the temperature of the
specimen reaches that of the bath as denoted
by no further changes in the measuring device
reading over a period of 5 to IO min. Record
the actual temperature and the measuring
device reading.
9.5 Without disturbing or jarring the dilatometer.
change to the -30°C (-22°F) bath
and repeat the procedure in 9.3.
NOTE 5 -It is convenient to use alternately two
baths at the proper tem eratures. Great care should
be taken not to distur \ the apparatus during the
transfer of baths. Tall Thermos bottles have been
successfully used. The use of two baths is referred
because this will reduce the time requiretfto bring
the specimen to the desired temperature. The test
should be conducted in as short a time as possible
to avoid changes in physical properties during long
cxposures to high and ION tcmpcraturcs that might
possibly take place.
9.6 If the change in length per degree of
temperature difference due to heating does
not agree with the change in length per degree
due to cooling within IO % of their average.
the cause of the discrepancy shall be investigated
and. if possible. eliminated. The test
shall then be repeated until agreement is
reached.
10. Calculation
10.1 Calculate the coefficient of linear thermal
expansion over the temperature range
used as follows:
a = AL./L,,AT
where:
a = coefficient of linear thermal expansion
per degree Celsius.
AL = change in length of test specimen due
to heating or to cooling.
L,, = length of test specimen at room tem-
145

0 696
perature (AL and Lo being measured
in the same units). and
37' = temperature differences. "C, over
which the change in the length of the
specimen is measured.
The values of a for heating and for cooling
shall be averaged to give the value to be
reported.
11. Report
11.1 The report shall include the following:
11.1.1 Designation of material, including
name of manufacturer and information on
composition when known.
I I .I .2 Method of preparation of test specimen,
1 1.1.3 Form and dimensions of test specimen.
I I. I .4 Type of apparatus used,
1 1.1 .S Temperatures between which the
coefficient of linear thermal expansion has
been determined.
1 I .I .6 Average coefficient of linear thermal
expansion per degree Celsius,
1 I .I .7 Location of phase change or transition
point temperatures. if this is in the range
of temperatures used. and
1 I .I .8 Complete description of any unusual
behavior of the specimen. for example. differences
of more than 10 % in measured values
of expansion and contraction.
12. Precision
12.1 The intralaboratory coefficient of variation
by this method is 1 .S to 2 %.
146

FllR RECI)PJIM
\ L.V.D.T.
\
VITREOUS SILICA Ra]
VITREOUS SILICA TURF
15 Ma (,5% IN.)
FIG. 1 MTmbe Dibtometer.
The American Society for Testin and Materials takes no position respecting the validity of an atent rights asserted in
connritioti with my item mentione fir; :his srandard. Llsers cf this standard are .-xpr.-ssl advkedlkr de!mninnticn of the
validity of any such patent rights, and the risk of infiingvment of such rights. is entirely deir own responsibility.
ThiF standard is subject to revkion at any time by the responsible technical committee and must be reviewed every five
years and if not revised. either reapproved or withdrawn. Your comments are invited either fir revision of this standard or
fir additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration
I a meeting of the responsible technical committee, which you may attend. If you fie1 that your comments have not received
a fiir hearing you should make your vuws known to the ASTM Committee on Standards, 1916 Race SI., Philadelphia, Pa.
19103, which will schedule a further hearing regarding your comments. Failing satisfiction there, you may appeal IO the
ASTM Board of Directors.
147

4Ib
Designation: D 882 - 83
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
If not listed in the current combined index, will appear in the next edition
Standard Test Methods for
TENSILE PROPERTIES OF THIN PLASTIC SHEETING'
This standard is issued under the fixed designation D 882: the number immediately following the designation indicates the year of
original adoption or. in the case of revision. the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (0 indicates an editorial change since the last revision or reapproval.
T1ii.v mcvliod hus hivn approved,fi)r use by ugcncie.s qj'thi. Department oj' Dctfi.n.se to replace Method 1013 o$ Federal Test Method
Stundurd 406. und.fi)r listing in the DoD Index of Specifications and Standards.
1. Scope
I. 1 These test methods cover the determination
of tensile properties of plastics in the form
of thin sheeting, including film (less than I .O mm
(0.04 in.) in thickness).
NOTE I-Film has been arbitrarily defined as sheeting
having nominal thickness not greater than 0.25 mm
(0.010 in.).
NOTE 2-Tensile properties of plastics 1 .O mm (0.04
in.) or greater in thickness shall be determined according
to Test Method D 638.
I .2 Two types of tension tests are described in
these test methods, differing basically only in
manner of load application. These test methods
may be used to test all plastics within the thickness
range described and the capacity of the
machine employed.
I .2.1 Method A. Stalic Weighing-Conslant-
Ratcc$Grip Separation Test-This method employs
a constant rate of separation of the grips
holding the ends of the test specimen.
1.2.2 Melhod B. Pendtilum Weighing-Constant-Rare-ocPower-Grip
Motion Test-This
method employs a constant rate of motion of
one grip and a variable rate of motion of the
second grip. The variable-rate grip is attached to
a pendulum weighing head, and its movement is
dependent on the load-deformation behavior of
the material under test.
1.3 Specimen extension may be measured in
these methods by grip separation, extension indicators,
or displacement of gage marks.
1.4 A procedure for determining the tensile
modulus of elasticity is included, using Method
A at one strain rate.
1.5 The values stated in SI units are to be
regarded as the standard.
NOTE .3-This
modulus determination procedure is
based on the use of grip separation as a measure of
extension; however, the desirability of using extension
indicators accurate to k I .O % or better as specified in
Test Method D 638 is recognized, and provision for the
use of such instrumentation is incorporated in the
procedure.
I .6 This .stundurd rnuj- involve hazardous matc~riul.~,
operations, and equipment. This standard
docs not pirrport to uddress all of'thc. sakty proh-
Ions associated with its i~sc. It is the responsihilit??
oj whoever irses lhis slandard to con.sirlt and
estuhlish uppropriate sufkty and health practices
and determine ihe applicahility o~rcgirlatory limitations
prior to irse.
2. Applicable Documents
2.1 ASTM Standards:
D374 Test Methods for Thickness of Solid
Electrical Insulation'
D6 I8 Methods of Conditioning Plastics and
Electrical Insulating Materials for Testing'
D638 Test Method for Tensile Properties of
Plastics'
E 69 1 Practice for Conducting an Interlaboratory
Test Program to Determine the Precision
of Test Methods3
3. Significance and Use
3.1 Tensile properties determined by these
methods are of value for the identification and
characterization of materials for control and
specification purposes. Tensile properties may
' These methods are under the jurisdiction of ASTM Committee
D-20 on Plastics and are the direct responsibility of
Subcommittee D20. IO on Mechanical Properties.
Current edition approved July 29. 1983. Published October
1983. Originally published as D882 - 46 T. Last previous
edition D 882 - 81.
Annual Book qf ASTM Standard.s, Vol08.0 I.
'.Jnnrtul Rook ofASTM Standards, Vols 08.03 and 14.02.
I48

D 882
vary with specimen thickness, method of preparation,
speed of testing, type of grips used, and
manner of measuring extension. Consequently,
where precise comparative results are desired,
these factors must be carefully controlled. Since
the actual loading rates vary between Methods A
and B, the results obtained using these two methods
cannot be directly compared. Method A is
preferred and shall be used for referee purposes,
unless otherwise indicated in particular material
specifications.
3.2 Tensile properties may be utilized to provide
data for research and development and engineering
design as well as quality control and
specification. However, data from such tests cannot
be considered significant for applications differing
widely from the load-time scale of the test
employed.
3.3 The tensile modulus of elasticity is an
index of the stiffness of thin plastic sheeting. The
reproducibility of test results is good when precise
control is maintained over all test conditions.
When different materials are being compared for
stiffness, specimens of identical dimensions must
be employed.
3.4 The tensile energy to break (TEB) is the
total energy absorbed per unit volume of the
specimen up to the point of rupture. In some
texts this property has been referred to as toughness.
It is used to evaluate materials that may be
subjected to heavy abuse or that might stall web
transport equipment in the event of a machine
malfunction in end-use applications. However,
the rate of strain, specimen parameters, and especially
flaws may cause large variations in the
results. In that sense, caution is advised in utilizing
TEB test results for end-use design applications.
3.5 Materials that fail by tearing give anomalous
data which cannot be compared with those
from normal failure.
4. Definitions
4.1 Definitions of terms and symbols relating
to tension testing of plastics appear in the Annex
to Test Method D 638.
4.2 tear failure-a tensile failure characterized
by fracture initiating at one edge of the specimen
and progressing across the specimen at a rate
slow enough to produce an anomalous loaddeformation
curve.
4.3 line grips-grips having faces designed to
concentrate the entire gripping force along a single
line perpendicular to the direction of testing
stress. This is usually done by combining one
standard flat face and an opposing face from
which protrudes a half-round.
5. Apparatus
5. I Grips-A gripping system that minimizes
both slippage and uneven stress distribution.
NOTE 4-Grips lined with thin rubber, crocus-cloth,
or pressure-sensitive tape as well as file-faced or serrated
grips have been successfully used for many materials.
The choice of grip surface will depend on the material
tested, thickness, etc. More recently, line grips padded
on the round face with I .O-mm (40-mil) blotting paper
have been found superior. Air-actuated grips have been
found advantageous, particularly in the case of materials
that tend to “neck” into the grips, since pressure
is maintained at all times. In cases where samples
frequently fail at the edge of the grips, it may be
advantageous to increase slightly the radius of curvature
of the edges where the grips come in contact with the
test area of the specimen.
5.2 Thickness Gage-A dead-weight dial micrometer
as prescribed in Method C of Test
Methods D 374, reading to 0.0025 mm (O.OOO1
in.) or less.
5.3 Width-Measuring Devices-Suitable test
scales or other width measuring devices capable
of measuring 0.25 mm (0.010 in.) or less.
5.4 Specimen Cutter-Razor blades, fixtures
incorporating razor blades, suitable paper cutters,
or other devices capable of cutting the specimens
to the proper width and producing straight, clean,
parallel edges with no visible imperfections, shall
be used. Devices that use razor blades have
proved especially suitable for materials having an
elongation-at-fracture above 10 to 20 %. A device
consisting of two parallel knives mounted firmly
against a precision-ground base shear block (similar
to a paper cutter) has also proved satisfactory.
The use of striking dies is not recommended
because of poor and inconsistent specimen edges
which may be produced. It is imperative that the
cutting edges be kept sharp and free from visible
scratches or nicks.
5.5 Extension Indicalors (if employed) shall
conform to requirements specified in Test
Method D 638. In addition, such apparatus shall
be so designed as to minimize stress on the
specimen at the contact points of the specimen
and the indicator (see 8.3).
5.6 Testing Machines:
5.6.1 For Method A-A testing machine of
149

the constant rate-of-jaw-separation type. The machine
shall be equipped with a weighing system
that moves a maximum distance of 2 % of the
specimen extension within the range being measured.
The machine shall be equipped with a
device for recording the tensile load and the
amount of separation of the grips; both of these
measuring systems shall be accurate to +-2 %.
The rate of separation of the jaws shall be uniform
and capable of adjustment from approximately
1.3 to 500 mm (0.05 to 20 in.)/min in
increments necessary to produce the strain rates
specified in 9.3 and 9.4. This method (A) shall
be used for tensile modulus of elasticity measurements
(Note 5).
5.6.2 For Method B-A testing machine of
the pendulum type. This machine shall be
equipped with a pendulum weighing head to
measure the load applied to the test specimen
and a device for indicating or recording the tensile
load carried by the specimen with an accuracy
of +2 %. The rate of travel of the poweractivated
grip shall be uniform and capable of
adjustment to 50.8 and 508 mm (2 and 20 in.)/
min.
NOTE 5-A high response speed in the recording
system is desirable, particularly when relatively high
strain rates are employed for rigid materials. The speed
of pen response for recorders is supplied by manufacturers
of this equipment. Care must be taken to conduct
tests at conditions such that response time (ability of
recorder to follow actual load) will produce less than
2 % error.
6. Test Specimens
6.1 The test specimens shall consist of strips
of uniform width and thickness at least 50 mm
(2 in.) longer than the grip separation used.
6.2 The nominal width of the specimens shall
be not less than 5.0 mm (0.20 in.) or greater than
25.4 mm (1.O in.).
6.3 A width-thickness ratio of at least eight
shaii be used. Narrow specimens magnify effects
of edge strains or flaws, or both.
6.4 The utmost care shall be exercised in cutting
specimens to prevent nicks and tears which
are likely to cause premature failures (Note 6).
The edges shall be parallel to within 5 % of the
width over the length of the specimen between
the grips.
NOTE 6-Microscopical examination of specimens
may be used to detect flaws due to sample or specimen
preparation.
6.5 Wherever possible, the test specimens
shall be selected so that thickness is uniform to
within 10 % of the thickness over the length of
the specimen between the grips in the case of
materials 0.25 mm (0.010 in.) or less in thickness
and to within 5 % in the case of materials greater
than 0.25 mm (0.010 in.) in thickness but less
than 1 .OO mm (0.040 in.) in thickness.
NOTE 7-In cases where thickness variations are in
excess of those recommended in 6.5, results may not
be characteristic of the material under test.
6.6 If the material is suspected of being anisotropic,
two sets of test specimens shall be prepared
having their long axes respectively parallel
with and normal to the suspected direction of
anisotropy.
6.7 For tensile modulus of elasticity determinations,
a specimen gage length of 250 mm (10
in.) shall be considered as standard. This length
is used in order to minimize the effects of grip
slippage on test results. When this length is not
feasible, test sections as short as 100 mm (4 in.)
may be used if it has been shown that results are
not appreciably affected. However, the 250-mm
gage length shall be used for referee purposes.
The speed of testing of shorter specimens must
be adjusted in order for the strain rate to be
equivalent to that of the standard specimen.
NOTE 8-Two round robins4 have shown that, for
materials of less than 0.25-mm ( IO-mil) thickness, line
grips padded on the round side with 1.0-mm (40-mil)
blotting paper give the same results with a 100-mm test
section as a 250-mm test section produces with flatface
grips.
Note 9-Excessive jaw slippage becomes increasingly
difficult to overcome in cases where high modulus
materials are tested in thicknesses greater than 0.25 mm
(0.010 in.).
7. Conditioning
7.1 Conditioning-Condition the test specimens
at 23 f 2°C (73.4 + 3.6"F) and 50 f 5 %
reiative humidity for not iess than 40 h prior to
test in accordance with Procedure A of Methods
D 6 18 for those tests where conditioning is required.
In cases of disagreement, the tolerances
shall be 1 "C ( 1.8"F) and 22 % relative humidity.
7.2 Test Conditions-Conduct tests in the
Standard Laboratdry Atmosphere of 23 rt 2°C
(73.4 rt 3.6"F) and 50 f 5 % relative humidity,
A summary report is available from ASTM Headquarters.
Request RR:D20-1058.
150

D 882
unless otherwise specified in the test methods or
in this specification. In cases of disagreements,
the tolerances shall be f 1°C (f 1.8"F) and f 2 %
relative humidity.
8. Number of Test Specimens
8. I In the case of isotropic materials, at least
five specimens shall be tested from each sample.
8.2 In the case ofanisotropic materials, at least
ten specimens, five normal and five parallel with
the principal axis of anisotropy, shall be tested
from each sample.
8.3 Specimens that fail at some obvious flaw
or that fail outside the gage length shall be discarded
and retests made, unless such flaws or
conditions constitute a variable whose effect is
being studied. However, jaw breaks (failures at
the grip contact point) are acceptable if it has
been shown that results from suck tests are in
essential agreement with values obtained from
breaks occurring within the gage length.
NOTE l&In the case of some materials, examination
of specimens, prior to and following testing, under
crossed optical polarizers (polarizing films) provides a
useful means of detecting flaws which may be, or are,
responsible for premature failure.
9. Speed of Testing
9. I The speed of testing is the rate of separation
of the two members (or grips) of the testing
machine when running idle (under no load). This
rate of separation shall be maintained within 5 %
of no-load value when running under full-capacity
load.
9.2 The speed of testing shall be calculated
from the required initial strain rate as specified
in Table 1. The rate of grip separation may be
determined for the purpose of this test method
from the initial strain rate as follows:
A=BC
WhPTP:
A = rate of grip separation, mm (or in.)/min
B = initial distance between grips, mm (or in.),
and
C = initial strain rate, mm/mm.min (or in./
in.. min).
9.3 The initial strain rate shall be as in Table
I unless otherwise indicated by the specification
for the material being tested.
Note 1 I-Results obtained at different initial strain
rates are not comparable; consequently, where direct
comparisons between materials in various elongation
classes are required, a single initial strain rate should
be used. For some materials it may be advisable to
select the strain rates on the basis of percentage elongation
at yield.
9.4 In cases where conflicting material classification,
as determined by percentage elongation
at break values, results in a choice of strain rates,
the lower rate shall be used.
9.5 If modulus values are being determined,
separate specimens shall be used whenever strain
rates and specimen dimensions are not the same
as those employed in the test for other tensile
properties.
10. Procedure
10.1 Select a load range such that specimen
failure occurs within its upper two thirds. A few
trial runs may be necessary to select a proper
combination of load range and specimen width.
10.2 Measure the cross-sectional area of the
specimen at several points along its length. Measure
the width to an accuracy of 0.25 mm (0.010
in.) or better. Measure the thickness to an accuracy
of 0.0025 mm (0.OOOl in.) or better for films
less than 0.25 mm (0.0 IO in.) in thickness and to
an accuracy of I % or better for films greater
than 0.25 mm (0.010 in.) but less than 1.0 mm
(0.040 in.) in thickness.
10.3 The initial grip separation shall be at least
50 mm (2 in.) for materials having a total elongation
at break of 100 % or more, and at least
100 mm (4 in.) for materials having a total
elongation at break of less than 100 %.
NOTE 12-Since slippage is a potential problem in
these tests, as great an initial distance between grips as
possible should be employed.
10.4 Set the rate of grip separation to give the
desired strain rate based on the initial distance
between the grips (Note 13). Balance, zero, and
calibrate the load weighing and recording system.
Nun i 3-Suggesied crosshead speeds and iniiiai
grip separation to give the desired initial strain rate
described in Table I are shown in Table 2.
10.5 In cases where it is desired to measure a
test section other than the total length between
the grips, mark the ends ofthe desired test section
with a soft, fine wax crayon or with ink. Do not
scratch these marks onto the surface since such
scratches may act as stress raisers and cause
premature specimen failure. Extensometers may
be used if available; in this case, the test section
151

D 882
will be defined by the contact points of the extensometer.
NOTE 14-Measurement of a specific test section is
necessary with some materials having high elongation.
As the specimen elongates, the accompanying reduction
in area results in a loosening of material at the inside
edge of the grips. This reduction and loosening moves
back into the grips as further elongation and reduction
in area takes place. In effect this causes problems similar
to grip slippage, that is, exaggerates measured extension.
10.6 Place the test specimen in the grips of
the testing machine, taking care to align the long
axis of the specimen with an imaginary line
joining the points of attachment of the grips to
the machine. Tighten the grips evenly and firmly
to the degree necessary to minimize slipping of
the specimen during test.
10.7 Start the machine and record load versus
extension.
10.7.1 When the total length between the grips
is used as the test area, record load versus grip
separation.
10.7.2 When a specific test area has been
marked on the specimen, follow the displacement
of the edge boundary lines with respect to
each other with dividers or some other suitable
device. If a load-extension curve is desired, plot
various extensions versus corresponding loads
sustained, as measured by the load indicator.
10.7.3 When an extensometer is used, record
load versus extension of the test area measured
by the extensometer.
10.8 If modulus values are being determined,
select a load range and chart rate to produce a
load-extension curve of between 30 and 60" to
the X axis. For maximum accuracy, use the most
sensitive load scale for which this condition can
be met. The test may be discontinued when the
load-extension curve deviates from linearity.
10.9 In the case of materials being evaluated
for secant modulus, the test may be discontinued
when the specified extension has been reached.
IO. 10 If tensile energy to break is being determined,
some provision must be made for integration
of the stress-strain curve. This may be
either an electronic integration during the test or
a subsequent determination from the area of the
finished stress-strain curve (see Annex A 1).
1 1. Calculations
1 1. I Breaking Factor (nominal) shall be calculated
by dividing the maximum load by the
original minimum width of the specimen. The
result shall be expressed in force per unit of
width, usually newtons per metre (or pounds per
inch) of width, and reported to three significant
figures. The thickness of the film shall always be
stated to the nearest 0.0025 mm (O.OOO1 in.).
Example-Breaking Factor = 1.75 kN/m
(10.0 Ibf/in.) of width for 0.1300-mm (0.0051-
in.) thickness.
NOTE 15-This method of reporting is useful for
very thin films (0.13 mm (0.005 in.) and less) for which
breaking load may not be proportional to cross-sectional
area and whose thickness may be dificult to
determine with precision. Furthermore, films which are
in effect laminar due to orientation, skin effects, nonuniform
crystallinity, etc., have tensile properties disproportionate
to cross-sectional area.
11.2 Tensile Strength (nominal) shall be calculated
by dividing the maximum load by the
original minimum cross-sectional area of the
specimen. The result shall be expressed in force
per unit area, usually megapascals (or poundsforce
per square inch). This value shall be reported
to three significant figures.
NOTE 16-When tear failure occurs, so indicate and
calculate results based on load and elongation at which
tear initiates, as reflected in the loaddeformation curve.
11.3 Tensile Strength at Break (nominal) shall
be calculated in the same way as the tensile
strength except that the load at break shall be
used in place of the maximum load (Notes 16
and 17).
NOTE 17-In many cases tensile strength and tensile
strength at break are identical.
1 1.4 Percentage Elongation at Break shall be
calculated by dividing the elongation at the moment
of rupture of the specimen by the initial
gage length of the specimen and multiplying by
100. When gage marks or extensometers are used
to define a specific test section, only this length
shall be used in the calculation, otherwise the
distance between the grips shall be used. The
result shall be expressed in percent and reported
to two significant figures (Note 16).
1 1.5 Yield Strength, where applicable, shall be
calculated by dividing the load at the yield point
by the original minimum cross-sectional area of
the specimen. The result shall be expressed in
force per unit area, usually megapascals (or
pounds-force per square inch). This value shall
be reported to three significant figures. Alternatively,
for materials that exhibit Hookean behav-
152

D 882
ior in the initial part of the curve, an offset yield
strength may be obtained as described in the
Appendix of Test Method D 638. In this case the
value should be given as “yield strength at--%
ofTse t .”
I I .6 Pcwvnrugi> Elongution UI Yield where applicable
shall be calculated by dividing the elongation
at the yield point by the initial gage length
of specimen and multiplying by 100. When gage
marks or extensometers are used to define a
specific test section, only this length shall be used
in the calculation. The results shall be expressed
in percent and reported to two significant figures.
When offset yield strength is used, the elongation
at the offset yield strength may be calculated.
11.7 Elastic Modulus shall be calculated by
drawing a tangent to the initial linear portion of
the load-extension curve, selecting any point
on this tangent, and dividing the tensile stress by
the corresponding strain. For purposes of this
determination, the tensile stress shall be calculated
by dividing the load by the average original
cross section of the test section. The result shall
be expressed in force per unit area, usually megapascals
(or pounds-force per square inch), and
reported to three significant figures.
11.8 Secanr Modulus at a designated strain
shall be calculated by dividing the corresponding
stress (nominal) by the specified strain. Elastic
modulus values are preferable and shall be calculated
whenever possible. However, for materials
where no proportionality is evident, the
secant value shall be calculated. Draw the tangent
as directed in 11.7 and start the measurement of
strain where the tangent line goes through zero
stress. The stress to be used in the calculation is
then determined by dividing the load at the designated
strain on the load-extension curve by the
original average cross-sectional area of the specimen.
11.9 For each series of tests, the arithmetic
mean of all values obtained shall be calculated
to the proper number of significant figures.
1 1.10 The standard deviation (estimated)
shall be calculated as follows and reported to two
significant figures:
s = J(ZX2 - nX2)/(n - I )
where:
s = estimated standard deviation,
X = value of a single observation,
n = number of observations, and
X = arithmetic mean of the set of observations.
1 I . 11 Tensile Energy lo Break where applicable
shall be calculated by integrating the energy
per unit volume under the stress-strain curve or
by integrating the total energy absorbed and dividing
it by the volume of the original gage region
of the specimen. As indicated in Annex AI, this
may be done directly during the test by an electronic
integrator, or subsequently by computation
from the area of the plotted curve. The result
shall be expressed in energy per unit volume,
usually in megajoules per cubic metre (or inchpounds-force
per cubic inch). This value shall be
reported to two significant figures.
11.12 See Appendix X 1 for information on
toe compensation.
12. Report
12.1 The report shall include the following:
12.1.1 Complete identification of the material
tested, including type, source, manufacturer’s
code number, form, principal dimensions, previous
history, and orientation of samples with
respect to anisotropy (if any),
12.1.2 Method of preparing test specimens,
12.1.3 Thickness, width, and length of test
specimens,
12.1.4 Number of specimens tested,
12.1.5 Strain rate employed,
12. I .6 Grip separation (initial),
12.1.7 Crosshead speed (rate of grip separa-
tion),
12.1.8 Gage length (if different from grip separation),
12.1.9 Type of grips used, including facing (if
any),
12.1.10 Test method (A or B),
12.1.11 Conditioning procedure (test conditions,
temperature, and relative humidity if nonstandard),
12.1.12 Anomalous behavior such as tear failure
and failure at a grip,
12.1. I 3 Average breaking factor and standard
deviation,
12.1.14 Average tensile strength (nominal)
and standard deviation,
12.1.15 Average tensile strength at break
(nominal) and standard deviation,
12.1. I6 Average percentage elongation at
break and standard deviation,
12. I. 17 Where applicable: Average tensile energy
to break and standard deviation,
12.1.18 In the case of materials exhibiting
“yield” phenomenon:
153

D 882
Average yield strength and standard deviation,
and
Average percentage elongation at yield and
standard deviation,
12.1.19 For mdterials which do not exhibit a
yield point:
Average-% offset yield strength and standard
deviation, and
Average percentage elongation at-% offset
yield strength and standard deviation,
12.1.20 Average modulus of elasticity and
standard deviation (if secant modulus is used, so
indicate and report strain at which calculated),
and
12. I .2 1 When an extensometer is employed,
so indicate.
13. Precision and Bias
13.1 An interlaboratory test was run in 1977
in which randomly drawn samples of four thin
(- 0.025 mm (0.001-in.)) materials were tested
with five specimens in each laboratory. Elastic
(tangent) modulus measurements were made by
six laboratories, and secant (I %) modulus measurements
were taken by five laboratories, with
one laboratory in common. The four materials
were 0.0014-in. low-density polyethylene
(LDPE), 0.00 16411. highdensity polyethylene
(H DPE), 0.00 I I -in. polypropylene (PP), and
0.0009-in. poly(ethy1ene terephthalate) (PET).
The relative precision obtained in this interlaboratory
study is in Table 3.
13.1.1 In deriving the estimates in Table 3,
statistical outliers were not removed, in keeping
with Practice E 69 I. In the table, Sa; ?6 is defined
as standard deviation, expressed as a percentage
of the average value, of one specimen replicate
measurement of modulus for one material in one
laboratory during the course of one day. Si., % is
defined as standard deviation, expressed as a
pxcentage cf the grand zverage value, of mu!&
laboratory measurements of modulus for one
material, with the within-laboratory component
of variability removed.'
13.2 For within-laboratory measurements, for
n replicate specimens per sample of one material,
the standard deviation, S,, of a mean value, X, is
as follows:
S, = Sw/(n)'/'
13.3 For between-laboratory measurements,
for n replicate specimens per sample of one material
in each lab, the standard deviation, SR, for
the distribution of lab means, f, about the grand
mean, X, is as follows:
s/l = (S? + SL*)'/'
NOTE 18-Since S, as used here (and in the interlaboratory
study) does not contain all of the components
of variability that could be included in the definition of
S,for example different operators, different days, etc.,
the variability associated with these components is
transferred into the value of SL.
13.4 From derived values of S, and SR, and
by selection of the appropriate value of the deviate,
u, from a table of the normal distribution
for any chosen confidence level, other statistics
can be derived as desired, such as 95 % (or other)
probability limits for an 2 in one laboratory, the
least significant difference between means for one
material in two laboratories, etc.
13.5 An interlaboratory test was run in 1981-
82 in which randomly drawn samples of six
materials (one of these in three thicknesses) ranging
in thickness from 0.019 to 0.178 mm
(0.00075 to 0.007 in.) were tested in seven laboratories.
A test result was defined as the mean of
five specimen determinations. The materials and
their thicknesses are identified in Tables 4 to 8.
which correspond to Table 2 in Practice E 691.
Each of Tables 4 to 8 contain data for one of the
following properties: tensile yield stress, yield
elongation, tensile strength, tensile elongation at
break, and tensile energy at break (see Note 19h6
13.6 Bias-There is no basis for defining the
bias of the values obtained by this test method.
NOTE 19-Subsequent to filing the research report.
examination of the LDPE used in this study between
crossed polariLers revealed lengthwise lines representing
substanila! widthwig vanatinn in mnlecular orientation
that probably was not successfully randomized out
of the SI values.
' Supporting data are available on loan from ASTM Headquarters.
Request RH:D20- 1084.
*Supporting data are available on loan from ASTM Headquarters.
Request RR:I>ZO-I 101.
154

~~~ ~~
TABLE 1
SpeedofTesting
Modulus of Elasticity Determination
A 0.1
Determinations other than Elastic Modulus
A Less than 20 0. I
20 to 100 0.5
Greater than 100 10.0
B Less than 100 0.5
Greater than 100 10.0
Method
Percentage Elongation
at Break
TABLE 2 Crosshead Speeds and Initial Grip !%paration
Initial Strain Rate, Initial Grip Separation Rate of Grip Separation
mm/mm .min
mm in. mm/min in./min
(Win..min)
Modulus of Elasticity Determination
A 0. I 250 10 25 1 .o
Determinations other than Elastic Modulus
A Less than 20 0. I 125 5 12.5 0.5
20 to 100 0.5 100 4 50 2.0
Greater than 100 10.0 50 2 500 20.0
B Less than 100 0.5 100 4 50 2.0
Greater than 100 10.0 50 2 500 20.0
TABLE 3 Precision Data
Tangent Modulus
Material Average, MPa (psi) SW, % SI., %
LDPE 372 (53 900) 7.5 16
HDPE 1320(191 OOO) 6.4 8
PP 2930(425 OOO) 5.4 7
PET 4630 (672 OOO) 4.6 8
Secant Modulus
LDPE 310 (45 OOO) 10.5 6
HDPE 1030(150 OOO) 4.9 6
PP 2570(372 OOO) 2.8 7
PET 4410(640 OOO) 3.5 4
TABLE 4 Yield Stress
Material Thickness, mils Average, IO’ psi (S,); IO’ psi (SL): IO’ psi /(r): IO’ psi I(R)P IO’ psi
LDPE 1 in .” !.49 O.OS! 0.!2 0.14 0.37
HDPE I .o 4.33 0.084 0.13 0.24 0.44
PP 0.75 6.40 0.13 0.50 0.37 I .46
Pc 4.0 8.59 0.072 0.28 0.20 0.82
CTA 5.3 11.4 0.12 0.49 0.34 I .43
PET 4.0 14.3 0.12 0.20 0.34 0.66
PET 2.5 14.4 0.14 0.52 0.40 I .52
PET 7 .O 14.4 0.13 0.34 0.37 1.03
A (S,z = The estimated repeatability standard deviation within laboratories for the ,th material.
(SL), = The estimated between laboratory variability, expressed as the square root of the component of variance for the fh
material.
c/(r)i= 2 &(S,),. See Practice E691.
/(R), = 2 ~((SL),’ + (S,):)’’z. See Practice E 691.
155

~~ ______~
~
TABLE 5 Yield Elongation
PP
PET
PET
PET
CTA
Pc
HDPE
LDPE
NOTE-*
~~
0.75
2.5
4.0
7.0
5.3
4.0
I .o
1 .O
Table 4 for footnote explanation.
3.5
5.2
5.3
5.4
5.4
6.9
8.8
10.0
0.15
0.26
0.25
0.14
0.19
0.24
0.32
0.55
0.38
0.88
0.55
I .04
0.97
0.95
I .79
3.36
0.42
0.74
0.7 1
0.40
0.54
0.68
0.9 I
I .56
I .2
2.6
I .7
3 .O
2.8
2.8
5.2
9.6
TABLE 6 Tensile Strength
Material Thickness, mils Average, IO3 psi (S,); IO’ psi (SLIP IO3 psi IO3 psi I(RIiD IO3 psi
LDPE I .o 3.42
HDPE I .o 6.87
Pc 4.0 12.0
CTA 5.3 14.6
PP 0.75 28.4
PET 4.0 28.9
PET 7.0 30.3
PET 2.5 30.6
NOTE-*
Table 4 for footnote explanation.
TABLE 7
0.14 0.5 I
0.27 0.76
0.34 0.86
0.20 I .36
1.57 4.28
0.65 1.09
0.83 I .02
I .22 2.34
Elongation at Break
0.40 I .5
0.76 2.3
0.96 2.6
0.57 3.9
4.4 12.9
I .8 3.6
2.3 3.7
3.4 7.5
Material Thickness, mils Average, % csr,;. % (SL),B, %I 4rd % I(RhD, %
CTA
PP
PET
PET
PET
5.3
0.75
2.5
7.0
4.0
26.4
57.8
I20
I32
134
1 .o
4.4
8.0
5.8
4.4
4.2
11.9
12.2
8.9
11.4
3
12
23
16
12
12
36
41
30
35
Pc
4.0
I55
5.4
16.2
I5
48
LDPE
I .o
205
24.4
69. I
69
210
HDPE
I .O
570
26.0
87.9
74
260
Nan-See Table 4 for footnote explanation.
TABLE 8 Tensile Energy to Break
Average, 10) (S,),” IO3 (sL): 103 I(rhc 10’ I(R)P IO’
Material Thickness, mils - in./lb - in./lb
-
in./lb
-
in./lb
- in./lb
in.’ in.3 in? in.3 1n.3
CTA
LDPE
PP
PC
HDPE
PET
PET
PET
NOTE-see
5.0
I .o
0.75
4.0
I .o
2.5
4.0
7 .O
Table 4 for footnote explanation.
3.14
5.55
11.3
12.9
26.0
26.1
27. I
28.4
0.14
0.84
1.19
0.59
I .87
2.13
I .42
1.71
0.69
2.32
2.87
1.43
4.66
3.62
2.35
2.12
0.4 2.0
2.4 7.0
3.4 8.8
I .7 4.4
5.3 14.2
6.0 11.9
4.0 7.8
4.8 7.7
156

ANNEX
(Mandatory Information)
Al. DETERMINATION OF TENSILE ENERGY TO BREAK
A1.I Tensile energy to break (TEB) is defined by
the area under the stress-strain curve, or
TEB = s“ Sdr
where S is the stress at any strain, e; and CT is the strain
at rupture. The value is in units of energy per unit
volume of the specimen’s initial gage region. TEB is
most conveniently and accurately measured with a
tension tester equipped with an integrator. The calculation
is then:
TEB
(full scale load) (chart speed)
(crosshead speed/chart speed)
= (VK)
(mean caliper) (specimen width)
(gage length)
where I is the integrator count reading and K is the
maximum possible count per unit time for a constant
full scale load. This whole calculation is typically done
electronically. The results are best expressed in megajoules
per cubic metre (or inch-pounds-force per cubic
inch).
A1.2 Without an integrator, the area under the recorded
stress-strain curve can be measured by planimeter,
counting squares, or weighing the cut-out
curve. These techniques are time-consuming and likely
to be less accurate, since the load scale on some chart
paper is not in round-number dimensions. Moreover,
if the curve coordinates are in terms of force and
extension instead of stress and strain, the calculated
energy, corresponding to the measured area, must be
divided by the product of gage length, specimen width,
and mean caliper:
TEB
(curve area) (force per unit chart scale)
- (extension per unit chart travel)
(mean caliper) (specimen width)
(gage length)
A1.3 For example, if the area under a force-extension
curve is 60 OOO mm2, the load coordinate is 2.0
N/mm of chart scale, the extension coordinate is 0.25
mm of extension per mm of chart travel, and the
specimen dimensions are 0. I mm caliper, 15 mm width
and lo0 mm gage length, then the calculation for tensile
energy to break is:
TEB
(60 000 mm2) (2.0
-
N/mm) (0.25 x IO-’ m/mm)
(0.1 x IO-’m) (I5 x IO-’ m) (100 x IO-’ m)
TEB = 200 MJ/m3
157

APPENDIX
(Nonmandatory Information)
Xl. TOE COMPENSATION
X I. I In a typical stress-strain curve (Fig. X 1. I ) there
is a toe region, AC, which does not represent a property
of the material. It is an artifact caused by a takeup of
slack, and alignment or seating of the specimen. In
order to obtain correct values of such parameters as
modulus, strain, and offset yield point, this artifact must
be compensated for to give the corrected zero point on
the strain or extension axis.
X 1.2 In the case of a material exhibiting a region of
Hookean (linear) behavior (Fig. X 1. I), a continuation
of the linear (C'D) region of the curve is constructed
through the zero-stress axis. This intersection (B) is the
corrected zero-strain point from which all extensions
or strains must be measured, including the yield offset
(BE), if applicable. The elastic modulus can be determined
by dividing the stress at any point along the line
CD (or its extension) by the strain at the same point
(measured from point E, defined as zero-strain).
X 1.3 In the case of a material that does not exhibit
any linear region (Fig. X1.2), the same kind of toe
correction of the zero-strain point can be made by
constructing a tangent to the maximum slope at the
inflection point (H'). This is extended to intersect the
strain axis at point E', the corrected zero-strain point.
Using point B' as zero strain, the stress at any point
(G') on the curve can be divided by the strain at that
point to obtain a secant modulus (slope of line B' G').
For those materials with no linear region, any attempt
to use the tangent through the inflection point as a basis
for determination of an offset yield point may result in
unacceptable error.
A B E Strain
NOTE-some chart recorders plot the mirror image of this
graph.
FIG. XI.l Material with Haokean Region
158

I
Strain
NOTE-some chart recorders plot the mirror image of this
graph.
FIG. XI.2 Material with No Hookean Region
7'llc .4 mivicun Society./i)r Tecting and Murerial.s takes no position respecting the validity cfany putcnr righ1.s asscrtcd in tnnncction
with unv iicrn nicntioncd in this standurd. Userr 01'thi.c standard urc csprcssly advised that diwrmination of the validity of any such
putcnt rights. and the risk ofinfiingiv"t of such rights. urc intircly thcir onn re.sponsihilily.
This stundurd is tirbjci~to rcvision at any time bv thc~ responsihk technical commirke und must be reviewed cvivjj,/ivr ycars and
I/' titit rcviscd. cVthcr rcupproved or withdrawn. Your cvm"~s are invitcd i4hcr .fiw revision of this srandard or jiir additionul
,stundurd.s and shoirld hi. addriwcd to ASTM I~c.crdqiiartiw. Yoirr tamtnmts nil1 receive cari$il consideration UI a meeting of the
rc..sponvihlc tcchtiii~cil tommitti.e which jroic may attcnd. l/yoirji.(.l that ymr cctnmmts have not rc.ceived a Juir hearing you shoiild
tnuki~ !.ow vicw know to the .4STM Committee on Stundards. I916 Race SI., Philadelphia. Pa. 19/03.
159

Designation: D 896 - 84
AMERICAN SOCIETY FOR TESTING AND MATERIALS
la16 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
RESISTANCE OF ADHESIVE BONDS TO CHEMICAL
REAGENTS'
This standard is issued under the fixed designation D 896; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval..
This method has been approved for use by agencies of the Department of Defense to replace method 201 I. I of Federal Test Method
Standard No. I75a and for listing in the DoD Index of Specijkations and Standards.
1. scope
1.1 This test method covers the testing of all
types of adhesives for resistance to chemical reagents.
It includes provisions for reporting loss
in strength in accordance with ASTM test methods
for strength properties of adhesives.
NOTE I-See ASTM Test Methods D 897, Test for
Tensile Properties of Adhesive Bonds? D 2095, Tensile
Strength of Adhesives by Means of Bar and Rod Specimens?
D 1344, Cross-Lap Specimens for Tensile Prop
erties of Adhesives? D 903, Test for Peel or Stripping
Strength of Adhesive Bonds? D 1876, Test for Peel
Resistance of Adhesives (T-Peel Test)? D 905, Test for
Strength Properties of Adhesive Bonds in Shear by
Compression Loading,' D 906, Test for Streogth hap
erties of Adhesives in Ply\;vood Type Construction in
Shear by .Tension Loading? D 950, Test for Impact
Strength of Adhesive Bonds? D 1002, Test for Smngth
Properties of Adhesive in Shear by Tension Loading
(Metal-to-Metal): and D 1062, Test for Cleavage
Strength of Metal-to-Metal Adhesive Bonds.' Other
methods of test covering strength properties ace in
process of formulation by Committee PI4 on Adhesives.
NQTE 2-A short-time test is permissible for the
purpose of eliminating those materials that are unsuitable
or unduly affected by the reagents. The screening
test may be performed on films or suitable specimens
of the adhesive prepared according to the inanufacturer's
instructions with regard to dry time, cure, etc.
NOTE 3-Adhesives may be subjected to salt spray
(fog) testing by utilizing Method B 117.
1.2 This standard may involve hazardous
materials, operations, and equipment. This
standard does not purport to address all of the
safety problems associated with its use. It is the
responsibility of whoever uses this standard to
consult and establish appropriate safety and
health practices and determine the applicability
of regulatory limitations prior to use.
2. Applicable Documents
2.1 ASTM Standards:
B 117 Methods of Salt Spray (Fog) Testing3
D 471 Test Method for Rubber Property-Effect
of Liquids4
D 543 Test Method for Resistance of Plastics
to Chemical Reagents'
D 1151 Test Method for Effect of Moisture
and Temperature on Adhesive Bonds'
3. Apparatus
3.1 The apparatus shall consist of containers
for test specimens and a cabinet for maintaining
a temperature of 23 f 1.1"C (73.4 f 2°F). Other
suitable apparatus will be required for conducting
immersion tests above and below rwm temperature.
NOTE 4-Exercise care in the choice of materials
t to adherend and containers in that they
are with una "R-" ected by the chemicals and solvents used in
the test.
3.2 Apparatus for making strength tests is
specified in the method far the prowqy to be
measured (see Notes I and 2).
4. Rwsnts
NCYTE 5-Directions for preparations of reagents are
for approximately I-L quantities. All percentages are
by weight.
This method is under the jurisdiction of ASTM Committee
D14 on Adhesives and is the direct responsibility of Subcommittee
P 14.20 on Durability.
Cpnent edition approved Feb. 24, 1984. Published April
1984. Qngtnally published as D 896 - 46. Last previous edition
D 896 - 66 (1979)."
Annual Book of ASTM Standards, Vol 15.06.
'Annual Book of ASTM Standards, Vol03.02.
' Annual Book of ASTM Standards, Vol09.0 I.
Annual Book of ASTM Standards, Vol08.01.
160

D 896
4.1 Standard chemical reagents shall be selected
from the list given in Test Method D 543.
Standard oils and fuels shall be selected from the
list given in Test Method D 47 1.
4.2 Distilled Water-Freshly prepared distilled
water shall be used wherever water is specified
in this method.
5. Supplementary Reagents (Note 5)
5.1 Hydrocarbon Mixture No. 1:
Isooctane (2,2,4-trimethylpentane)
Benzene
Toluene
Xylene
5.2 Standard Jet Fuel No. 1:
600 mL
50 mL
200 mL
150 mL
Toluene
300 mL
Cyclohexane
600 mL
Isooctane (2,2,4-trimethylpen- 100 mL
tane)
n-Butyl disulfide
10 mL
n-Butyl mercaptan
0.125 g
equivalent to 0.005 weight % of
mercaptan sulfur)
5.3 Standard Jet Fuel No. 2:
Toluene
300 mL
Cyclohexane
600 mL
Isooctane (2,2,4-trimethylpen- 100 mL
tane)
n-Butyl disulfide
1 mL
n-Butyl mercaptan
0.010 g
(equivalent to 0.004 weight % of
mercaptan sulfur)
5.4 Silicone Fluid (Polydimethysiloxane),
having a viscosity of 200 cSt (mm2/s) at 25°C.
5.5 Engine Antifreeze (Ethylene Glycol), (inhibited).
5.6 Butyl Alcohol (Normal Butanol).
5.7 Brake Fluid.
5.8 Automotive Power Steering Fluid.
5.9 Trichloroethylene (+ 5 % Acetone).
NOTE 6-Additional reagents may be substituted for
or supplemented to those listed in Section 5 on agreement
between the purchaser and the manufacturer,
provided such reagents are within the general scope of
this method.
6. Test Specimens
6.1 The test specimens shall be identical with
those required in ASTM test methods for the
strength properties to be measured (see Notes 1
and 2), and the conditioning period before exposure
shall correspond to the conditioning period
before testing as given in the specified ASTM
test method.
6.2 Select matched specimens for control and
exposure treatments.
7. Procedure
7.1 Place each specimen in a separate container
and totally immerse in a sufficient quantity
of the reagent (Note 7) for 7 days at a temperature
of 23 f 1.1"C (73.4 f 2'F) (Note 8). Place the
specimen on edge in the container in the case of
flat specimens so that it is supported at an angle
from the bottom and side wall of the container.
Stir the reagent every 24 h by moderate manual
rotation of the container. Maintain the strength
of the chemical solutions constant. Use completely
closed containers to minimize evaporation
or any change in concentration (for example,
due to hygroscopicity). Where the reagent-specimen
combination may result in vaporizing or
outgassing, the container should be selected to
withstand the pressure resulting from the test
temperature so that the test reagent stays liquid.
NOTE 7-The volume of reagent used shall be ten
times the volume of the specimen.
NOTE 8--Selection of an alternative test temperature
and immersion time is permissible upon agreement
between the purchaser and the manufacturer. The alternative
test temperature may be selected from the
table in Test Method D 1151.
7.2 Remove the individual specimen from the
reagent. Rinse aqueous reagents off the specimen
with distilled water. Rinse off other reagents with
a suitable organic solvent. Blot the specimen dry
with a clean dry cloth or blotting paper. Determine
the strength of the specimen immediately
at a temperature of 23 2 1.1"C (73.4 2 2'F) in
accordance with the specified method (see Notes
1, 2, and 9).
7.3
I.J Using air as the contact medium, condition
the control specimens at 23 k 1.1 "C and 50
f 2 % relative humidity during the same 7 days
that the test specimens are exposed to the chemical
treatment. Determine the strength of the
control specimens, testing in accordance with the
specified method (see Notes 1 and 2) and at a
temperature of 23 2 l.l"C, and calculate the
average control strength.
7.3.1 When an alternative temperature is selected
for exposure of test specimens (see Notes
8 and 9), hold the control specimens in a closed
161

D 896
container for the 7-day period at the same temperature
as the test specimens. Return the controls
to 23 f 1.1 "C before testing.
NOTE 9-Selection of an alternative temperature for
determining the strength of the specimen is permissible
upon agreement between the purchaser and the manufacturer.
The altemative temperature shall be selected
from the table in Test Method D 1 I5 1.
8. Report
8.1 The report shall include the individual and
average strength property values of the control
specimens and the temperature at which the values
were determined.
8.2 The report shall include the following information
for each adhesive tested in all the
standard reagents and any specified supplementary
reagents:
8.2.1 Immersion time and temperature.
8.2.2 Strength property value of each specimen
and temperature at which value was determined.
8.2.3 Percentage change in average strength
resulting from the immersion test, calculated to
the nearest I % taking the average strength property
value of control test specimens as 100 %.
8.2.4 General appearance and behavior of
each specimen during and after immersion.
8.2.5 Type of specimen.
8.2.6 Trade name and type of adhesive used.
8.2.7 ASTM designation of materials and test
procedure used, and
8.2.8 Application, drying, and curing conditions
used in preparing the specimens.
The American Societyfor Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
$ not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you @el that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, Pa. 19103.
162

AMERIUW NATIONAL
L STANDARD
ASTM D 903 - 49 (Reapproved 1978)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
15 not listed in the current combined index, will appear in the next edition.
Standard Test Method for
PEEL OR STRIPPING STRENGTH OF
ADHESIVE BONDS'
This Standard is issued under the fixed designation D 903; the number immediately following the designation indicates
the year of original adoption or, in. the case of revision, the year of last revision. A number in parentheses indicates the
year of last reapproval.
This method has been approved for use by agencies of the Department of Dejense to replace method 1041.1 of Federal Test
Method Standard No. I7Sa andfor listing in the DoD Index of Specifications and Standards.
INTRODUCTION
The accuracy of the results of strength tests of adhesive bonds will depend on the
conditions under which the bonding process is carried out. Unless otherwise agreed
upon by the manufacturer and the purchaser, the bonding conditions shall be prescribed
by the manufacturer of the adhesive. In order to ensure that complete information
is available to the individual conducting the tests, the manufacturer of
the adhesive shall furnish numerical values and other specific information for each
of the following variables:
(I) Procedure for preparation of surfaces prior to application of the adhesive,
including the moisture content of wood, the cleaning and drying of metal surfaces,
and special surface treatments such as sanding which are not specifically limited by
the pertinent test method.
(2) Complete mixing directions for the adhesive.
(3) Conditions for application of the adhesive including the rate of spread or
thickness of film, number of coats to be applied, whether to be applied to one or
both surfaces, and the conditions of drying where more than one coat is required.
(4) Assembly conditions before application of pressure, including the room temperature,
length of time, and whether open or closed assembly is to be used.
(5) Curing conditions, 'including the amount of pressure to be applied, the length
of time under pressure and the temperature of the assembly when under pressure.
It should be stated whether this temperature is that of the glue line, or of the atmosphere
at which the assembly is to be maintained.
(6) Conditioning procedure before testing, unless a standard procedure is specified,
including the length of time, temperature, and relative humidity.
A range may be prescribed for any variable by the manufacturer of the adhesive
if it can be assumed by the test operator that any arbitrarily chosen value within
such a range or any combination of such values for several variables will be acceptable
to both the manufacturer and the purchaser of the adhesive.
1. Scope
2. Description of Terms
1.1 This method covers the determination 2.1 Peel or Stripping Strength-The
of the comparative peel or stripping characteristics
of adhesive bonds when tested on
standard sized specimens and under defined
mittee D-14 on Adhesives.
conditions Of pretreatment, temperature, and
Current edition effective %Dt.
testing machine speed. issued 1946. Replaces D 903 - 46 t.
163
' This method is under the jurisdiction of ASTM Corn-
30. 1949. Orieinallv
1 -

D 903
average load per unit width of bond line required
to separate progressively one member
from the other over the adhered surfaces at
a separation angle of approximately 180 deg
and at a separation rate of 152 mm (6 in.)/
min. It is expressed in kilograms per millimeter
(pounds per inch) of width.
2.2 Flexible-The designation “flexible”
in this test indicates a material of the proper
flexural strength and thickness to permit a
turn back at an approximate 180-deg angle in
the expected loading range of the test without
failure. In order to fulfill all terms of the definition,
at least one of the adhered materials
must be flexible.
3. Apparatus
3.1 Testing Machine-A power-driven
machine, with a constant rate-of-jaw separation
or of the inclina’tion balance or pendulum
type, which shall fulfill the following
requirements:
3.1.1 The applied tension as measured and
recorded shall be accurate within &l percent.
3.1.2 Specimens shall be held in the testing
machine by grips which clamp firmly and
prevent slipping at all times.
3.1.3 The rate of travel of the power-actuated
grip shall be 305 mm (12 in.)/min. This
rate which provides a separation of 152 mm
(6 in.)/min shall be uniform throughout the
tests.
3.1.4 The machine shall be operated without
any device for maintaining maximum load
indication. In pendulum-type machines, the
weight lever shall swing as a free pendulum
without engagement of pawls.
3.1.5 The machine shall be autographic
giving a chart having the inches of separation
as one axis and applied tension as the other
axis of coordinates.
3.1.6 The machine shall be of such capacity
that the maximum applied tension during
test shall not exceed 85 percent nor be less
than 15 percent of the rated capacity.
3.2 Conditioning Room or Desiccators-
A conditioning room capable of maintaining
a relative humidity of 50 f 2 percent at
23 * IC (73.4 * 2 F), or desiccators filled
with a saturated salt solution (Note 1) to give
a relative humidity of 50 f 2 percent at
23 + 1 C are required for the conditioning
of some specimens.
NOTE 1-A saturated salt solution of calcium
nitrate will give approximately 5 1 percent relative
humidity at the testing temperature.
4. Test Specimen
4.1 The test specimen, shown in Fig. I(a),
shall consist of one piece of flexible material,
25 by 304.8 mm (1 by 12 in.), bonded for 152.4
mm (6 in.) at one end to one piece of flexible
or rigid material, 25 by 203.2 mm (I by 8 in.),
with the unbonded portions of each member
being face to face.
4.2 In order to maintain a separation rate
of 152.4 mm (6 in.)/min the specimen shall
be relatively nonextensible in the expected
loading range. Where a material is sufficiently
extensible to lessen radically the separation
rate, it shall be backed up with a suitable
nonextensible material. In reporting such a
test, the backing material and method shall
be completely identified.
4.3 Test materials shall be thick enough
to withstand the expected tensile pull but
not over 3 mm in.) in thickness. Wherever
possible, the standard thickness of
specimens shall be: metals, 1.6 mm (‘/M in.),
plastics, 1/16 in., woods, ‘/a in., rubber compounds,
1.9 mm (0.075 in.), and cotton duck,
627.4 gm/m2 (30 oz/yd2). Other special materials,
as well as the standard materials, shall
be completely identified in the test report as
specified in Section 9.
4.4 At least ten test specimens shall be
tested for each adhesive.
4.5 Any specimen whose test result is out
of line due to some obvious flaw shall be discarded
and retest made.
5. Preparation of Test Specimen
4.1 5 1 P.w J nr~cenditi~ning
y.’
cx s-ecia! y preparation
of the areas to be bonded shall be done
in accordance with the recommendations of
the manufacturer of the adhesive.
5.2 All bonding shall be done in accordance
with the procedure and recommendations as
outlined by the manufacturer of the adhesive.
5.3 While individual specimens may be
prepared, it is recommended that specimens
be cut from bonded panels approximately
152.4 mm (6 in.) in width as shown in Fig.
I@), so that five standard 25-mm (I-in.) wide
164

specimens may be obtained from each panel.
6. Conditioning
6.1 Condition all specimens for 7 days by
exposure to a relative humidity of 50 f 2
percent at 23 f 1 C (73.4 f 2 F) or until
equilibrium is reached, except where the adhesive
manufacturer may specify such an
aging period to be unnecessary or a shorter
period to be adequate.
6.2 Special conditioning procedures may be
used by agreement between the purchaser and
the manufacturer.
7. Procedure
7.1 Conduct the test as soon as possible
after removing the test specimens from the
conditoning atmosphere and preferably under
the same conditions.
7.2 Separate the free end of the 25-mm
(l-in.) wide flexible member by hand from the
other member for a distance of about 1 in.
Place the specimen in the testing machine by
clamping the free end of the 8-in. long member
in one grip, turning back the free end of
the flexible member and clamping it in the
other grip as shown in Fig. 2. Attach the separated
end of the specimen, with all separate
parts except the one under test securely
gripped, to the recording head by means of a
clamp using care to adjust it symmetrically in
order that the tension is distributed uniformly.
Maintain the specimen during the test approximately
in the plane of the clamps. This
may be done either by attaching the minimum
weight required to the free end of the specimen
or by holding the specimen against an
alignment plate (Fig. 2) attached to the stationary
clamp. In either case, take into account
the added weight in determining the
load causing separation. Grip the I-in. wide
flexible mefiber symmetrically 2nd fiimly
without twisting in the power-actuated clamp.
Adjust the autographic mechanism and chart
to zero and start the machine. Strip the separating
member from the specimen approximately
at an angle of 180 deg and continue the
D 903
separation for a sufficient distance to indicate
the peel or stripping value. Peel at least one
half of the bonded area, even though a peel or
stripping value may be indicated before this
point.
8. Calculations
8.1 Determine the actual peel or stripping
strength by drawing on the autographic chart
the best average load line that will accommodate
the recorded curve. Report the load so indicated,
corrected for any tare weight which
may have been used with the specimen as described
in 7.2 expressed in kilograms per millimeter
(pounds per inch) of width for separation
at 152.4 mm (6 in.)/min, as the peel or
stripping strength for the particular specimen
under test.
8.2 For each series of tests, calculate the
arithmetic mean of all the values obtained and
report as the “average value.”
9. Report
9.1 The report shall include the following:
9. I . I Complete identification of the adhesive
and specimen tested, including types,
source, manufacturer’s code numbers, form,
etc.,
9. I .2 Method of preparing test specimens,
9.1.3 Conditioning procedure used,
9.1.4 Testing room conditions,
9.1.5 Number of specimens tested,
9. I .6 Speed of testing,
9.1.7 Average value of peel or stripping
strength,
9.1.8 Maximum and minimum strength
values of the series,
9.1.9 Individual rest values, individual
autographic charts, and other statistical data
requested by the purchaser, and
9. I . IO Type of failure; whether in adhesion,
cohesion in the adhesive or in the material
being bonded.
NOT^ 2 Cohesive or adhesive failure may be
determined by observation. A cohesive failure is
one which has occurred in the adhesive or specimen
material itself. Adhesive failure refers to the lack of
adherence to the materials being bonded.
165

------
ir-*-
I
I
I
Original I
Panel 4 ~),, -
I
I.
Flexible
Member
/
- 1
Bond k~ I
Line
-----
a) Test Specimen. (b) Specimens from Bonded Panel.
Metric Equivalen ts
in. I 2 6 I2
ni m 25 51 152.4 305
i I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
1
FIG. 2
Specimen Under Test.
FIG. I
Test Specimen.
The American Society for Testin and Materials takes no position res ecting the validity of an atent rights asserted in
connection with any item mentionetin this standard. Users of this standrd are expresslv advisedYtRat determination of the
validity of any such patent rights, and the risk of infringement of such rights, is enlirels their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five
years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or
for additional standards and should be addrkssed to A STM Headquarters. Your comments will receive careful consideration
at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received
a fair hearing you should make your views known to the ASTM Committee on Standards, I916 Race SI., Philadelphia, Pa.
19103, which will schedule a further hearing regarding your comments. Failing satisfaction there, you may appeal to the
ASTM Board of Directors.
166

Designation: D 904 - 57 (Reapproved 1981)"
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Practice for
EXPOSURE OF ADHESIVE SPECIMENS TO ARTIFICIAL
(CARBON-ARC TYPE) AND NATURAL LIGHT'
This standard is issued under the fixed designation D 904; the number immediately following the designation indicates the year of
original adoption or, in the case of revision. the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (6) indicates an editorial change since the last revision or reapproval.
NOTE-section 2 was added editoriallv and subseauent sections renumbered in Mdrch 1985.
1. Scope
1.1 This practice defines conditions for the
exposure of adhesives in the form of glued transparent
or translucent assemblies to ( I ) artificial
and (2) natural light sources. Where such information
is of value, the same exposure conditions
may be used on adhesive film or any other suitable
form in which light may be a deteriorating
factor.
1.2 This practice is limited to the method of
obtaining the exposure conditions and procedure
to be followed, but does not cover methods of
test to be used in evaluating the effects of the
exposure.
2. Applicable Documents
2.1 ASTM Standards:
D749 Method for Calibrating a Light Source
Used For Accelerating the Deterioration of
Rubbe9
D879 Test Method for Tensile Properties of
Adhesive Bonds3
D903 Test Method for Peel or Stripping
Strength of Adhesive Bonds3
3. Apparatus
3.1 Artijkial Light Exposure Unit (Note 1)-
The exposure unit4 shall consist of a carbon-arc
light source and suitable specimen supports, with
means being provided for measuring and controlling
the current-voltage of the light source,
temperature of the air surrounding the specimens,
and exposure cycle.
NOTE 1 -Follow
recommendations.
equipment manufacturer's safety
3.1 Light Source (Note 1 )-A carbon-arc with
suitable transparent globe or window.
3.1.2 Specimen Supports-Supports shall be
provided for mounting the specimens vertically
and in such a manner that uniform distribution
of light is obtained at the specimen. The specimens
shall be rotated around the arc to ensure
further uniform distribution of light. If the specimens
are mounted both above and below the
horizontal center line of the light source, they
may be mounted at an angle with the vertical not
greater than 30" so that the light from the arc has
a normal incidence upon the specimens. Specimens
above and below the horizontal line shall
be transposed periodically to provide uniform
distribution of the light over the face of the
specimens.
3.1.3 Thermometer-A suitable shielded thermometer
for determining the temperature of the
air at the position of the specimen in the drum.
3.2 Natural Sunlight Exposure Rack-The
I This practice is under the jurisdiction of ASTM Committee
D-14 on Adhesives and is the direct responsibility of Subcommittee
D14.20 on Durability.
Current edition approved Sept. 30. 1957. Published November
1957. Originally published as D904 -46. Last previous
edition D 904 - 55 T.
Discontinued. see 1975 Annual Book of.4STM Standards.
Part 37.
' Annual Book of ASTM Standards. Vol 15.06.
' Units that successfully fulfill all requirements of this method
are the Atlas Single and Twin Arc Apparatus (Alternating or
Direct Current), Atlas FadeOmeter. and the National Carbon
Apparatus.
167

D 904
rack shall consist of any suitable framework on
which the test specimens may be fastened at an
angle of 45" facing south. The specimens shall be
protected from direct contact with other weathering
elements and foreign matter by means of a
transparent shield' which will allow transmission
of normal solar radiation, but no attempt shall
be made to control temperature or relative humidity
surrounding the specimens. The roof of a
building is a satisfactory location for an exposure
rack.
4. Test Specimens
4. I Test specimens shall be prepared and aged
prior to test in accordance with the recommendations
of the manufacturer for use of the adhesive.
These specimens shall be of a suitable form
and number to meet the requirements of the
investigation and shall conform in detail with the
requirements prescribed in Test Method D 897,
Test Method D903, or any other ASTM test
method pertaining to strength properties of adhesives
for the desired strength test or with other
established test methods such as for light transmission,
haze, etc. Where visual inspection or
arbitrary evaluation is resorted to, the specimens
may be of any designated shape and size or in
the form of a film.
5. Test Method
5. I Artificial Light:
5. I. 1 Firmly fasten the test specimens in their
holders and then expose to the carbon-arc light
source. Also provide check specimens, shielded
from the light source, to determine any degradation
resulting from temperature and humidity
effects rather than radiation alone. Maintain the
temperature of the air surrounding the specimens
between 35 and 50°C as measured by the shielded
thermometer. Recommended exposure time
shall he !@ h or a mu!tip!e of !!I h unless a
significant change can be expected in a shorter
time. Exposure period may be repeated as often
as desired. Operate the units at all times under
the following conditions:
5.1.1.1 Atlas Single and Twin Arc Apparatus
(Alternating Current )-The average for each
trim or burning period shall be 135 V f 2 % and
I6 A f 2 % at the arc. During the burning period,
the voltage may vary between 125 and 145 V
and the amperage between 15 and 18 A.
5.1.1.2 Atlas Single and Twin Arc Apparatus
(Direct Current)-The average for each trim or
burning period shall be 135 V f 2 % and 12 A
f 2 % at the arc. During the burning period, the
voltage may vary between 130 and 145 V and
the amperage between 11 and 13 A.
5. I. 1.3 Atlas FadeOmeter-Same as prescribed
in 5.1.1.1 and 5.1.1.2.
5.1.1.4 National Apparatus-The average for
each trim or burning period shall be 50 V f 2 %
and 60 A f 2 % at the arc.
5.1.2 Replace filters (globes and windows)
after 2000 h of use, or when pronounced discoloration
or milkiness develops, whichever occurs
first (Note 2). Clean filters each day by washing
with detergent and water.
NOTE 2-The use of Method D 749, is suggested for
checking the uniformity of operation of the light source.
5.2 Natural Light-Attach the specimens to
the 45" angle rack and place the transparent
shield in position. Provide check specimens
shielded from the sun to determine any degradation
resulting from temperature and humidity
effects rather than radiation alone. Examine sgecimens
at 2-week intervals and conduct final evaluation
or testing at a predetermined time. A
suitable exposure period is 1 year, although it
may be shorter or longer as agreed upon by the
manufacturer and the purchaser. Clean and inspect
the transparent shield at least once every 2
weeks and replace at the first sign of discoloration
or milkiness.
6. Report
6.1 The report shall include the following:
6. I. I Complete identification of the adhesives
and specimen materials used.
6. I .2 Method of preparation of specimens, including
thickness of glue line or film.
6.1.3 Type and duration of exposure to light
including a complete description of the exposure
unit used for artificial light, and the geographical
location, dates of the exposure period, and general
climatic conditions for natural light.
6.1.4 Description of any visual changes in appearance
that may have occurred during each
exposure period for both the test and check spec-
s Pyrex glass. 9200 PX, has been found satisfactory for the
shield.
168

imens.
6.1.5 Results of any physical, chemical or
other tests made to determine the extent of deg-
radation resulting from the exposure. This shall
also include tests on the check specimens. The
test methods used shall be adequately described.
The American Societyji)r Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users qfthis standard are expre.ss1.v advised that determination qf the validity of any such
patent rights, and the risk of infringement qf such rights, are entirelv their own re~sponsibility.
This slundurd is subject to revision at any time by the responsible technical commitlee and must be reviewed every,five years and
If not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or ,for additional
.standards and should be addre.ssed to ASTM Headquarters. Your comments will receive careful consideration at a meeting cfthe
responsible technical committee, which you may attend. If you .fie1 that your comments have not received a ,fair hearing you should
makevour views known to fhe ASTM Committee on Standards. 1916 Race Sf., Philadelphia, PA 19103.
169

ab
Designation: D 950 - 82 (Reapproved 1987)"
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition
Standard Test Method for
IMPACT STRENGTH OF ADHESIVE BONDS'
This standard is issued under the fixed designation D 950 the number immediately following the designation indicates the
year of original adoption or, in the case of revision. the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This method has been approved for use by agencies of the Department of Defense to replace methods 1033 and 1033.1 T of Federal
Test Method Standard No. 17Sa and for listing in the DoD Index of Specifications and Standards.
'I NmE-Sections 3 and 4 were editorially transposed in October 1986.
INTRODUCTION
The accuracy of the results of strength tests of adhesive bonds will depend on the
conditions under which the bonding process is carried out. Unless otherwise agreed
upon between the manufacturer and the purchaser, the bonding conditions shall be
prescribed by the manufacturer of the adhesive. In order to ensure that complete
information is available to the individual conducting the tests, the manufacturer of the
adhesive shall furnish numerical values and other specific information for each of the
following variables:
(I) Procedure for preparation of surfaces prior to application of the adhesive,
including the moisture content of wood, the cleaning and drying of metal surfaces, and
special surface treatments such as sanding which are not specifically limited by the
pertinent test method.
(2) Complete mixing directions for the adhesive.
(3) Conditions for application of the adhesive including the rate of spread or thickness
of film, number of coats to be applied, whether to be applied to one or both surfaces,
and the conditions of drying where more than one coat is required.
(4) Assembly conditions before application of pressure, including the room temperature,
length of time, and whether open or closed assembly is to be used.
(5) Curing conditions, including the amount of pressure to be applied, the length of
time under pressure and the temperature of the assembly when under pressure. It should
be stated whether this temperature is that of the glue line, or of the atmosphere at which
the assembly is to be maintained.
(6) Conditioning procedure before testing, unless a standard procedure is specified,
including the length of time, temperature, and relative humidity.
A range may be prescribed for any variable by the manufacturer of the adhesive if it
can be assumed by the test operator that any arbitrarily chosen value within such a
range or any combination of such values for several variables will be acceptable to both
the manufacturer and the purchaser of the adhesive.
1. scope
1.1 This test method coven the determination
of the comparative impact value of adhesive
does not purport to address all of the safety prob-
[ems associated with its use. It is the responsibility
Of the User Of this standard to establish appro-
bonds in when tested On standard 'peCi-
I This test method is the juridiction of ASTM Cornmens
under specified conditions of preparation, mitt= D-14 on Adhesives and is the dim responsibility of
conditioning, and testing.
Subcommittee D14.30 on Wood Adhesives.
Current edition approved Nov. 26, 1982. Published January
This standard may hazardous ma- 1983. Originally published D 950 - 52 T. Last pmrious editerials,
operations, and equipment. This standard tion D 950 - 78.
170

D 950
priute sufety and health practices and determine
the upplicability of regulatory limitations prior to
use.
2. Referenced Documents
2. I ASTM Standards:
A 108 Specification for Steel Bars, Carbon,
Cold-Finished, Standard Quality2
B 16 Specification for Free-Cutting Brass
Rod, Bar, and Shapes for Use on Screw
Machines"
B 107 Specification for Magnesium-Alloy
Extruded Bars, Rods, Shapes, Tubes, and
Wire4
B 133 Specification for Copper Rod, Bar,
and Shapes3
B 139 Specification for Phosphor Bronze
Rod, Bar, and Shapes:'
B 15 1 Specification for Copper-Nickel-Zinc
Alloy (Nickel Silver) and Copper-Nickel
Rod and Bar3
B 2 1 I Specification for Aluminum-Alloy
Bars, Rods, and Wire"
D 143 Methods of Testing Small Clear Specimens
of Timber5
D 905 Test Method for Strength Properties of
Adhesive Bonds in Shear by Compression
Loading6
E 23 Methods for Notched Bar Impact Testing
of Metallic Materials7
3. Description of Term Specific to This Standard
3.1 impuct vaalue-the energy absorbed by a
specimen of standard design when sheared by a
single blow of a testing machine hammer. Impact
value is expressed in joules per square metre or
foot-pounds-force per square inch.
4. Significance and Use
4. I Adhesives can fail under a sudden impact
load and not under a slowly applied load of the
same or greater force.
4.2 This test method can be used to compare
the sensitivity of various adhesives to suddenly
applied loads.
5. Apparatus
5.1 Testing Machine:
5.1.1 A pendulum-type impact machine with
a hand velocity of 3.4 m/s (1 1 Ws), comprising
essentially the following:
5.1.1.1 Impact Head equipped with a flat
striking face slightly wider than the test speci-
men, aligned to strike the specimen full-face.
5.1.1.2 Jig to hold the test specimen, as
shown in Fig. 1. The jig illustrated is not suitable
for use with all impact machines and vises.
Dimensions and design of the jig may be varied
as required for adaptation to machines and
vises available, provided the following general
requirements are met: It is necessary that the
jig be machined from a solid piece of steel and
be solidly bolted to the base of the testing
machine. Corners shall be drilled to ensure that
the test specimen sets flush against the retaining
end of the jig; the drilled corners are required
to minimize dirt collection at the corners which
could hold the end of the specimen away from
the face of the jig. The jig shall be provided
with a screw to tighten the specimen in the jig,
to minimize the tendency of the specimen to
overturn when struck. To prevent the holding
screw from splitting specimens of wood, a metal
plate shall be placed between the end of the
wood block and the end of the screw. The jig
shall be so located that the specimen will be
struck at the point of maximum head velocity.
5.1. I .3 Vise or Bolts to hold the jig rigid and
immobile under the stress of the testing machine
hammer. The total height of the vise, jig,
and test specimen shall be such that the lower
edge of the striking face of the impact head
strikes the specimen as near the adhesive line
as possible, preferably within 0.79 mm ('h in.).
Ordinarily the distance between the top of the
jaws of the vise of the machine and the bottom
of the striking face of the head is 22 mm (0.866
in.), and proper height of the specimen may be
obtained by adjusting its height in the jig.
5.1.2 Additional information on impact testing
machines and their calibration may be
found in Methods E 23.
5.2 Conditioning Room or Desiccators---A
conditioning room capable of maintaining a
relative humidity of 50 k 2 % at 23 -L 1.1 "C
(73.4 A 2"F), or desiccators fiiied with a saturated
salt solution (Note 1) to give a relative
humidity of 50 k 2 % at 23 k 1.1"C (73.4 f
2°F).
NOIL 1- A saturated salt solution of calcium nitrate
will give approximately 51 % relative humidity
at the test temperature.
Annual Book ofASTM Siandards, Vol 0 I .05.
'Annual Book (4 ASTM Siandards, Vol02.0 I.
'Annual Book ifASTM Standards. Vol02.02.
'Annual Book of ASTM Standards, Vol04.09.
.4nnual Book of ASTM Standards, Vol 15.06.
' Annual Book of ASTM Standards, Vol03.01.
17 1

D 950
6. Test Specimens
6.1 The test specimen for metal-to-metal adhesives
shall conform to the dimensions given
in Fig. 2(a), whenever possible. In cases where
this specimen cannot be fractured in the testing
machine available, the square dimensions of
the 25.4 by 25.4-mm (1 by 1-in.) block may be
reduced to a smaller square, keeping the dimensions
of the 25.4 by 445" (1 by l%-in.)
block constant. The dimensions of the specimen
and bonded area shall be clearly stated in
the report (Section 12). In any case, it is desirable
that the specimen size be such as to give
impact strengths that fall somewhere near the
middle range of the testing machine, since readings
in the highest and lowest ranges are often
unreliable. The specimen shall be assembled so
the face receiving the impact load is at the point
of maximum velocity of the impact head. The
impact face of the specimen shall be square and
flat, perpendicular to the plane of the glue line,
and parallel to the striking face of the pendulum.
Metals conforming to the following specifications
are recommended:
Metal
Designation
Brass
ASTM B 16. C36000 half-hard tem-
Per
Copper
ASTM B 133, C I IOOO, hard temper
Aluminum ASTM B 21 I, A92024: G-3
Steel
AIS1 1020, G 10200; cold-finished bar
Phosphor bronze ASTM B 139, C54400
Magnesium ASTM B 107, AZ61A or MIA-F
Nickel silver ASTM B 151, C77000, quarter-hard
Tests on adhesives with high impact strength
preferably should be run on steel to minimize
deformation. Specimens may be re-used after
testing, provided that the face receiving the
impact is not deformed.
6.2 Test specimens for wood-to-wood adhesives
shall conform to the dimensions shown in
Fig. 2 (b). The specimens may be prepared by
gluing blocks 9.5 mm (3/e in.) thick by 1 in. wide,
of convenient length, to blocks 19 mm (% in.)
thick by 44.4 mm ( 13/4 in.) wide, of the same
convenient length, where the 25.4-mm ( 1-in.)
and 1 3/4-in. dimensions, respectively, are those in
the direction of the grain. Specimens, each 1 in.
in width, may then be cut from the glued assembly
by cutting across the long dimension, in the
grain direction. Hard maple (mer saccharrum or
acer Nigrum), having a minimum specific gravity
of 0.65 based on oven-dry weight and volume,
shall be selected (Note 2). These blocks shall be
of straight grain and free from defects, including
knots, birdseye, short grain, decay, and any unusual
discolorations within the test area. The
blocks shall be at the equilibrium moisture content
recommended by the manufacturer of the
adhesive. In the absence of such recommendation,
the moisture content shall be from 10 to
12 %, based on oven-dry weight as determined
on representative samples in accordance with
Sections 124 to 127 of Methods D 143. Just prior
to gluing, the blocks shall be surfaced, preferably
with a hand-feed jointer and then weighed and
assembled in pairs so that blocks of approximately
the same specific gravity are glued together.
The surfaces sMl remain msanded and
shall be free from dirt. Blocks shall be glued as
described in Section 7, after which test specimens
conforming to Fig. 2 (b) shall be prepared.
NOTE 2-A method of selecting maple blocks of
satisfactory specific gravity is described in the Appendix
of Test Method D905. For referee tests, the specific
gravity of blocks may be determined in accordance with
Sections I16 and I17 of Method D 143.
7. Gluing
7.1 Gluing shall be done in accordance with
the procedure outlined by the manufacturer of
the adhesive.
7.1.1 For metal-to-metal specimens, preparation
of areas that are to be cemented shall be
in accordance with the recommendationsof the
manufacturer of the adhesive.
7.1.2 For wood-to-wood specimens, the
grain of the wood shall be parallel in the two
pieces and parallel to the glue line as shown in
Fig. 2 (6). If, due to circumstances, wood with
a slight taper in the grain must be used, the
pieces shall be assembled so the grain runs
toward the glue line toward the back of the
specimen. Thus, failures that start in the wood
will be directed toward the glue line. Excess
glue at the impact face should be removed
carefuuliy to ensure proper striking of the impact
head. Also squeeze-out should be removed
when necessary to ensure proper positioning of
the specimen in the jig.
8. Conditioning
8.1 Preconditioning is not required for
metal-to-metal bonds. The adhesive is ready
for test purposes when it has been applied in
accordance with Section 7, unless otherwise
specified by the manufacturer or the purchaser.
172

D 950
8.2 All wood specimens shall be conditioned
at a humidity of50 f 2 %, and at a temperature
of 23 f 1.1OC (73.4 f 2"F), either for a period
of 7 days or until specimens reach equilibrium
as indicated by no progressive changes in
weight, whichever is the shorter period.
8.3 Special conditioning procedures may be
used by agreement between the manufacturer
and the purchaser.
9. Number of Test Specimens
9.1 At least ten test specimens shall be tested
for each adhesive in the case of metal-to-metal
specimens.
9.2 At least 20 specimens shall be tested,
representing at least four different joints, in the
case of wood-to-wood adhesives.
9.3 Specimens that break at some obviously
fortuitous flaw remote from the glue line shall
be discarded and retests made, unless such
flaws constitute a variable the effect of which
it is desired to study.
10. Procedure
10.1 Test in an atmosphere such that the
moisture content of the wood specimens developed
under the conditions prescribed in 8.2 is
not noticeably altered during testing, and test
as soon as possible after the conditioningperiod
prescribed in 8.2.
10.2 Place the specimen in the jig in the vise
of the impact machine so that the specimen
butts squarely against the retaining end of the
jig. Rest the impact head of the machine gently
against the specimen and adjust the jig so that
the head fits squarely against the impact face
of the specimen.
10.3 Raise the impact head to a predetermined
height and release the safety catch. The
impact energy absorbed by the specimen may
then be read directly.
10.4 Record the foilowing information:
10.4.1 Record joules or foot-pounds-force of
energy absorbed in producing failure of the
specimen.
10.4.2 Record bonded area of specimen.
10.4.3 In case of metal-to-metal adhesives,
record the percentages of cohesion, adhesion,
and contact failures (Note 3). This will be based
on visual inspection.
10.4.4 In case of wood-to-wood adhesives,
record the percentages of wood, glue, and con-
tact failures. This will be based on visual inspection.
NOTE 3-Cohesion failure may be obtained by
observing how much of the failure has occurred in
the adhesive itself. That is, if the cement has adhered
to the metal test pieces and no voids are visible, it
represents a 100 % cohesion failure. Adhesion failure
refers to the lack of adhering to metals being fastened.
Contact failure refers to lack of glue lines being in
contact due to uneven surfaces, poor pressure distribution,
etc.
11. Calculation
1 1. I Calculate the impact value of the specimen
as the energy absorbed in producing failure
of the specimen divided by the bonded area
of the specimen, and express in joules per
square metre or foot-pounds-force per square
inch. Report the values to the nearest 100 J/m2
(0.1 ft..lbf/in.'). Unit results cannot be extended
to different areas than those tested.
12. Report
12.1 The report shall include the following:
12.1.1 Complete identification of the adhesive
tested, including type, source, manufacturer's
code numbers, form, etc.,
12.1.2 Method of preparing test specimens,
dimensions of specimens, and materials
bonded,
12.1.3 Average thickness of adhesive layer
after formation of the joint, within 0.03 mm
(0.001 in.). The method of obtaining the thickness
of the adhesive layer shall be described
including procedure, location of measurements,
and range of measurements.
12.1.4 Conditioning procedure used,
12.1.5 Atmosphere conditions in test room,
12.1.6 Number of specimens tested,
12.1.7 Actual bonded area, and
12.1.8 Maximum, minimum, and average
value of impact strength, with an average value
of the percentages of wood, glue, and contact
failures for !he wood specimens, or cohesion,
adhesion, and contact failures for the metal
specimens.
13. Precision and Bias
13.1 At the present time there is no basis for
a statement of precision or bias concerning the
reproducibility of results among laboratories.
Such information may be available in the future
following round-robin testing among laboratories.
173

4$lb
D950
13.2 The precision and bias of the test is a the wood's variability. Precision shall be reported
function of the properties of the cured bondline; in terms of the standard deviation of the data
and if wood failure occurs, they are a function of and the standard error of the mean.
IMPACT
....................
....................
....................
'--TESTING
MACHINE
Metric Equivalents
I
ALL SURFACES "O'* FINISH OR BETTER
MATERIAL: S.A.E. 1020 SOFT ROLLED
NO. REO: ON€
-- 3i
STEEL OR
EQUAL
.. ...
1
pit + I----
L~ORILL-C'BORE ?jp, DIA x 3 DEEP-4HOLES
in. mm in. mm
. -. . . . ___
L/x 3.2 1.005 + 0.005 25.527 + 0.127
:YU 9.5 -O.m -0.OOO
% 12.7 1 Y2 38. I
'K2 14.9 I .800 + 0.005
45.720 + 0.127
K 16 -0.OoO -0.OOO
R 19 2 50.8
I 25.4 2% 52.8
3 Y2 88.9
5 %2 131
FIG. I
Adapter Jig for Impact Machines
174

4m 0950
Adhesive Bond
L 13,i-----l
(a) Metal-to-Metal Specimen
Adhesive Bond
-
'LI 3; -A
Directicn of Grain
(b) Wood-to-Wood Specimen
Metric Equivalents
in. YH Y4 I I :%
mm 9.5 19 25.4 44.4
FIG. 2 Block Shear Impact Test Specimens
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquariers. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. uyoufiel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.
175

Designation: D 1002 - 72 (Reapproved 1983)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition
Standard Test Method for
STRENGTH PROPERTIES OF ADHESIVES IN SHEAR BY
TENSION LOADING (METAL-TO-METAL)'
This standard is issued under the fixed designation D 1002; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This method has been approved for use by agencies of the Department of Defense to replace methods I032 and 1032.IT of Federal
Test Method Standard No. I7Sa and for listing in the DoD Index of Specifcations and Standards.
The accuracy of the results of strength tests of adhesive bonds will depend on the
conditions under which the bonding process is camed out. Unless otherwise agreed upon
by the manufacturer and the purchaser, the bonding conditions shall be prescribed by the
manufacturer of the adhesive. In order to ensure that complete information is available to
the individual conducting the tests, the manufacturer of the adhesive shall furnish numerical
values and other specific information for each of the following variables:
(1) Procedure for preparation of surfaces prior to application of the adhesive, the cleaning
and drying of metal surfaces, and special surface treatments such as sanding that are not
specifically limited by the pertinent test method.
(2) Complete mixing directions for the adhesive.
(3) Conditions for application of the adhesive, including the rate of spread or thickness
of film, number of coats to be applied, whether to be applied to one or both surfaces, and
the conditions of drying where more than one coat is required.
(4) Assembly conditions before application of pressure, including the room temperature,
relative humidity, length of time, and whether open or closed assembly is to be used.
(5) Curing conditions, including the amount of pressure to be applied, the length of time
under pressure, method of applying pressure (pressure bag, press platens, etc.), heat-up rate,
and the temperature of the assembly when under pressure. It should be stated whether this
temperature is that of the bondline or of the atmosphere at which the assembly is to be
maintained.
(6) Conditioning procedure before testing, unless a standard procedure is specified,
including the length of time, temperature, and relative humidity.
A range may be prescribed for any variable by the manufacturer of the adhesive if it can
be assumed by the test operator that any arbitrarily chosen value within such a range or
any combination of such values for several variables will be acceptable to both the
manufacturer and the purchaser of the adhesive.
1. Scope does not purport to address all of the safety prob-
1.1 This test method covers the determination lems associated with its use. It is the responsibilof
the comparative shear strengths of adhesives ity of whoever uses this standard to consult and
~-
for bonding metals when tested On a standard
I This test method is under the jurisdiction of ASTM Cornspecimen
and under specified conditions ofprep- mittee D-14 on Adhesives and is the direct resmnsibilitv of
aration and test.
Subcommittee D14.80 on Metal Bonding Adhesives.
Current edition approved July 28, 1972. Published October
This standard may hazardous ma-
1972. Originally publish& as D 1002 - 49 T. Last previous
terials, operations,'and equipment. This standard edition D 1002 - 64 (1970).
176

D 1002
establish appropriate safety and health practices
and determine the applicability of regulatory limitations
prior to use.
2. Apparatus
2.1 The testing machine shall conform to the
requirements of ASTM Methods E4, Verification
of Testing Machines.* The testing machine
shall be so selected that the breaking load of the
specimens falls between 15 and 85 percent of the
full-scale capacity. The machine shall be capable
of maintaining a rate of loading of 80 to 100 kg/
cm2 (1 200 to 1400 psi)/min, or, if the rate is
dependent on crosshead motion, the machine
should be set to approach this rate of loading. It
shall be provided with a suitable pair of selfaligning
grips to hold the specimen. It is recommended
that the jaws of these grips shall engage
the outer 25 mm (1 in.) of each end of the test
specimen firmly (Note 1). The grips and attachments
shall be so constructed that they will move
into alignment with the test specimen as soon as
the load is applied, so that the long axis of the
test specimen will coincide with the direction of
the applied pull through the center line of the
grip assembly.
NOTE 1 -The length of overlap of the specimen may
be vaned where necessary. The length of the specimen
in the jaws, however, must not be varied. The distance
from the end of the lap to the end of the jaws should
be 63 mm (2% in.) in all tests.
3. Test Specimens
3.1 Test specimens shall conform to the form
and dimensions shown in Fig. 1. These shall be
cut from test panels prepared as prescribed in
Section 4. The recommended thickness of the
sheets is 1.62 2 0.125 mm (0.064 f 0.005 in.).
The recommended length of overlap for most
metals of 1.62 mm (0.064 in.) in thickness is 12.7
2 0.25 mm (0.5 f 0.01 in.).
NOTE 2-Since it is undesirabie IO exceed the yield
point of the metal in tension during test, the permissible
length of overlap in the specimen will vary with the
thickness and type of metal, and on the general level of
strength of the adhesive being investigated. The maximum
permissible length may be computed from the
following relationship:
L = Fty tJr
where:
L = length of overlap, in.,
t = thickness of metal, in.,
Fty = yield point of metal (or the stress at pro-
portional limit), psi, and
7 = 150 percent of the estimated average shear
strength in adhesive bond, psi.
NOTE 3-A variation in thickness of the metal, and
the length of overlap, will likely influence the test values
and make direct comparison of data questionable. For
this reason, in comparative or specification tests, the
thickness should preferably be 1.62 k 0.125 mm (0.064
k 0.005 in.) and the length of overlap should preferably
be 12.7 & 0.25 mm (0.5 & 0.01 in.), or not in excess of
the value computed in Note 2. For development tests
values could be different, but should then be constant.
3.2 The following grades of metal are recommended
for the test specimens:
Metal
ASTM Designation”
BW B 36, Alloy 8
copper
B 152, Type A
Aluminum
B 209, Alloy 2024, T3 temper
Steel A 109, Grade 2
Corrosion-resisting steel A 167, Type 302
Titanium B 265
” These designations refer to the following specifications of
the American Society for Testing and Materials:
B 36, for Brass Plate, Sheet, Strip, and Rolled Bar:
B 152, for Copper Sheet, Strip, Plate, and Rolled Bar,3
B209, for Aluminum and Aluminum-Alloy Sheet and Plate4
A 109, for Cold-Rolled Carbon Steel Strip,’
A 167, for Stainless and Heat-Resisting Chromium-Nickel
Steel Plate, Sheet, and Strip,’ and
B265, for Titanium and Titanium Alloy Strip, Sheet, and
Plate6
3.3 At least 30 specimens shall be tested, representing
at least four different joints. However,
if statistical analysis of data and variance is employed,
it should be possible to reduce this number.
4. Preparation of Test Joints
4.1 It is recommended that test specimens be
made up in multipies of at least five specimens,
and then cut into individual test specimens (Note
4), Figs. 2 and 3. Cut sheets of the metals prescribed
in 3.1 and 3.2 to suitable size. All edges
of the metal panels and specimens which will be
within (or which wiIi boundj the iap joints shaii
be machined true (without burrs or bevels and at
right angles to faces) and smooth (rms 160 max)
before the panels are surface-treated and bonded.
Clean and dry the sheets carefully, according to
the procedure prescribed by the manufacturer of
the adhesive, and assemble in pairs. Prepare and
Annual Book of ASTM Standards, Vol03.0 1.
’ Annual Book of ASTM Standards, Vol02.01.
‘Annual Book of ASTM Standards, Vol02.02.
’ Annua/ Book of ASTM Standards, Vol 01.03.
Annual Book of ASTM Standardr, Vol02.04.
177

D 1002
apply the adhesive according to the recommendations
of the manufacturer of the adhesive. Ap
ply the adhesive to a sufficient length in the area
across the end of one or both metal sheets so that
the adhesive will cover a space approximately 6
mm (11’4 in.) longer than the overlap as selected in
Section 3. Assemble the sheets so that they will
be held rigidly so that the length of the overlap
will be controlled, as indicated in Section 3,
within 0.25 mm (kO.01 in.), and the adhesive
allowed to cure as prescribed by the manufacturer
of the adhesive.
NOTE 4-Bonding specimens in multiple panels is
believed to give more representative specimens. However,
individual specimens may be prepared if agreeable
to the supplier or the purchaser of the adhesive.
5. Preparation of Test Specimens
5.1 Cut the test specimens, as shown in Fig.
1, from the panels, Figs. 2 and 3. Perform the
cutting operation so as to avoid overheating or
mechanical damage to the joints (Note 5). For
final preparation trim panel area according to
Fig. 5. Measure the width of the specimen and
the length of the overlap to the nearest 0.25 mm
(0.01 in.) to determine the shear area.
NOTE 5-A five-tooth, typesetter’s circular saw has
been found suitable for such purposes.
6. Procedure
6.1 Test the specimens, prepared as prescribed
in Section 5, as soon after preparation as possible.
The manufacturer of the adhesive may, however,
prescribe a definite period of conditioning under
specific conditions before testing.
6.2 Place the specimens in the grips of the
testing machine so that the outer 25 mm (1 in.)
of each end are in contact with the jaws (Note 1)
and so that the long axis of the test specimen
coincides with the direction of applied pull
through the center iine of the grip assembiy.
Apply the loading immediately to the specimen
at the rate of 80 to 100 kg/cm2 (1200 to 1400
psi) of the shear area per min. Continue the load
to failure. This rate of loading will be approximated
by a free crosshead speed of 1.3 mm (0.05
in.)/min.
7. Calculations
7.1 Record the load at failure and the nature
and amount of this failure (cohesion in adhesive
or metal, or adhesion) for each specimen. Express
all failing loads in kilograms per square centimeter
(pounds per square inch) of shear area,
calculated to the nearest 0.06 cm2 (0.01 in.’).
8. Report
8.1 The report shall include the following information:
8.1.1 Complete identification of the adhesive
tested, including type, source, date manufactured,
manufacturers’ code numbers, form, etc.,
8.1.2 Complete identification of the metal
used, its thickness, and the method of cleaning
and preparing its surfaces prior to bonding,
8.1.3 Application and bonding conditions
used in preparing specimens,
8.1.4 Average thickness of adhesive layer after
formation of the joint within 0.001 in. The
method of obtaining the thickness of the adhesive
layer shall be described including procedure, location
of measurements, and range of measurements.
8.1.5 Length of overlap used,
8.1.6 Conditioning procedure used for speci-
mens prior to testing,
8.1.7 Number of specimens tested,
8.1.8 Number of joints represented and type
of joint if other than single overlap,
8.1.9 Maximum, minimum, and average values
for the failing load, and
8.1.10 The nature of the failure, including the
average estimated percentages of failure in the
cohesion of the adhesive, contact failure, and
adhesion to the metal.
178

'
-- I 6 mm
(0.064")
-GLUE LINE
IN-
TEST
FIG. 1
--- 127t L mm-- 1
L 177.8 t Lmm---
Form and Dimensions of Test Specimen
TEST
GRIPS
t-
-
25.4"
20.254
(1.000"
+-O.OIO 1
%I
Typical
.
177.8mm23.175
(7.0:' to. 125)
FIG. 2 Standard Test Panel
179

4.775"
t 0.127
(0.188"
f+o.oosl
igi
t0.002 - 0.0001
7.137 mm
t 0.1 27
(0.281''
31.775 mrr
20.127
-----
(1.251''
+O.OOS) J
25.4 mm
t0.254
1(1.00"-
f0.010)
FIG. 3 Optional Panel for Acceptance Tests Only
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyjive years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St.. Philadelphia, Pa. 19103.
180

ab
Designation: D 1006 - 73 (Reapproved 1986)"
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Practice for
CONDUCTING EXTERIOR EXPOSURE TESTS OF PAINTS
ON WOOD'
This standard is issued under the fixed designation D 1006; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reappmval.
A superscript epsilon (0 indicates an editorial change since the last revision or reapproval.
This practice has been approved for use by agencies of the Department of Definse to replace Method 6161.1 of Federal Test Method
Standard No. 141A and for listing in the DoD index of Spec8cations and Standards.
'I Nom-Editorial changes were made throughout in April 1986.
1. Scope
1.1 This practice deals only with the testing of
house paints and trim paints on new, previously
unpainted wood.
1.2 This practice describes a test procedure
that embodies the principles considered necessary
for reliable results. Variations necessitated
by circumstances may be introduced by agreement
provided they do not violate these principles.
One procedure embodying the principles is
described in the Annex for use by those who find
it coqvenient.
1.3 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of the user of this standard to establish appropriate
safety and health practices and determine
the applicability of regulatory limitations prior to
use.
2. Referenced Documents
2.1 ASTM Standards:
D358 Specification for Wood to Be Used As
Panels in Weathering Tests of Paint and
Varnishes2
D 1 150 Single and Multi-Panel Forms for Recording
Results of Exposure Tests of Paints2
2.2 US. Federal Standard:
TT-W-57 1 b Federal Specification for Wood-
Preservative, Recommended Treating Practice3
3. Significance and Use
3.1 The procedure described in this practice is
intended to aid in evaluating the performance of
house and trim paints applied to new, previously
unpainted wood.
3.2 Since natural environment varies with respect
to season, geography, and topography, test
results can vary in accordance with location and
may not correlate to actual in-service performance
(5.1).
4. Extent of Test Program
4.1 The extent of the exterior exposure test
program must be governed by the breadth of the
conclusions desired. The types of paints to be
tested, the range in climatic conditions to be met,
also the types of woods and structures on which
the paints are to be used are important factors to
be considered in establishing the exposure program.
5. Location of Test Stations
5.1 The climatic conditions of the test sites
should be representative of those of the area in
' This practice is under the jurisdiction of ASTM Committee
D-l on Paint and Related Coatings and Materials and is the
direct responsibility of Subcommittee W1.27 on Accelerated
Testing.
Current edition approved Oct. 29,1973. Published December
1973. Originally published as D 1006 - 51 T. Last previous edi-
tion D 1006 - 56 ( 1970).
Annual Book of ASTM Standards, Vol06.0 1.
' Available from Naval Publications and Forms Center, 5801
Tabor Ave., Philadelphia, PA 19120.
181

D 1006
which the paints are to be used. The type and
rate of failure of a paint film will vary when
exposed to different combinations of climatic
and atmospheric conditions. For reliable results,
exposure sites should be selected that are representative
geographically, climatically, and in atmospheric
contaminations with those of the locality
in which the paint will be used. To obtain
conclusions that are valid for paints with national
distribution requires exposure at several sites,
selected to cover a wide range in climatic condition~.~
6. Exposure Positions
6.1 Panels for testing house paints and trim
paints should be exposed on vertical test fences
facing both south and north. In comparisons
where dirt collection and mildew resistance are
not pertinent, north vertical exposures may be
omitted. There should be no obstructions close
enough to shade test panels from the sun more
than 2 h after sunrise, or 2 h before sunset.
6.2 In the case where it is desirable to expose
coated panels in a sheltered area, such as under
eaves, a suitable test fence with a sheltered or
eave arrangement can be used (see Annex).
7. Construction of Test Fences
7.1 Test fences should be durable and rigid
enough to remain upright under the action of
prevailing winds and frost throughout the contemplated
period of testing5
7.2 Lower edges of test panels, when mounted
on test fences, should be at least I8 in. (460 mm)
above ground level to avoid dampness and mud
splash. Backs of painted boards or plywood
should be protected against direct exposure to
the weather by methods such as, (I) having panels
on both sides of the fence, (2) mounting the
panels on sheathing, and (3) closing the opposite
side of the fence.
7.3 Fences should have watertight caps to
keep water from getting behind test panels.
8. Selection of Woods for Test Panels
8.1 Paint need be tested only on woods on
which it is likely to be used in practice. Conclusions
drawn from tests made on a limited variety
of woods, however, should not be generalized for
woods of other kinds.
NoTE-Se Specification D 358.
8.2 Prior to use, test lumber and panels should
be stored under such conditions that the moisture
content of the wood will be maintained within
the normal range for exterior woodwork in the
region in which the tests are made.
9. Construction of Test Panels
9. I For house paints, unless the pattern of the
siding requires some other choice, test panels
should be made of one or the other of two
patterns of siding, namely, ‘12 or 3/4 by 6-in. (1 3
or 20 by 150-mm) bevel siding or 1 by 6411. (25
by 150-mm) drop siding.
9.2 If the panels in the house paint test are
not subdivided, one 3-ft (900-mm) length of 6-
in. (1 50-mm) siding will be acceptable. If the
panels are subdivided, two 18411. (460-mm)
lengths are sufficient. Exposures on wood panels
should preferably be carried out on three panels
to allow for variations in the wood.
9.3 For trim paints, the test panel should carry
1 by 4411. (25 by 100-mm) pieces of trim lumber
at each end.
9.4 A test panel of I .5 ft2 (I 400 cm2) or more
in area, as provided in 9.2, may be subdivided
into two or more test areas each not less than 10
in. (250 mm) long and 0.75 ft2 (700 cm2) in area.
Each test area is for painting with a different
paint. Paints placed on the test areas of one panel
furnish a comparison as to behavior.
9.5 When it will not interfere with the properties
to be tested, all panels should be coated on
the back to prevent warping.
10. Control or Comparison Paint for Extending
the Comparisons
10.1 When several paints are to be compared,
one paint should be selected as a standard of
comparison or “control.” The control paint
should then be applied on one test area of each
:est pane!. Variations caused bj: wood differences
are revealed in the behavior of the control paint,
and can be used to adjust the ratings of the other
paints to a common basis. For best results there
should be two controls-one known to perform
well and one known to perform poorly.
‘Suggested sites include the Great Lakes region. Florida,
extreme southern Louisiana. the southwest region. and northeast
region.
Fences, such as presented by W. A. Southard in the May
I959 issue of the O[ficiul Di~cw, are acceptable.
182

D 1006
1 1. Application of Paints
1 I. 1 All tests that are to be compared closely
with one another should be placed on exposure
as nearly simultaneously as possible. When a
group of tests is too extensive for completion
within a month, use a control paint or duplicate
of at least 5 % of the test areas at successive
exposure periods.
1 1.2 It is best in theory and practice to do the
painting out-of-doors in proper weather for
painting: however, indoor painting is permissible
provided no more than 1 week6 elapses between
successive coats and between applying the last
coat and exposing on the test fence: and provided,
further, that all painting is done under
essentially the same drying conditions. It is necessary
to allow each coat to cure sufficiently
before top coating.
11.3 Preferred procedure is to apply paints
with the test panel in a vertical position and kept
vertical until the paint has set. If paint is spread
on horizontal panels, the panels should be placed
vertically immediately thereafter.
1 1.4 Records should be kept of the spreading
rates at which paints are applied. When the purpose
of the tests is to compare commercial paints,
it may be appropriate to let the painter apply
them at what seems to be their natural spreading
rates. When the purpose is to study variation in
paint composition, application should usually be
at suitable predetermined spreading rates which
can be controlled by applying a given weight or
volume of coating to a measured area.
12. Inspections and Records
12.1 After panels have been exposed to the
weather, inspections should be made after not
more than 1 month, at 3 months, and at intervals
of 3 months during the first 2 years, and every 6
months thereafter. Midwinter inspections, however,
may be omitted in northern latitudes.' Inspections
may be made more frequently if desired.
Usually the exposures should be continued
for a considerable length of time after deterioration
has reached the point at which best practice
calls for repainting.
12.2 Records should be kept on forms such as
Standard D 1150.*
Seventy-two hours is the preferred maximum.
' Inspection should be made to assure that exposed panels
are not covered by accumulated snow banks.
'These record sheets may be obtained from ASTM Headquarters
(order Adjunct No. 12-4 I 1500- I I and 12-4 I 1500-2 I )
and from the Fedcration of Societies for Coatings Technology,
1315 Walnut St., Suite 832. Philadelphia, PA 19107.
ANNEX
(Mandatory Information)
Al. CONSTRUCTION OF TEST FENCE AND TEST PANELS
A I. I The plan for test fence and panels described in
this Annex conforms to the principles set forth in this
practice. It represents only one of numerous possible
embodiments of the priiiciples recommended.
A !.2 Canstrudio:: of Test Fence:
A1.2.1 The test fence, or test rack, runs east and
west, and is constructed to hold test panels on both
sides so that there are panels facing both north and
south. There are two rows of panels, one above the
other, on each side of the fence. A 90' cap is placed
along the top of the fence, and projects approximately
1 in. (25 mm) beyond the face of the mounted panels.
The fence must be suficiently sturdy in construction
to withstand strong winds. It is mounted on wood posts
that are impregnated with creosote under pressure, in
accordance with Fed. Spec. TT-W-57 1 b.
A1.2.2 Figure Al.l shows one span or unit. The
fence can be extended to as many units as the site
permits or as are needed for the number of exposure
tests to be made. Additional fences may be built parallel
to one another, but they should be spaced far enough
apart to keep each fence from casting shadows on the
adjacent fences during all but the first 2 h after sunrise
and the !as? 2 h befQre s "e at the time ofthe winter
solstice.
A 1.2.3 When cleated panels of drop siding, which
do not have backing, are used, there shall always be a
pair of panels, one facing north and one facing south,
to give the backs mutual protection from the weather.
If for any reason there are panels on one side only of
the fence, the other side shall be covered with rooting
paper or other covering to protect the backs of the
panels.
A I .3 Construction of Test Panels:
A 1.3. I House Paints-The boards of siding are assembled
in a manner similar to house construction.
Five pieces of '/2 by 6-in. ( I3 by 150-mm) bevel siding
are nailed securely on a backing of %-in. (64" ply-
183

D 1006
wood exterior grade, as shown in Fig. A I .2. The top
board is a blank connecting board, cut to narrower
width and painted as hereinafter described. The other
four boards are test boards: they may be all of one
species or two each of two different species. The overlap
between boards should be not less than I in. (25 mm).
Cadmium- or zinc-coated nails, 1% in. (28 mm) long,
should be used and should be spaced as indicated, and
clinched on the back. The lower edge of the bottom
board is shimmed out from the plywood with a wood
shim and the bottom board projects Vi in. beyond the
shim in order to permit insertion of a panel underneath.
The top of the panel, which is a blank board precoated
with chalk-resisting exterior paint such as aluminum
paint, is cut to a width of 4% in. (I I5 mm); the cutting
makes a suitable shim for use under the bottom board.
The plywood projects '/2 in. beyond the boards at the
ends and I in. (25 mm) at the bottom; at the top the
plywood projects 2 in. (50 mm) beyond the top of the
second board and is overlapped by about 2'12 in. (65
mm) by the top blank board. Holes are bored through
the top blank board as indicated to permit positioning
ofthe panel on the fence by means of small pegs. Holes
are bored through the projecting ends of the plywood
to permit secure fastening of the panels to the fence by
means of wood clamps held in position by bolts with
wing nuts as indicated (see also Fig. A I. I).
A I .3. I. I Panels made of 6-in ( 150-mm) drop siding
should consist of four test boards 37 in. (940 mm) long,
and a narrow blank connecting board 3 in. (75 mm)
wide, fitted snugly together and held by three cleats, %
by 2 in. (16 by 50 mm) wide, nailed firmly on the
backs. By adjusting the width of the blank connecting
board the dropsiding panels can be made to fit on
fences designed as shown in Fig. A 1.1, although it may
be impracticable to mount both types of panel together
on the same fence.
A1.3.2 Trim Paints-An example of a panel for
testing trim paint is shown in Fig. A1.3. It is a modification
of the panel shown in Fig. A 1.2. The modification
consists in shortening the pieces of siding to 27 in.
(685 mm) to make room for two pieces of trim lumber,
1 by 4 in. (25 to 100 mm), at each end; and in narrowing
the exposed width of the siding to 4 in. to make room
for another piece of trim lumber, 1 by 6 in. (25 by 150
mm), across the top. This piece is undercut, as shown
in the sketch, so as to fit over the siding. The cap may
be made ofgalvanized iron, aluminum, or painted iron.
No blank connecting boards between two panels are
needed. The panel may be fastened to the fence in the
same way as the body paint panel. A much less elaborate
panel, satisfactory in many cases, is merely a plain
board, approximately 1 by 6 by 36 in. (25 by 150 by
915 mm).
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyfive years and
not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee. which you may attend. If you fie1 that your comments have not received ahir hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.
184

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37"
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-
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FLAT 'I x6' LUMBER
-
BEVELED SIDING,
5 baa
8
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NOTE-] in. = 25.4 mm.
FIG. A13 ASTM Test Panel for Exterior Exposure of Trim Mats
tSlDE VIEW
(center crosa -roction)

Designation: D 1084 - 63 (Reapproved 1981)"
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 49103
Reprinted from the Annual Book of ASW Standards, Copyright ASTM
If not listed iwthe current combined index, will appeaf in the next edition.
Standard Test Methods for
VISCOSITY OF ADHESIVES'
This standard is issued under the fixed designation D 1084: the number immediately following the designation indicates the year of
original adoption or. in the case of revision. the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
These methods have been approvedfir use by agencies of the Department of Ddense to replace method 4021 of Federal Test Method
Standard No. I75a and for listing in the DoD Index of Spec@cations and St4rds.
NmE-Section 2 was added editorially and subsequent d ons renumbered in March 1985.
1. Scope
I. 1 These test methods cover the determination
of the viscosity of free-flowing adhesives.
Four methods are covered, as follows:
1.1. I Method A is applicable only to adhesives
that will deliver 50 mL in a st&dy uninterrupted
stream from one of the cups described in Section
3.
1.1.2 Method B is intended for measuring the
viscosity of adhesives covering a range from 50
to 200 000 CP and is limited to materials that
have or approach Newtonian flow characteristics.
1.1.3 Method C is intended primarily as a
control method for determining the viscosity of
adhesives that have or approach Newtonian flow
characteristics.
1.1.4 Method D is intended primarily as a
control method for determining the viscosity of
materials which have an equivalent viscosity no
greater than approximately 3000 CP and is limited
to materials that have or approach Newtonian
flow characteristics.
NOTE 1-For adhesives that do not exhibit Newtonian
or near Newtonian flow characteristics, Test
Method D 2556, shr???ld ?x mnsidered.
2. Applicable Documents
2. I ASTM Standards:
D 88 Test Method for Saybolt Viscosity2
D 1 15 Methods of Testing Varnishes Used for
Electrical Insulation'
D 562 Test Method for Consistency of Paints
Using the Stormer Viscometer"
D 1208 Test Methods for Common Properties
of Certain Pigments'
D 1545 Test Method for Viscosity of Transparent
Liquids by Bubble Time Methods4*'
D 1601 Test Method for Dilute Solution Viscosity
of Ethylene Polymers6
D2256 Test Method for Breaking Load
(Strength) and Elongation of Yam by the
Single Strand Method'
METHOD A
3. Apparatus
3.1 The apparatus (Fig. 1) shall consist of a
set of four viscosity cups so designed as to deliver
50 mL of the sample in from 30 to 100 s at a
temperature of 23 k 0.5"C (73.4 k 0.9"F).
4. Procedure
4.1 Bring the sample to be tested and the
viscosity cup to a temperature of 23 +. OS'C
(73.4 & 0.9"F) (preferably in a constant-temperature
room). Then mount the consistency cup in
the clamp provided for the purpose and place the
receiving cylinder in position. With the outlet of
the cup closed by means of the finger, pour the
sample into the cup until it is filled to overflowing.
Strike off the excess with a straightedge, and
I These test methods are under the jurisdiction of ASTM
Committee D-14 on Adhesives and are the direct responsibility
of Subcommittee D 14.10 on Working PropertieS.
Current edition approved Nov. 19, 1963. Published January
1964. Originally published as D 1084 - 50.Last previous edition
D 1084- 60.
Annual Book of ASTM Standards, Vol. 04.04.
'Annual Book of ASTM Standards, Vol. 10.01.
'Annual Book of ASTM Standards, Vol. 06.01.
Annual Book of ASTM Standards, Vol. 06.02.
Annual Book of ASTM Standards, Vol. 08.02.
'Annual Book ofASTM Standards, Vol. 07.01.
188

then remove the finger from over the outlet and
allow the sample to flow into the receiving cylinder.
Determine the number of seconds from
the time the finger is removed from the orifice
until the top of the meniscus reaches to 50-mL
mark on the cylinder by a stop watch and record
as the viscosity of the material.
5. Report
5.1 The report shall include the following:
5.1.1 Complete identification of the adhesive
tested, including type, source, manufacturer’s
code numbers, form, date of test, date of manufacture,
etc.,
5.1.2 Conditioning procedure used for samples
prior to testing,
5.1.3 Number of tests made, and
5.1.4 Average consistency in seconds and the
number of the viscosity cup used.
METHOD B
6. Apparatus
6.1 Viscometer-The apparatus shall consist
of a Brookfield synchrolectric viscosimeter,”
Model RVO, RVF, MVO, or MVF, or an equivalent
instrument. A series of spindles with various
sized disks is provided with each instrument
covering a standard range of viscosities. Scored,
warped, or otherwise damaged spindles shall not
be used. To ensure uniform edge effects, a spindle
guard and cylindrical calibration sleeve shall be
used whenever the data are to be reported in
centipoises. By mutual agreement the instrument
may be USBd without the calibration sleeve or
guard in a standard container such as a 1 qt paint
can, or glass jar, but care must be taken to center
the spindle in the container. Values obtained
without the calibration sleeve shall be reported
as apparent centipoises, and the container shall
be completely described in the report.
5.2 Themomder-A pm5siion thermometer
with graduations not greater than 0.2”C divisions.
7. procedure
7.1 Conditioning-Bring the sample of the adhesive
and the instrument to a temperature of 23
f 0.5% (preferably in a constant-temperature
room), and maintain the sample uniformly at
this standard temperature throughout the test.
Protect adhesives containing volatile solvents
from evaporation during conditioning. If special
conditioning methods are neoessary, such as the
D 1064
use of a circulating water bath, they shall be
specified in 7.1.2.
7.2 Adjustment-Select a spindle suitable to
the viscosity range of the material and firmly fit
it into the shaft extension which comes down
through the center of the dial casing.
7.3 Determination-Insert the spindle perpendicularly
into the material to be tested until
immersed to the depth indicated by the groove
cut into the shaft. Press down the clutch lever
and start the motor by snapping the toggle switch.
Then release the lever and allow rotation to
continue until the pointer has reached the position
where it is stationary in relation to the
rotating dial. Again press down the clutch lever
and snap the switch off. If the pointer is not in
view when the dial has come to rest, the motor
should be started again and allowed to run until
the pointer reaches the vision plate, keeping the
clutch lever depressed. Take the reading at the
pointer. A check reading can also be made by
restarting the motor before releasing the clutch.
If the pointer makes a complete turn of the dial,
this indicates that the viscosity is too great for
the capacity of the spindle used. A slower speed
of rotation or a spindle with a greater range
should be used. If the pointer moves less than
20 % of the way around the dial, this indicates
that the viscosity is too low for accurate measurement
with the spindle or rate of rotation
used. A faster speed of rotation or a spindle with
a lower range should be used. Make a minimum
of three nxdings. Some instruments have two
concentric scales, and great care should be taken
to read the pointer on the corm3 scale as spxified
by the manufacturer for the spindle used.
8. Calibration
8.1 When used for referee purposes, calibrate
the instrument by measuring the VisCosity of a
standard oil: using the same spindle and speed
of rotation employed to measure the wpk. If
the ViscOSity of the oil as read by the instrument
differs by more than 2 % and less than 20 I
from the certified viscosity of the oil, calculate
the viscosity of the unknown by means of the
appropriate correction factor. Investigate a difference
of more tban 20%, and determine a
* Manufactured by the Brookfield Engineering Laboratories,
Stouphton. -.~ MA.
ivailabk from the Cannon Instrument Co., Box 16, State
College, PA 16801.
189

D 1084
calibration curve using at least two standard oils
with viscosities on either side of the sample for
the instrument.
9. Report
9.1 The report shall include the following:
9.1. I Complete identification of the adhesive
tested, including type, source, manufacturer's
code numbers, form, date of test, date of manufacture,
etc.,
9.1.2 Name and model number of the instrument
used,
9.1.3 Number of the spindle used,
9.1.4 Speed used,
9.1.5 Conditioning procedure employed, including
details of the container and time elapsed
between various operations used in the preparation
of the adhesive mix,
9.1.6 Temperature of the sample at the conclusion
of the test,
9. I .7 Number of tests made, and
9.1.8 Viscosity in centipoises, together with
the range of the observation in centipoises.
METHOD C
10. Apparatus
IO. I Viscometer-The apparatus shall consist
of a Stormer viscosimeter with double flag paddle-type
rotor as specified in Test Method D 562,
or an equivalent apparatus. The viscometer shall
be in good repair and the spindle shall spin freely
when started without the paddle.
10.2 Containers-Round friction-top metal
cans having a capacity of 1 qt (0.9 L). Nonstandard
containers may be used by mutual agreement,
when necessary to prevent corrosion or
other deleterious effects of metal cans.
10.3 Thermometer-A precision thermometer
with graduations not greater than 0.2"C divisions.
10.4 Timer-A stop watch or suitable timer
measuring to 0.2 s.
11. Procedure
I 1.1 Conditioning-Bring the containers
holding the samples to be tested and the paddle
to be used to a temperature of 23 +. OS'C (preferably
in a constant-temperature room), and
maintain the sample uniformly at this standard
temperature throughout the test. Protect adhesives
containing volatile solvents from evaporation
during conditioning. If special conditioning
methods are necessary, such as the use of a
circulating water bath, they shall be specified in
12.1.2.
1 1.2 Adjustment-Prepare the instrument for
use by raising the weight to the top by winding
up the cord with the ratchet provided for that
purpose. Set the revolution counter at 10 revolutions
below the zero mark. The falling weight
shall be of such magnitude that a minimum time
of 20 s is required for 100 revolutions of the
paddle when the test is conducted as specified in
11.2. Choose the weight from the series 50, 100,
200, 500, and 1000 g. Fasten the paddle securely
on the shaft, place the container on the platform,
and raise until the surface of the adhesive just
reaches the mark on the stem of the paddle. This
ensures uniform depth of immersion of the paddle.
1 I .3 Determinution-Release the brake on
the large cog wheel, and start the timing device
when the needle on the revolution counter passes
the zero mark. Note the time for 100 revolutions
accurately to the closest 0.2 s. Make a minimum
of three determinations.
12. Report
12. I The report shall including the following:
12.1.1 Complete identification of the adhesive
tested, including type, source, manufacturer's
code numbers, form, date of test, date of manufacture,
etc.,
12. I .2 Conditioning procedure employed, including
time elapsed between various operations
used in the preparation of the adhesive mix,
12.1.3 Details of nonstandard containers, if
used,
12.1.4 Temperature of the sample at the conclusion
of the test,
12.1.5 Weight used,
12.1.6 Number of tests made, and
12.1.7 Average viscosity in seconds for 100
revolutions, together with the range of the observations.
NOTE 2-The limitation of this method to self-leveling
adhesives eliminates thixotropic and plastic materials
whose viscosity is a function of the rate of stirring
and previous history of the adhesive.
13. Apparatus
METHOD D
13. I The apparatus (Fig. 2) shall consist of a
set of five Zahn viscosity C U~S'~SO designed as to
l0Manufactured by the General Electric Co., West Lynn,
MA.
190

D1084
allow a sample to flow through the calibrated
orifice in approximately 1 min or less, best results
being obtained when the flow time is between 20
and 40 s.
13.2 The following figures are given only for
the purpose of selecting the proper viscometer.
They are not intended for use in converting
centipoises to Zahn seconds.
Orifice Size,
Range,
in. (mm) Range, CP Zahn's
0.0788 (2.002) 20 to 85 40 to 85
0.1082 (2.748) 30 to 170 20 to 70
0.1487 (3.777) 170 to 550 25 to 60
0.1684 (4.277) 200 to 900 20 to 65
0.2072 (5.263) 250 to 1200 15 to 60
(and above)
14. Procedure
14.1 Conditioning-Bring the sample of the
adhesive and the cup to a temperature of 23 &
0.5"C (73.4 & 0.9"F), preferably in a constanttemperature
room, and maintain the sample uniformly
at this standard temperature throughout
the test. Other temperatures of test are optional.
Protect adhesives containing volatile solvents
from evaporation during conditioning. If special
conditioning methods are necessary, such as the
use of a circulating water bath, they shall be
specified in 15.1.2.
14.2 Determination-Hold the viscometer in
a vertical position (by means of a small ring at
the end of the handle) and completely immerse
the cup into the. sample being tested. Lift the
viscometer out of the sample (Note 3). Determine
by means of a stop watch the number of seconds
from the time the top edge of the viscometer cup
breaks the surface until the steady flow from the
orifice first breaks, and record this time as the
consistency of the material. Record the temperature
of the sample and the number of the cup.
NOTE 3-Time of removal must be rapid; unless
build-up of adhesive on the side of the cup occurs, the
time of removal should be about 1 s.
15. Report
15.1 The report shall include the following:
15.1.1 Complete identification of the adhesive
tested, including type, source, manufacturer's
code numbers, form, date of test, date of manufacture,
etc.,
15.1.2 Conditioning procedure employed for
samples prior to testing,
15.1.3 Number of tests made, and
15.1.4 Average viscosity in seconds and the
number of the viscosity cup used.
NOTE I-Four consistency cups constitute a set: as follows:
Diameter of Orifice, in.
First cup
0.07 f O.OOO1
Second cup
0.10 f o.Oo01
Third cup
0.15 f O.OOO1
Fourth cup
0.25 f O.Oo01
NOTE 2-Cups made of brass or bronze. Orifice disks made
of I8 X chromium, 8 % nickel stainless steel. The diameter of
the orifice pressed in the cup shall be stamped on the cup.
NOTE 3-Fractional dimensions subject to permissible variations
of plus or minus 0.01 in., unless otherwise specified.
FIG. 1
Consistency Cups and Apparatus Assembly
(Method A)
191

-4
19.5 2 8)
14 (34.666)
-r
T 2.398
f .005
(6.091
i
2.013)
NOTE I -Five
DRIFICE~
AREA
JOINTS
-1.397 f .010 DIA.4
(3.548 .025)
L 375
953)
-F
1.00 u
(2.54)
I
(Dimensions in Inches, Centimetres in Parentheses)
viscosity cups constitute a set, as follows:
Diameter of Orifice
in. + 0.0003 mm + 0.0076
- 0.0002 - 0.005 I
I'
1
I
1
i
I
1.197
- f .005 1.0.
(3.294
- .013)
First cup 0.0788 2.002
Second cup 0.1082 2.748
Third cup 0.1487 3.777
Fourth cup 0. I684 4.277
Fifth cup 0.2072 5.263
N~TE 24ups shall be made of stainless steel, 0.050 in. (1.27 mm) thick. The number of the cup shall be stamped on a plate
on the cup.
FIG. 2 Viscosity Cups (Method D)
192

D1084
APPENDIX
(Nonmandatory Information)
X1. REFERENCE VISCOSITY METHODS
XI.l Reference viscosity methods giving equipment used are shown on the following table:
Test Method for Refers to Equipment Used
Viscosity of Transparent Liquids by Bubble Time D 1545 Gardner-Holdt tubes
Method
Saybolt Viscosity D 88 Saybolt viscometer
Dilute Solution Viscosity of Ethylene Polymers D 1601 Modified Ubbelohde viscometer
Viscosity of Paints, Varnishes, and Lacquers by D 1200 Ford cup
Ford Viscosity Cup
Varnishes Used for Electrical Insulation D 115 MacMichael viscosimeter
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination ofthe validity of any such
patent rights, and the risk of infiingement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyjve years and
is not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.
193

(Nb
Designation: D 1144 - 84
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 49103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index. will appear in the next edition.
Standard Practice for
DETERMINING STRENGTH DEVELOPMENT OF ADHESIVE
BONDS'
This standard is issued under the fixed designation D 1 144; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (6) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This practice covers the determination of
the strength development of adhesive bonds
when tested on a standard specimen under specifed
conditions of preparation and testing. It is
applicable to adhesives in liquid or paste form
that require curing at specified conditions of time
and temperature or specific substrate preparation.
It is intended primarily to be used with
metal-to-metal adherends; however, plastics,
woods, glass, or combinations of these may be
substituted.
1.2 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health practices
and determine the applicability of regulatory limitations
prior to use.
2. Applicable Documents
2. I ASTM Slandards:=
D 1002 Test Method for Strength Properties of
Adhesives in Shear by Tension Loading
(Metal-to-Metal)
D I338 Test Method for Working Life of Liquid
or Paste Adhesives by Consistency and
Bond Strength
3. Significance and Use
3. I This standard contains suggested provisions
for reporting strength values. Any ASTM
test method for determining strength properties
of adhesive bonds may be used. This practice is
not intended to determine the pot or working life
of two-component epoxy of similar type adhe-
sives. Refer to Test Method D 1338. It should be
noted that there are adhesives whose testing requires
special techniques and whose properties
are difficult to reproduce from tester to tester.
These variables should be kept in mind when
analyzing the data obtained using this method.
4. Terminology
4.1 Descriptions of Terms Specific to This
Standard:
4.1.1 jxture time (set time)-the shortest
time required by an adhesive to develop handling
strength such that test specimens can be removed
from fixtures, undamped, or handled without
stressing the bond, thereby affecting bond
strength.
4.1.2 handling strength-a low level of
strength initially obtained by an adhesive that
allows specimens to be handled, moved, or unclamped
without causing disruption of the curing
process or affecting bond strength.
4.1.3 activator, or accelerator (surface)-an
adhesive curing agent that is applied to a bonding
surface for the purpose of affecting or speeding,
or both, the cure of an adhesive.
5. Test Specimens
5.1 It is suggested that lap-type shear specimens
in accordance with Test Method D 1002,
be used. Other types of test specimens may be
' This practice is under the jurisdiction of ASTM Committee
D-14 on Adhesives and is the direct responsibility of Subcommittee
D14.10 on Working Properties.
Current edition approved Feb. 24, 1984. Published April
1984. Originally published as D I 144 - 5 I . Last previous edition
D 1144-57(1975).
Annual Book ofASTM Standards, Vol 15.06.
194

D 1144
used with agreement between the manufacturer
and the purchaser.
6. Preparation of Test Specimens
6.1 Prepare test specimens in accordance with
Test Method D 1002, or other applicable test
method. Preparation of the bonding surface
should be accomplished by a method mutually
agreed upon between the manufacturer and the
purchaser. Vapor phase degreasing, grit blasting,
hand abrasion, or testing on oiled surfaces are
some of the methods that are available. If a
surface activator or accelerator is used, it should
be applied in accordance with the instructions of
the manufacturer. Whether one- or two-surface
activation is used, should be agreed upon between
the manufacturer and the purchaser. Allow
assembled specimens to cure at the temperature
and period of time prescribed by the manufacturer
to develop full strength. This is intended to
determine if any post curing of the adhesive
occurs that would cause a strength increase and
decrease. Bond strength variability could be
caused by embrittlement or a further hardening
of the adhesive during the cure cycle.
6.2 In addition, prepare assemblies for curing
at the same temperature and time intervals to
determine fixture time and 20, 50, and 80%
strength. If the adhesive is cured by heat, specimens
should be heated at a predetermined rate
such that a consistent temperature rise is obtained.
Differences in heating rates will naturally
occur between different types of test specimens
due to different conductivities. Determine the
temperature of the adhesive by means of a
properly insulated thermocouple or contact pyrometer
placed in the geometric center of the
bond area. Bring the adhesive layer to the curing
temperature as promptly as possible and start the
measurement of curing time when the adhesive
has reached the curing temperature.
6.3 After the i;iliiilg tieaimeat, d10~ the S ~ C -
imens to return to room temperature by natural
air convection. Preconditioning of the specimens
prior to testing is permissible upon agreement
between the purchaser and the manufacturer.
Altering the manner in which the cured specimens
are to be returned to room temperature
also is permissible, provided the method is agreeable
to the purchaser and manufacturer. Room
temperature-curing adhesives are allowed to cure
for specific time intervals at a temperature of 22
k 3'C (72 f 6°F). Cure time is measured from
the initial assembly and clamping of test specimens.
If the test adhesive has an unusual cure
mechanism, or does not adapt to conventional
assembly and test methods, a test procedure
should be mutually agreed upon between the
manufacturer and the purchaser. This procedure
should adhere as closely as possible to those
outlined in this practice.
7. Procedure for Determining Fixture Time (Set
Time)
7.1 Prepare test specimens as outlined in Section
6. Apply a specified amount of adhesive, as
recommended by the manufacturer, to one surface.
If a surface activator or accelerator is used,
apply this to the other surface, or both, if specifically
required by the manufacturer or purchaser.
Assemble specimens and clamp as recommended
by the manufacturer.
7.2 After a specified time, remove clamps and
determine if the bond has developed handling
strength. The initial test time should be longer
than is expected to develop handling strength. In
subsequent tests, intervals should be shortened
such that the minimum time to develop handling
strength eventually is determined.
7.3 In testing parts for handling strength, specimens
should be loaded, axially, torsionally, or
in cleavage, to ensure that the blocking strength
of the adhesive is not mistaken for handling
strength. Once the minimum time has been determined,
the test should be repeated a minimum
of three times to ensure its accuracy. For adhesive
types where fixture time is irrelevant or too short
to test, this test should be excluded at the agreement
of the manufacturer and purchaser.
7.4 Test the specimens as described in the
selected appropriate ASTM test method. Test
heat-cured specimens immediately after reaching
room temperature. Room temperature-cured
speciinens are tested iinmzdiately a hi the specified
cure time has elapsed.
8. Report
8.1 The report shall include the following:
8.1.1 Complete identification of the adhesive
tested, including type, source, manufacturer's
code number, lot number, form, and activator,
8.1.2 Complete identification of the adherend
used, its type, thickness, method ofcleaning, and
preparation of surface prior to bonding,
195

D 1144
8.1.3 Standard test method used, unit of time (second, minute, hour),
8.1.4 Application and bonding conditions 8.1.7 Fixture time and cure speed data as acused
in preparing the specimens,
tual test values, versus test time, to the nearest
8.1.5 Cure procedure used for specimens prior standard unit of time,
to testing,
8.1.8 Number of specimens tested, and
8.1.6 Fixturing time to the nearest standard 8.1.9 Number of joints represented.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights. are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
is not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St.. Philadelphia, Pa. 19103.
196

4Tb
Designation: D 1151 - 84
AMERICAN SOCIETV FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annu$l Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
EFFECT OF MOISTURE AND TEMPERATURE ON ADHESIVE
BONDS'
This standard is issued under the fixed designation D 1 I5 I ; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This method has been approved for use by agencies ofthe Department ofDe/;.nse IO replace Methods 2052-T and 2031 of Federal
Test Method Standard No. I75a and for listing in the DoD Index of Specifications and Standards.
1. Scope
1.1 This test method defines conditions for
determining the performance of adhesive bonds
when subjected to continuous exposure at specified
conditions of moisture and temperature. The
performance is expressed as a percentage based
on the ratio of strength retained after exposure
to the original strength.
1.2 This test method may be used to determine
the performance, for suitable materials, in
terms of any desired strength property of adhesive
bonds. Test conditions of temperature and
moisture only are here specified. The duration of
exposure is dependent upon the nature of the
adhesive and the type of specimens, and will,
therefore, be covered by material specifications.
1.3 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safity and health practices
and determine the applicability of regulatory limitations
prior to use.
2. Applicable Documents
2.1 ASTM Standards?
D 897 Test Method for Tensile Properties of
Adhesive Bonds
D903 Test Method for Peel or Stripping
Strength of Adhesive Bonds
D 906 Test Method for Strength Properties of
Adhesives in Plywood Type Construction in
Shear by Tension Loading
D 1002 Test Method for Strength Properties
of Adhesives in shear by Tension Loading
(Metal-to-Metal)
3. Apparatus
3.1 Conditioning Cabinets or Ovens, with
temperature and humidity control.
4. Test Specimens
4.1 Test specimens shall be prepared in accordance
with the recommndations of the manufacturer
of the adhesive. The specimens shall be
of a suitable form and number to meet the requirements
of the investigation. They shall conform
in detail with the requirements prescribed
in the ASTM test method covering the desired
strength property, as listed in Section 2, and any
other ASTM test method pertaining to strength
properties of adhesives for the desired strength
test.
4.2 Matched specimens shall be selected for
control and exposure treatments, the number to
be fixed by the variability inherent in the method.
5. Conditioning
5.1 Preconditioning-All test specimens shall
be conditioned for 7 days at 50 k 2 % relative
humidity and 23 f 1°C (73.4 f 1.8"F) immediately
prior to exposure, or prior to testing in the
' This test method is under the jurisdiction of ASTM Committee
D-14 on Adhesives and is the direct responsibility of
Subcommittee D 14.20 on Durability.
Current edition approved Feb. 24, 1984. Published April
1984. Originally published as D I15 I - 5 I T. Last previous
edition D I I5 I - 72( 1979).
.4nnual Book of ASTM Standards, Vol 15.06.
197

~
case of control specimens. Prior history of the
test specimens should be known and recorded.
5.2 Exposure Conditions-The exposure conditions
shall conform to one of the standard test
exposures given in Table 1.
6. Procedure
6.1 Test the control specimens for strength by
the appropriate method immediately after the
preconditioning period. Average the values obtained.
Record this average as the original
strength against which the strength after exposure
is to be compared in calculating performance.
6.2 Subject the preconditioned specimens to
the designated exposure conditions (Table 1) for
the length of time prescribed by the specification
for the adhesive being tested. At the end of the
exposure period, test the specimens using one of
the following procedures:
6.2.1 Test the specimens under conditions at
which they were exposed, or
6.2.2 Condition the specimens for 4 h at 50 f
2 % relative humidity and 23 +. 1°C (73.4 f.
1.8"F) and test immediately thereafter, or
6.2.3 Condition the specimens for 7 days at
50 f 2 % relative humidity and 23 f. 1°C (73.4
f 1.8"F) and test immediately thereafter.
6.3 Average the strength values obtained and
record the value as the average strength of the
specimens after exposure.
NOTE 1-The conditions under which the exposed
specimens are tested will depend upon the nature of
the adhesive, the adherend, and the strength property
being investigated. This will be prescribed by the material
specifications or by written agreement between
the manufacturer and purchaser of the adhesive.
7. Calculations
7.1 Calculate the performance of the adhesive
under test, as follows:
Performance A = (A/O) x 100,
Performance B = (B/D) x 100,
D 1151
or
Performance C = (C/O) x 100.
where:
A = average strength when tested under the
designated exposure condition in accordance
with 6.2.1,
B = average strength after exposure, when determined
in accordance with 6.2.2,
C = average strength after exposure, when determined
in accordance with 6.2.3, and
D = original strength, determined in accordance
with 6.1.
NOTE 2-Alternative methods of expressing results
may be used.
8. Report
8.1 The report shall include the following:
8.1.1 Complete identification of the adhesive
tested, including type, source, manufacturer's
code number, form, and method of preparation
for use,
8.1.2 Bonding conditions used in preparing
test specimens, and history of specimens prior to
testing.
8.1.3 Description of test specimens, including
materials, size, shape, and designation of ASTM
test method covering the detailed requirements,
8.1.4 Average thickness of adhesive layer after
formation of the joint, within 0.001 in. The
method of obtaining the thickness of the adhesive
layer shall be described including procedure, location
of measurements, and range of measurements.
8.1.5 Test conditions used, any deviation
from conditions listed in Table 1, duration of
exposure, and condition of specimens at test
(6.2.1 or 6.2.2).
8.1.6 Number of specimens tested, strength of
each specimen, and average strength for both
control and exposed specimens, including the
types of failure and am~unts of each tjjpe, and
8.1.7 Performance expressed as a percentage
(Section 7).
_
198

f@
D1151
TABLE I Standard Test Exposures
Test Expo- Temperature“
sure Number
T ‘F
1 -57
2 -34
3
4
-34
0
5 23
6 23
7 38
8 63
9 63
10 63
I1 70
12 70
13 82
14 87
15 82
16 100
17 100
18 I05
19 149
20 204
21 260
22 316
-70
-30
-30
32
73.4
73.4
100
I45
145
145
I58
158
180
I88
180
212
212
22 1
300
400
500
600
Moisture Conditions
as conditioned
as conditioned
presoaked’
as conditioned
50 % RH
immersed in water
88 % RH
oven, uncontrolled
humidity
over wateF
immersed in water
oven, uncontrolled
humidity
over wateF
oven, uncontrolled
humidity
oven, uncontrolled
humidity
over wateF
oven, uncontrolled
humidity
immersed in water
oven, uncontrolled
humidity
oven, uncontrolled
humidity
oven, uncontrolled
humidity
oven, uncontrolled
humidity
oven, uncontrolled
humidity
” The tolerance for test temperature shall be & 1°C or 1.8’F
up to 82’C or 180°F. and -+I % for temperatures above 82°C or
180°F.
’ Presoaking shall consist of submerging specimens in water
and applying vacuum at 5 I cm (20 in.) of mercury until weight
equilibrium is reached.
CThe relative humidity will ordinarily be 95 to 100 %.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item meniioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infiingement of such rights, are entirely their own responsibility.
This standard is subject to revision ai any time by the responsible technical committee and must be reviewed every jive years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which YOU may attend. If you feel that your comments have not received a fair hearing ynu should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, Pa. 19103.
199

#Tb
Designation: D 1200 - 82
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
VISCOSITY OF PAINTS, VARNISHES, AND LACQUERS BY
FORD VISCOSITY CUP'
This standard is issued under the fixed designation D 1200, the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parenthesesindicates the year of last
reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This method has been approvedfor use by agencies of the Department of Defense to replace Method 4282 of Federal Test Method
Standard No. 141A md
for listing in the DoD Index of Specifications and Standards.
1. Scope
1.1 This method covers the determination of
the viscosity of Newtonian or near-Newtonian
paints, varnishes, lacquers, and related liquid
materials with the Ford-type efflux viscosity
cup. If the material is non-Newtonian, that is,
shear-thinning or thixotropic, Method D 2196
should be used.
1.2 The cup-orifice combination (Ford No.
2, No. 3, or No. 4) is selected to provide an
efflux time within the range 20 to 100 s. When
the time of efflux is beyond this range, accurate
temperature control is difficult. Any departure
from Newtonian behavior may result in a lack
of reproducibility because of the diffkulty of
judging the break in the stream.
2. Applicable Documents
2.1 ASTM Standards:
D 2196 Test for Rheological Properties of
Non-Newtonian Materials2
E 1 Specification for ASTM Thermometers3
3. Summary of Method
3.1 The Ford viscosity cup is filled level full
with the liquid under test, and the time f ~ the r
material to flow through one of the standard
orifices is measured.
4. Significance and Use
4.1 This method is useful for the determination
of package and application viscosities of
a number of paints and other Coatings and in
the thinning of these materials, but is limited
to Newtonian or near-Newtonian liquids.
4.2 There are other types of apparatus for
measuring viscosity in the laboratory that produce
more accurate results.
5. Definitions
5.1 Newtonian liquid-a liquid in which the
viscosity is independent of the shear stress or
shear rate. If the ratio of shear stress to shear
rate is not constant, the liquid is non-Newtonian.
5.2 Near-Newtonian liquid-a liquid in
which the variation of viscosity with shear rate
is small and the effect on viscosity of mechanical
disturbances such as stirring is negligible.
6. Apparatus
6.1 Ford Viscosity Cup-No. 2, No. 3, and
No. 4 Ford viscosity cups made of corrosionand
solvent resistant materials assembled as
complete units (Note l), and conforming to the
dimensional requirements shown in Fig. 1. The
orifice dimensions are considered as a guide for
manufacture only and standardization of the
instruments shall be based upon the calibration
procedure described in the Appendix.
NOTE 1-If the orifice is removed from the cup
for any reason the cup should be recalibrated before
use as described in the Appendix.
6.2 Thermometer-Saybolt Viscosity Ther-
'This test method is under the jurisdiction of ASTM
Committee D-l on Paints and Related Coatines and Materials
and is the direct responsibilityof SubcomGittee D01.24
on Physical Properties of Liquid Paints and Paint Materials.
Current edition approved Nov. 26, 1982. Published January
1983. Originally published as D 1200 - 52 T. Last previo;s
edition D 1200 - 70 (1976).
1983 Annual Book of ASTM Standards, Vol06.01.
1983 Annual Book of ASTM Standards, V0103.04.
200

D1200
mometer conforming to the requirements for
Thermometer 17C or 17F (66 to 80°F) as prescribed
in Specification E 1.
6.3 Timing Device-Stop watch or other timing
device graduated in divisions of 0.2 s or
less, and accurate to within 3.6 s as compared
to an electric clock operated for a period of 1
h.
NOTE 2-Timing devices actuated by synchronous
motors may be used on electric circuits of
controlled frequency only if they are accurate and
capable of being read to 0.2 s.
7. Test Sample
7.1 The sample of the material to be tested
shall be visibly homogeneous and free of any
foreign material or air bubbles.
8. Temperature of Testing
8.1 All measurements with the Ford viscosity
cup shall be made at 77°F (25°C) or a
temperature agreed upon between producer
and user. Temperature drift during the test
should be kept to a minimum.
NOTE 3-A reasonable temperature tolerance and
drift limit is +l.O°F (*OS0C). It is impossible to
predict the effect of temperature change on each
product with which the apparatus may be used. This
factor may be less than 1 % per degree Celsius for
some liquids while others may be considerably
higher.
9. Calibration
9.1 Cups should be calibrated in accordance
with the procedure described in the Appendix.
The frequency of this calibration check depends
upon the amount of use and the care
that the individual cup receives. If the cup
varies more than 10 5% from standard, it should
not be used.
10. Conditioning
10.1 Bring the material to a temperature a
few degrees below that desired and then agitate
vigorously for 10 min on a reciprocating shaker
in a pint can two thirds full. Allow to stand
undisturbed for 10 min while adjusting further
to the desired temperature. Make the viscosity
determination at the end of the 10-min period.
11. Procedure
11.1 Make viscosity determinations in a
room free of drafts and rapid changes in temperature.
For the highest degree of precision
the room temperature should be between 72
and 82'F (22 and 28°C). Determinations
should be made at a temperature above the
dew point of the atmosphere surrounding the
apparatus.
11.2 Choose the proper cup so that the time
of efflux will be between 20 and 100 s for cups
No. 3 and 4 and between 40 and 100 s for cup
No. 2 (Fig. 2).
11.3 Level the instrument so that a cup may
be filled level full without a meniscus or overflow
at one side.
11.4 Determine the time in seconds of efflux
as follows: Close the orifice with the finger and
fill the cup with the prepared sample. The
preferred method is to overfill the cup and
scrape off the excess with a straight edge. Remove
the finger and measure the time from the
moment efflux starts until the first break in the
stream.
11.5 If the cup has been established to be
nonstandard when calibrated as described in
the Appendix, apply the percent difference to
the measured seconds to get the corrected viscosity
in Ford cup seconds.
12. Care of Cup
12.1 Following each determination, clean
the cup by the use of a suitable solvent and a
soft brush. Under no conditions should metal
cleaning tools be brought into contact with the
instrument. Particular care must be exercised
in cleaning the orifice to avoid any film deposit
or nicks on the inside walls.
13. Report
13.1 Report the efflux time to the nearest 0.2
s for the cup orifice combination (for example,
viscosity 23.2 s with No. 4 Ford cup) the temperature
of the test specimen (and where measured,
for example, in efflux stream, cup, or
container in which the material was conditioned),
and the immediate history of agitation
and rest prior to the measurement.
14. Precision
14.1 On the basis of an interlaboratory test
of the method in which eight cooperators from
four different laboratories made measurements
on five different paints, the within-laboratories
coefficient of variation was found to be 2.8 %
with 35 degrees of freedom and the betweenlaboratories
coefficient of variation was found
20 1

D1200
to be 6.9% with 30 degrees of freedom. Based
on these coefficients, the following criteria
should be used for judging the acceptability of
results at the 95 % confidence level:
14.1.1 Repeatability-Two results obtained
by the same operator on different days should
be considered suspect if they differ by more
than 8%.
14.1.2 Reproducibility-Two results obtained
by operators in different laboratories
should be considered suspect if they differ by
more than 20%.
9.5 mm-24 N.F. 2
FORD VISCOSITY CUP
v)
W
Y
0
I-
F"
z
W
V
i
t
v)
0
0
s
>
TIME, SECONDS
FIG. 2 Approximate Viscosity Curves for Ford Cups
No.2 Orifice No.3 OiTfice, A.3.4 mm
No.4 Orifice, A.4.1 II
FIG. 1 Ford Viscosity Cup and Orifices
APPENDIX
XI. Calibration Procedure for Ford Cups
X1.l The orifice of the Ford cup is commonly
made of brass or some other corrosion-resistant material
which is subject to wear with use and cleaning
A small change in diameter of the orifice becomes
significant in the results obtained with the use of this
type of viscosity-measuring apparatus.
X1.2 The viscosity standards4 are available only
as 1-pt samples.
X1.3 Select the appropriate liquid viscosity standard
for the cup to be calibrated. Bring this cup and
the liquid viscosity standard to a constant temperature
as close as possible to 77.O"F (25.0"C) or to the
operating temperature of the cup. Determine the time
of efflux to the nearest 0.2 s using the procedure
detailed in Section 11. Keep the temperature drift to
within -+0.4"C. If the temperature is not 77'F, the
actual temperature must be noted and the viscosity
of the standard oil corrected to this temperature.
X 1.4 The fc!!cwing fermulas are used to conver:
the time of flow in seconds to kinematic viscosity:
Centistokes (No. 2 = 2.388t - 0.007t2 - 57.008
orifice)
Centistokes (No. 3 = 2.3 14t - 15.200
orifice)
Certified kinematic viscosity standards are available
from the Cannon Instrument Co., P.O. Box 16, State College,
Pa. 16801. For particular oils applicable for use with the
Ford Cups refer to Table X1.1. Oils available from other
sources, having known kinematic viscosities, may also be
used.
202

Centistokes (No. 4 = 3.846t - 17.300 cent variation of the cup from standard. A percent
orifice)
correction can be applied to the seconds flow when
where t = time of flow, s.
the cup is in normal use. If the cup varies more than
X 1.5 The difference between the certified viscosity 10 9% from standard, it is recommended that the
and the determined viscosity, multiplied by 100 and orifice be replaced and that the cup be recalibrated.
divided by the certified viscosity, will give the per-
TABLE Xl.1 Viscosity Standards Recommended for
Calibrating Ford Viscosity Cups
Designated
CUP
Number Range' 'St
Standard
Designation
Viscosity at
77°F
(25°C)A, cSt
2 25 to 120 s-20 35
3 40 to 220 S-60 I20
4 70 to 370 S-60 120
A Exact viscosities are suppIied with the oil samples.
The American Society for Testing and Materials takes no position respecting the validity of any parent rights asserted in
connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity
of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years
and f not revised, either reapproved or withdrawn. Your comments are invited either for revision ojthis standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, Pa. 19103.
203

AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appmr in the next edition.
Standard Test Method for
COLOR OF CLEAR LIQUIDS (PLATINUM-COBALT SCALE)'
This standard is issued under the fixed designation D 1209, the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parenthcscs indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This test method has been approved for use by agencies of the Department of Dqhie to replace Method 4243. I of Federal Test
Method Standard No. 141A and for listing in the DoD Inda ofSpeci$catim and Sta&r&.
1. scope
1.1 This test method describes a procedure for
the visual measurement of the color of essentially
light colored liquids (Note 1). It is applicable only
to materials in which the color-producing bodies
present have light absorption characteristics
nearly identical with those of the platinumabalt
color standards used.
NOTE I -A procedure for estimating color of darker
liquids, described for soluble nitrocellulose base solutions,
is given in Methods D 365.
1.2 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety prob
lems associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health practices
and determine the applicability of regulatory limitations
prior to use. Specific precautionary statements
are given in Section 6.
2. Applicable Documents
2.1 ASTM Standards:
D 156 Test Method for Saybolt Color of Petroleum
Products (Saybolt Chromometer
Method)'
D365 Methods for Testing Soluble Nitrocellulose
Base Solutions3
D 1 193 Specification for Reagent Water"
E 180 Recommended Practice for Developing
Precision Data on ASTM Methods for Analysis
and Testing Industrial Chemicals4
E 202 Method for Analysis of Ethylene Glycols
and Propylene Glycol4
E 346 Method for Analysis of Methanor
3. Signifiaulce and use
3.1 The property of color of a solvent varies
in importance with the application for which it
is intended, the amount of color that can be
tolerated being dependent on the color characteristics
of the material in which it is used. The
paint, varnish, and lacquer solvents, or diluents
commercially available on today's market normally
have little or no color. The presence or
absence of color in such material is an indication
of the degree of refinement to which the solvent
has been subjected or of the cleanliness of the
shipping or storage container in which it is handled,
or both.
3.2 For a number of years the term "waterwhite"
was considered sufficient as a measurement
of solvent color. Several expressions for
defining "water-white" gradually appeared and it
became evident that a more precise color standard
was needed. This was accomplished in 1952
with the adoption of Test Method D 1209 using
the platinum-cobalt scale. This test method is
similar to the description given in the Standard
Methods for the Examination of Water and
Waste Water of the American Public Health
Assn., 14th Ed., p. 65 and is referred to by many
as "APHA Color." The preparation of these platinum-cobalt
color standards was originally de-
' This test method is under the jurisdiction of ASTM Committee
Dl on Paint and Related Coatings and Materials and is
the direct responsibility of Subcommittee W1.35 on Solvents,
Plasticizers, and Chemical Intermediates.
Current edition approved April 27. 1984. Published August
1984. Originally published as D 1209 - 52. Last previous edition
D 1209 - 79.
Annual Book of ASTM Standards, Vol05.01.
'Annual Book of ASTM Standards, Vol06.02.
'Annual Book of ASTM Standards, Vol06.03.
204

D 1209
scribed by Hazen, A., American Chemical Journal,
Vol XIV, 1892, p. 300, in which he assigned
the number 5 (parts per ten thousand) to his
platinum-cobalt stock solution. Subsequently, in
their first edition ( 1905) of Standard Methods for
the Examination of Water, the American Public
Health Assn., using exactly the same concentration
of reagents, assigned the color designation
500 (parts per million) which is the same ratio.
The parts per million nomenclature is not used
since color is not referred directly to a weight
relationship. It is therefore recommended that
the incorrect term "Hazen Color" should not be
used. Also, because it refers primarily to water,
the term "APHA Color" is undesirable. The recommended
nomenclature for referring to the
color of organic liquids is "Platinum-Cobalt
Color, Test Method D 1209."
3.3 The petroleum industry uses the saybolt
colorimeter Method D 156 for measuring and
defining the color of hydrocarbon solvents; however,
this system of color measurement is not
commonly employed outside of the petroleum
industry. It has been reported by various sources
that a Saybolt color of +25 is equivalent to 25 in
the platinum-cobalt system or to colors produced
by masses of potassium dichromate ranging between
4.8 and 5.6 mg dissolved in l L of distilled
water. Because of the differences in the spectral
characteristics of the several color systems being
compared and the subjective manner in which
the measurements are made, exact equivalencies
are difficult to obtain.
4. Apparatus
4.1 Spectrophotometer, equipped for liquid
samples and for measurements in the visible
region.'
NOTE 2-The spectrophotometer used must be
clean and in first4a.s operating condition. The instrument
should be calibrated in accordance with the instructions
given in the Standards for Checking the
Calibration of Spectrophotometers (200 to IO00 nm)!
4.2 Spectrophotometer Cells, matched having
a IO-" light path.
4.3 Color Comparison Tubes-Matched 100-
mL, tall-form Nessler tubes, provided with
ground-on, optically clear, glass caps. Tubes
should be selected so that the height of the 100-
mL graduation mark is 275 to 295 mm above
the bottom of the tube.
4.4 Color Comparator-A color comparator
constructed to permit visual comparison of light
transmitted through tall-form, 100-mL Nessler
tubes in the direction of their longitudinal axes.
The comparator should be constructed so that
white light is passed through or reflected off a
white glass plate and directed with equal intensity
through the tubes, and should be shielded so that
no light enters the tubes from the side.
5. Reagents
5.1 Purity of Reagents-Reagent grade chemicals
shall be used in all tests. Unless otherwise
indicated, it is intended that all reagents shall
conform to the specifications of the Committee
on Analytical Reagents of the American Chemical
Society, where such specifications are available.'
Other grades may be used, provided it is
first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening
the accuracy of the determination.
5.2 Purity of Water-Unless otherwise indicated,
references to water shall be understood to
mean reagent water conforming to Type IV of
Specification D 1193.
5.3 Cobalt Chloride (CoC12-6H20).
5.4 Hydrochloric Acid (sp gr l.l9)-Concentrated
hydrochloric acid (HCI).
5.5 Potassium Chloroplatinate (K2PtC16).
6. !Safety Precautions
6.1 Concentrated hydrochloric acid is a corrosive
chemical. For further information, see
supplier's Material Safety Data Sheet.
7. Platinum-Cobalt Reference Standards
7.1 Platinum-Cobalt Stock Solution-Dissolve
1.245 g of potassium chloroplatinate
(K2Pt&) and 1 .00 g of cobalt chloride (CoC12 e
6H20) in water. Carefully add 100 mL of hydrochloric
acid (Ha, sp gr 1.19) and dilute to 1 L
with water. The absorbance of the 500 platinumcobalt
stock solution in a cell having a 10-mm
light path, with reagent water in a matched cell
as the reference solution,* must fall within the
limits given in Table I.
-
The Beckman Model Band its equivalents have been found
satisfactory for this purpose.
See National Bureau of Standards Letter Circular LC- 1017.
'"Reagent chemicals, American Chemical Society Specifications,"
Am. Chemical Soc.. Washington, DC. For suggestions
on the testing of reagents not listed by the American Chemical
Society, see *Reagent Chemicals and Standards," by Joseph
Rosin, D. Van Nostrand Co., Inc.. New York, NY, and the
. n
"United States wannacopcla.
*See the manufwtum's instruction manual for complete
details for operating the spctrophotametcr.
205

7.2 Platinum-Cobalt Standards-From the
stock solution, prepare color standards in accordance
with Table 2 by diluting the required volumes
to 100 mL with water in the Nessler tubes.
Cap the tubes and seal the caps with shellac or a
waterproof cement. When properly sealed and
stored, these standards are stable for at least 1
year and do not degrade markedly for 2 years.'
7.2.1 For a more precise measurement of light
colors below 15 platinumcobalt, prepare color
standards from the stock solution in accordance
with Table 3 by diluting the required volumes to
100 mL with water in the Nessler tubes. Use a
semi-microburet for measuring the required
amount of stock solution.
8. Procedure
8.1 Introduce 100 mL of sample into a Nessler
tube, passing the sample through a filter if it has
any visible turbidity. Cap the tube, place in the
comparator, and compare with the standards.
9. Report
9.1 Report as the color the number of the
standard that most nearly matches the specimen.
In the event that the color lies midway between
two standards, report the darker of the two.
9.2 If, owing to differences in hue between the
specimen and the standards, a definite match
cannot be obtained, report the range over which
an apparent match is obtained, and report the
material as "off-hue".
10. Precision'o
10.1 Color Standards:
10.1.1 These precision statements are based
upon an interlaboratory study in which five platinum-cobalt
standards having values of 25, 75,
170, 385, and 475 were prepared in accordance
with the instructions given in Section 7 of this
test method and were given coded labels. These
solutions were tested by one analyst in each of
ten different laboratories making a single observation
on one day and then repeating the observation
on a second day. The analysts were requested
to estimate the color to the nearest one
unit for solutions below 40 platinum-cobalt, to
the nearest five units for solutions b een 40
and 100 platinumabalt and to the nearest ten
units for solutions above 100 platinumabalt. In
this interlaboratory study, the within-laboratory
D 1209
coefficient of variation was found to be 1.8 %
with 60 degrees of freedom, and the betweenlaboratories
coefficient of variation was found to
be 5.3 % with 54 degrees of freedom. Based on
these results, the following criteria, calculated in
accordance with Recommended Practice E 180,
should be used for judging the acceptability of
results at the 95 % confidence level when the
results are obtained under optimum conditions
where the hue of the sample matches exactly the
hue of the standards. Poorer precision will be
obtained in varying degrees as the hue of the
sample departs from that of the standards.
10.1. I. 1 Repeafability-Two results, obtained
by the same analyst on different days,
should be considered suspect if they differ by
more than 5.1 %.
10. I. 1.2 Reproducibility-Two results, ob
tained by analysts in different laboratories,
should be considered suspect if they differ by
more than 15 %.
10.2 Specimen:' '
10.2.1 In an interlaboratory study of this test
method in which the standards described in Table
3 were used, the within-laboratory standard
deviation was found to be one platinum-cobalt
unit at 56 degrees of freedom and the betweenlaboratory
standard deviation was found to be 2
platinum-cobalt units at 25 degrees of freedom.
Based on these standard deviations, the following
criteria should be used for judging, at the 95 %
confidence level, the acceptability of results obtained
on light colored samples.
10.2.1.1 Repeatability-Two results, each the
mean of duplicates, obtained by the same operator
on different days should be considered suspect
if they differ by more than two platinumcobalt
units.
10.2. I .2 Reproducibility-Two results, each
the mean of duplicates, obtained by operators in
different laboratories should be considered suspect
if they differ by more tnan seven piatinumcobalt
units.
'Scharf, W. W., Ferbes, K. H., and White, R. G., 'Stability
of Platinum-Cobalt Color Standards," Materials Research and
Standards, Vol6, No. 6, June 1966, pp. 302-304.
lo Supporting data are available on loan from ASTM Headquarters,
1916 Race St., Philadelphia, PA 19103. Request RR
Dol-1024.
'I These precision statements arc based on interhboratory
studies conducted by Committee E-15 on Industrial Chemicals
on samples of ethylene glycol and methanol as reported in
Method E 202, Method E 346, and rrsearch report RR E 15-28.
_
_
206

~~
D 1209
TABLE 1 Abmrbmce TdeMee umits For No. 500
phti.racohlt stock solulion
Wavelength. nm
GAor
Standard
Number
Stock
Solution,
mL
Absorbance
430 0.1 10 to 0.120
455 0.130 to 0.145
480 0.105 to 0.120
510 0.055 to 0.065
5 I
IO 2
IS 3
20 4
25 5
30 6
35 7
40 8
50 10
60 12
Color
Standard
Number
Stock
Solution,
mL
70 14
100 20
I50 30
200 40
250 50
m 60
350 70
400 80
450
500
90
lW
A This is phtinumabalt color No. 10 in Methods D 365.
Color
Standard
Number
Stock
Solution,
mL
I 0.20
2 0.40
3 0.60
4 0.80
5 1 .00
6 I .20
I I .40
8 1-60
Color
Standard
Number
Stock
Solution,
mL
9 I .80
10 2.00
II 2.20
12 2.40
13 2.60
14 2.80
15 3.00
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights. and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyjive years and
ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
starhra3 and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
resjwnsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
&your views known to the ASTM Committee on Standards, 1916 Race St.. Philadelphia, Pa. 19103.
207

Designation: D 1210 - 79 (Reapproved 1983)’‘
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
FINENESS OF DISPERSION OF PIGMENT-VEHICLE
SYSTEMS‘
This standard is issued under the fixed designation D 12 10; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (c) indicates an editorial change since the last revision or reapproval.
This test method has been approved for use by agencies of the Department of Defense and for listing in the DoD Index of Spec~cations
and Standards.
‘I NoTE-Editorial changes were made throughout in December 1983.
1. Scope
1.1 This test method covers measurement of
the degree of dispersion (commonly referred to
as “fineness of grind”) of the pigment in a pigment-vehicle
system such as liquid coatings and
their intermediates. It may also be used to assess
the inclusion of particulates by a cleanliness rating.
1.2 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problcms
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health pratices
and determine the applicability of regulatory limitations
prior to use.
2. Summary of Method
2.1 The product is spread by means of a
scraper in a calibrated tapered path. At some
point in this path, particles or agglomerates, or
both, will become visible. A direct reading from
the calibrated scale is then made at the point
where the particles form a definite pattern. When
the single path gage is used it is also possible to
rate “cleanliness” (see 6.2).
3. Significance
3.1 In making pigmented products, the pigment
is usually dispersed in a portion of the
vehicle in some sort of mill. At this stage, it is
necessary to be able to judge if the pigment
agglomerates have been sufficiently broken up so
as not to interfere with the smoothness of the
finished coating film. This method describes a
way of making this judgment.
4. Apparatus
4.1 Gage-A hardened steel, stainless steel, or
chrome-plated steel block (Fig. 1) approximately
6.7 in. (170 mm) in length, and 0.6 in. (15 mm)
in thickness. The top surface of the block shall
be ground smooth and planar and shall contain
one or two paths 5 in. (127 mm) in calibrated
length. The path shall be tapered uniformly in
depth lengthwise from 100 pm (about 4 mils) at
10 mm from one end to zero depth at the other
with intermediate calibrations in accordance
with the depth at those points. Preferred calibrations
are Hegman units and micrometres (Note
1). Two path widths are covered by this method
of test:
4.1.1 Two parallel paths each 0.5 in. wide
(12.5 mm) and spaced 0.5 in. apart centered in a
block 2.5 in. (65 mm) wide.
4.1.2 One path 2 in. (50 mm) Ir! width cmtered
in a block 3.5 in. (90 mm) wide.
NOTE 1 -Several arbitrary scales and modifications
I This test method is under the jurisdiction of ASTM Committee
D-1 on Paint and Related Coatings and Materials, and is
the direct responsibility of Subcommittee W1.24 on Physical
Properties of Liquid Paint and Paint Materials.
Current edition approved Nov. 30, 1979. Published Januaw
1980. Originally published as D 12 10 - 52. Last previous editioh
D 1210- 78.
* The report on which this precision statement is based has
been filed at ASTM Headquarters, 1916 Race St., Philadelphia,
Pa. 19103 as RR DO1 - 1017.
208

of the gage are used by industry. In order that readings
obtained with these arbitrary scales and modifications
can be reported in the preferred units, the approximate
relationship of these scales to gage depth is shown in
the following example:
PC or
Hegman Depth, Depth, FSFT NPIRI
%le” pmB milsB Scale‘ kale’
0 100 4 0 40
I 90 3.5 1 ‘/4 35
2 15 3 2% 30
3 65 2.5 3% 25
4 50 2 5 20
5 40 1.5 6% 15
6 25 I 1’/2 IO
7 15 0.5 8% 5
8 0 0 10 0
” Sometimes referred to in error as the North Standard scale.
Rounded to nearest 5 pm or 0.5 mil.
‘ Federation of Societies for Paint Technology scale.
’National Printing Ink Research Institute scale, 0 to IO on
the NPIRI Production Grindometer, but extended on many
gages to 20 or 30.
4.2 Scraper-A double-edged hardened steel,
stainless steel, or chrome-plated steel blade (Fig.
2) 3.75 in. (95 mm) long, 1.5 in. (38 mm) wide,
and 0.25 in. (6.4 mm) thick. The two edges on
the 3.75-in. sides shall be rounded to a radius of
0.0 15 in. (0.38 mm).
5. Care of Gage
5.1 Clean the gage immediately after each use.
Use a solvent and a soft cloth. Keep the gage
covered or encased at all times when not in use.
Protect gages that lie idle for extended periods of
time from rust with an oil coating or oil soaked
wrap.
5.2 Do not allow any hard materials to come
in contact with the gage surface or scraper in any
manner that might result in scarring or nicking.
Avoid tapping or scratching with other metal.
5.3 The scraper may be rendered unsatisfactory
for use by wear or nicks of the contact edge
or warpage (Note 2). Replace or recondition unsatisfactory
blades.
NOTE 2-Wear or warpage of the scraper may be
noted by facing the edge of the scraper down on the
smooth level face of the gage, then inspecting the contact
edge by means of a strong light, placed behind the
gage. Rocking the scraper forward or back will reveal
poor contact due to wear or warpage. Any light coming
through between scraper and gage face shows that the
scraper has been damaged and is not satisfactory for
USe.
6. Visual Standards
6.1 The diagrams in Fig. 3 are reproductions
of six typical fineness gage patterns with the
double-path gage, 4.1.1, and they should be
viewed with the purpose of standardizing the
relationship of particle distribution to fineness
designation. The arrow in each drawing represents
the end point (reading) for that distribution.
These patterns are to be used for notation of
frequency of particles and should not be interpreted
according to the size of the dots. Although
called “standards,” they are really examples of
fineness readings to be used as a guide, since no
two particle distributions will be exactly the
same.
6.2 Similarly, Fig. 4 exhibits typical fineness
gage patterns for the 2-in. (5 1-mm) gage, 4.1.2.
These diagrams are to be used like those for the
double-path gage except that a “cleanliness” rating
is also shown. “Cleanliness” is descriptive of
the number of particles that appear in the path
above the fineness designation. Three ratings are
indicated: “A” (0 to 8 specks), “B” (9 to 15
specks), and “C” ( 16 or more specks).
7. Procedure
7.1 Place the gage on a horizontal flat, nonslippery
surface and wipe clean immediately before
the test. Be sure the gage surface is free of
lint.
7.2 Hand stir the sample (Note 3) vigorously
for 2 min, taki,ng care that air bubbles are not
whipped into the paint. To be sure of an accurate
grind reading, samples must be free of air bubbles.
NOTE 3-For this method to function properly, the
pigment particles in the samples to be tested should be
free to settle to the bottom of the gage channel after the
drawdown. Therefore, before testing, high-viscosity intermediate
samples which have little ability to flow
should be reduced with a compatible liquid. Reduction
should be in approximately the same proportion as the
intermediate will be reduced in practice.
7.3 Immediately place the material to be
tested in the deep end of the path, or paths, so
that it overflows the path slightly. When using
the double-path gage, place material in both
paths.
7.4 Holding the scraper in both hands, nearly
vertical but inclined slightly toward the operator,
draw the material down the length of the path
toward the shallow end of the gage with a uniform,
brisk motion in approximately 1 to 2 s.
Exert upon the scraper only sufficient pressure
to clean excess material from the face of the gage
within 10 s of placing the specimen on the gage,
make a reading as follows:
209

7.4.1 View the gage from the side, perpendicular
to the length of the path. Keeping the gage
between the operator and the light source, make
the angle between the face Of the gage and the
line of vision between 20 and 30 deg.
NOTE 4-clear finishes may have to be Viewed at a
lower angle or they may have to be Opacified with a
finely ground colorant or dye in order to see better the
particles of flatting pigment.
7*4*2 Observe the point where the mate.ria1
first shows a definite speckled pattern, not just
isolated specks (see Figs. 3 and 4). This is the
fineness reading. When using the two-path gage,
average the values in the two paths to the nearest
'/4 Hegman unit. This average is considered one
reading.
7.5 After the first drawdown and reading,
which are preliminary for establishing proper test
conditions and locating the position of the fineness
reading, repeat the procedure twice, beginning
with 7.3, to obtain two test readings. This
process allows the two test readings to be made
with limited time lapses between completion of
drawdown and reading. (Do not consider any
reading for the reported fineness when the time
lapse exceeds 10 s.) Average the two readings to
the nearest '/4 Hegman units (5 pm).
7.6 Interpretation of Dispersion Pattern:
7.6.1 Inspect the initial drawdown for pattern
and the approximate fineness. Determine the
point in the particle distribution that approximates
a similar end point pattern to that of the
pictorial standards.
7.6.2 Judge cleanliness on the one-path gage
either by comparison to the typical fineness patterns
(shown only at a 6 Hegman level but applicable
by analogy to any fineness level) or by
counting nibs coarser than the selected fineness
level (see 6.2 for cleanliness ranges).
8. ReDort
8.1 Report whether gage 4.1.1 (two path) or
gage 4.1.2 (one path) was used. The reported
reading is the average of two readings conforming
to the conditions of7.6. Micrometre readings are
to be reported to the nearest multiple of 5 pm
and Hegman readings to the nearest '14 unit.
Cleanliness may be reported also when using the
two path gage.
9. Precision
9.1 On the basis of an interlaboratory test of
this method in which 23 operators in 7 laboratories
tested 6 samples of paints covering a broad
range of compositions and finenesses, the singleoperator
standard deviation was found to be 0.27
Hegman units (3.4 pm), the within-laboratory
standard deviation was found to be 0.70 Hegman
units (8.8 pm) and the between-laboratories
standard deviation was found to be 0.74 Hegman
units (9.3 pm). Based on these standard deviations
and the requirement that readings are to be
reported to the nearest '/4 Hegman unit or multiple
of 5 pm, the following criteria should be
used for judging the precision of results at a 95 76
confidence level:
9.1.1 Repeatability-Two results obtained by
a single operator should be considered suspect if
they differ by more than 3/4 Hegman unit (10
pm).
9.1.2 Reproducibility-Two results, each the
mean of two results obtained by different operators
in the same or different laboratories should
be considered suspect if they differ by more than
29" Hegman units (25 pm).
210

H
0-
I -
2-
-
3-
-
4-
-
5-
6-
7-
-
8-
-
-60
-
-40
-
-
-2 0
-
-
-0
Two-Path Gage
FIG. 1 Fineness Gages
One-Path Gage
21 1

Note-! in. = 25.4 mm
FIG. 2 %per
212

D 1210
H
0-
- 100
H
0-
- 100
c
I -
-
2-
I -
C__
2-
-
-75
3-
4-
-50
4-
5-
-
-
5-
6-
_._-
-25
-
6-
-
7 --
--
7-
_c_
8-
13/4 Hegman 80 pm
FIG. 3a Typical Fineness Gage Patterns
8-
3% Hegman 60 pm
213

D1210
H
0-
-100
H
0-
- 190
I -
2-
0
-
I -
-75 2-
-7s
-
3-
3-
Ai-
-
5 -.-
:
-50
4-
5-
-50
6-
-- -
-25
6-
-25
7- I
7-
8-
4 Hegman 50 pm
0
8-
4% Hegman 40 pm
FIG. 3b Typical Fineness Gage Patterns
-0
214

H
0-
- 100
H
0 --
-
- IO0
I -
I -
-
2-
c__
3-
2-
-
3-
L__
4-
c_
5-
7-
--
8-
-50
-25
-
4-
-
5-
-
6-
--
>
7-
-
8-
6 Hegman 25 pm 6% Hegman 15 pm
FIG. 3c Typical Fineness Gage Patterns
-
-25
-
-0
215

D 1210
H
I
H
0-
0-
I -
-
.
I
3-
-
4-
-
5-
-
. .
I ’
. .
. .
- .
.. .. .
* ’
. - . -
- .-
. .I
. - .
. .
.-
..
6-
7-
-
7 -I
-
8-
I Hegman 85 pm “A” Cleanliness
FIG. 4a Typical Fineness Gage Pattern
8-
2 Hegman 75 pm “A” Cleanliness
FIG. 4b Typical Fineness Gage Pattern
216

D1210
&
- 100
42w
- 100
-
-75
-
-75
-
-50
-
-50
-
-25
-25
-
3 Hegman 60 pm "A" Cleanliness
FIG. 4c Typical Fineness Gage Pattem
-0
4 Hegman 50 pm "B" Cleanliness
FIG. 4d Typical Fineness Gage Pattern
-
-0
217

H
0-
-
I -
2-
-
3-
.
H
0-
-
I -
-
2-
_-
3-
L
4-
-
5-
-
6-
-
7-
-
8-
..
- :
' . . .,
. -
. . I - ,
. .' . -
.. .. I :
I . . - I * , .
5 Hegman 35 pm "C" Cleanliness
FIG 4e Typical Fineness Gage Pattern
-50
-
4-
-2s
- 6,
-
-0
c
7-
8-
6 Hegman 25 pm "A" Cleanliness
FIG. 4f Typical Fineness Cage Pattern
218

D1210
H
0-
-
I -
2-
-
3-
c
4-
-
5-
.
,
.*
L
__L.-6.1;
. . ‘0
-
7-
-
8-
. -
. . -. -
I .
. ,
..... . 1 . . . . .
..........
;...-.*: :,:;:
.........
...- ................. :...-......:’.’.’
.. .-,.-- , :..
6 Hegman 25 pm “B” Cleanliness
FIG. 4g Typical Fineness Gage Pattern
-0 8-
I
6 Hegman 25 pm “C” Cleanliness
FIG. 4h Typical Fineness Gage Pattern
219

H
0-
-
I -
--
2-
-
3-
r(m D1210
. . . .
._ . . .
. . . . ......
. .
....;*..:. . -‘ . *
;.,-.:;- .;:.:-.: ..........
............. .. :’:::’. ......
.. . - _ .
7 Hegman 10 pm “A” Cleanliness
FIG. 4i Typical Fineness Gage Pattern
The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection
with any item mentioned in [his standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights. are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyjve years and
f not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a medng yf the
responsible technical commiitee, which you may attend. rf you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 19/15 Race St.. Philadelphia, Pa. 19103.
220

Designation: D 1218 - 82
An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
REFRACTIVE INDEX AND REFRACTIVE DISPERSION OF
HYDROCARBON LIQUIDS'
This standard is issued under the fixed designation D 1218; the number immediately following the designation indicates the
year of on 'nal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapprova&a superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. scope
1.1 This method covers the measurement of
refractive indexes, accurate to six units in the
fitlh decimal place, and refractive dispersions,
accurate to twelve units in the fifh decimal
place, of transparent and light-colored hydrocarbon
liquids that have refractive indexes in
the range from 1.33 to 1 SO, and at temperatures
from 20 to 3OOC. The method is not applicable
within the accuracy stated to liquids having
colors darker than No. 4 ASTM Color as determined
by Method D 1500, to liquids having
bubble points so near the test temperature that
a reading cannot be obtained before substantial
weathering takes place, to liquids having a
refractive index above 1.50, or to measurements
made at temperatures above 30°C.
NOTE 1-The instrument can be successfully used
for refractive indexes above 1 SO, and at temperatures
both below 2OoC and above 3OoC, but as yet certified
liquid standards for the ranges above a refractive
index of 1.50 are not available, so the precision and
accuracy of the instrument under these conditions
have not been evaluated. Similarly, certified refractive
indexes of liquids at temperatures other than the
20 to 30°C range are not available, although the
instrument can be used up to 5OOC.
2. Applicable Documents
2.1 ASTM Standards:
D 841 Specification for Nitration Grade Toluene2
D 1500 Test Method for ASTM Color of
Petroleum Products (ASTM Color Scale)3
E 1 Specification for ASTM Thermometers4
3. Defmitions
3.1 refructive index-the ratio of the velocity
of light (of specified wavelength) in air, to its
velocity in the substance under examination. It
may also be defined as the sine of the angle of
incidence divided by the sine of the angle of
refraction, as light passes from air into the
substance. This is the relative index of refraction.
If absolute refractive index (that is, referred
to vacuum) is desired, this value should
be multiplied by the factor 1.00027, the absolute
refractive index of air. The numerical value
of refractive index of liquids varies inversely
with both wavelength and temperature.
3.2 refractive dispersion- the difference between
the refractive indexes of a substance for
light of two different wavelengths, both indexes
being measured at the same temperature. For
convenience in calculations, the value of the
daerence thus obtained is usually multiplied
by 10,OOO.
4. Summary of Method
4.1 The refractive index is measured by the
critical angle method with a Bausch & Lomb
Precision Refractometer using monochromatic
light. The instrument is previously adjusted by
means of a solid reference standard and the
observed values are corrected, when necessary,
by a calibration obtained with certified liquid
standards.
This method is under the jurisdiction of ASTM Committee
D-2 on Petroleum Products and Lubricants.
Current edition approved Aug. 27, 1982. Published January
1983. Originally published as D 1218 - 52 T. Last previous
edition D 1218 - 61 (1977).
1983 Annual Book of ASTM Standards, Vol05.03.
1983 Annual Book of ASTM Standards, Vol05.01.
' 1982 Annual Book of ASTM Standards, Parts 25 and 44.
22 1

D 1218
5. Significance and Use
5.1 Refractive index and refractive dispersion
are fundamental physical properties which
can be used in conjunction with other properties
to characterize pure hydrocarbons and their
mixtures.
6. Apparatus
6.1 Refractometer, Bausch & Lomb, “Precision”
type,‘ range 1.33 to 1.64 for the sodium
D line.
6.2 Thermostat and Circulating Pump, capable
of maintaining the indicated prism temperature
constant within 0.02”C of the desired test
temperature. The thermostating liquid should
pass the thermometer on leaving, not on entering,
the prism assembly.
6.3 Thermometer- ASTM Saybolt Viscosity
Thermometer 17C having a range from 19 to
27OC, and conforming to the requirements of
Specification E 1. The thermometer shall be
used in an approved holder,6 as shown in Fig.
1, such that almost total immersion (not more
than emergent stem) is obtained, and reading
to 0.0 1 “C is possible.
6.4 Light Sources-The following light
sources have been found satisfactory:
6.4.1 Sodium Arc Lamp-The Unitized
“Sodium Lab Arc” is furnished with the instrument.
6.4.2 Mercury Arc Lamp-The H-4 type
capillary mercury arc is furnished as an accessory
to the refractometer.
6.4.3 Hydrogen Discharge Lamp-Any type
of lamp capable of producing light having an
intensity of at least 32 Ix (3 footcandles) on an
area of 1 cm2 on the entrance face of the
illuminating prism. The luminous intensity
may be conveniently measured by means of a
photographic light meter held 254 mm (10 in.)
from the !amp asd perpeadicular to the !igh:
beam. For convenience, the lamp should be
mounted on an extension of the sodium lamp
support.
6.4.4 Other Sources-Helium may be used
in place of hydrogen in the lamp discussed in
6.4.3.
6.4.5 Light Filrers-For isolating the various
spectral lines from the above sources, special
light filters are required. The following are
tentatively recommended:
Wave- Spectral
length, Line Filter
A
6678 Helium Coming No. 2404
Y
6563 H, None required. May use Corning ~
No. 2404.
5893 NaD None required
5461 Hg, Wratten No. 62, or No. 77A, Corning
Nos. 3486 + 4303 + 5 120
5016 Helium Wratten No. 45 _
4861 HF Corning Nos. 5030 + 3387,4303, or
Wratten No. 45
4358 Hga Corning Nos. 5 I 13,3389 + 5850.
NOTE 2-In determinations of refractive indexes
above approximately 1.53 (wherever the short wavelengths
show a higher scale reading than the long)
this system of filters is rendered worthless and filters
must be chosen which remove all spectral lines of
shorter wavelength than the one being read. Below
this refractive index, the specific filters listed above,
which remove spectral lines of longer wavelengths
than the one being read, should be used.
7. Solvents
7.1 n-Pentane, 95 mol 96 minimum purity.
(Danger! Extremely flammable. Harmful if inhaled.
Vapors may cause flash fire. See Annex
Al.1.)
7.2 Toluene, conforming to Specification
D 841. (Warning! Flammable. Vapor harmful.
See Annex A1.2.)
8. Reference Standards
8.1 Solid Reference Standard, accurate to
+0.00002 with the value of the refractive index
engraved upon its upper face.
8.2 Primary Liquid Standards-The organic
liquids listed below, with the values of their
refractive indexes for the D, F, and C lines
certified at 20,25, and 30°C, obtained from the
API Standard Reference Office?
2,2,4-Trimethylpentane nD = 1.39
Methy lcyclohexane nD = 1.42
Toluene = 1.49
(Warning! Flammable; see Annex A1.3.)
9. Sample
9.1 A sample of at least 0.5 mL is required.
Manufactured by Bausch & Lomb Optical Co., Rochester,
N. Y., Catalog No. 33-45-03. All instrument terminology
used in this method corresponds with that used in the
“Reference Manual” supplied with the instrument. Production
of this refractometer was discontinuedin 1976. However
it may be obtainable from instrument exchanges or used
equipment suppliers. If other available instrumentation is
used, the precision statements of Section 13 will not apply.
Carnegie-Mellon University, Pittsburgh, Pa.
222

D 1218
The sample shall be free of suspended solids,
water, or other materials that tend to scatter
light. Water may be removed from hydrocarbons
by treatment with calcium chloride followed
by filtering or centrifuging to remove the
desiccant. The possibility of changing the composition
of a sample by action of the drying
agent, by selective adsorption on the filter, or
by fractional evaporation, shall be considered.
(Warning! Volatile hydrocarbon samples are
flammable; see Annex A1.3,)
10. Preparation of Apparatus
10.1 The refractometer shall be kept scrupulously
clean at all times. Dust and oil if
allowed to accumulate on any part of the instrument
will fmd their way into the moving
parts, causing wear and eventual misalignment;
if permitted to collect on the prism, dust will
dull the polish, resulting in hazy lines.
10.2 Thoroughly clean the prism faces with
a swab of surgicai-grade absorbent cotton saturated
with a suitable solvent such as toluene.
Pass the swab very lightly over the surface until
it shows no tendency to streak. Repeat this
procedure with n-pentane until both the glass
and the adjacent polished metal surfaces are
clean. Do not dry the prism faces by rubbing
with dry cotton.
10.3 Adjust the thermostat so that the temperature
indicated by the refractometer thermometer
is within 0.02"C of the desired value;
turn on the sodium vapor lamp and allow it to
warm up 30 min.
NOTE 3-An error of 0.02OC in temperature of
the sample will cause an error of 1 X IOv6 in the
refractive index of methylcyclohexane.
10.4 Control the ambient temperature
within 1 OC of the test temperature. This can be
done by regulation of the room temperature or
by placing the instrument inside a specially
designed constant-temperature box. The instrument
shall also be so situated that it will
not be subject to drafts.
11. Standardization of Apparatus and Technique
11.1 Thoroughly clean the prism faces and
surfaces of the solid reference standard as described
in 10.2, finally brushing the surfaces
with a clean camel's-hair brush. Fix the hinged
part in a wide-open position. Apply a drop of
monobromonaphthalene, about 1.5 mm in di-
ameter, to the center of the polished surface of
the reference standard. Press the reference
standard against the surface of the stationary
prism with the polished end toward the light.
If the proper amount of contacting liquid has
been used, a continuous film of liquid will form
between the prism and the reference standard,
and the field will appear evenly illuminated. If
not, irregular dark spots will appear in the
illuminated field of the telescope when the
knurled knob is turned and the light is in line
with the longitudinal axis of the telescope.
Gently manipulate the reference standard by
pressure on one edge or another until the interference
bands, as seen with the aid of the
auxiliary lens, appear to extend horizontally in
the rectangular contact area. It is well to keep
the liquid wedge at such an angle that three to
five bands can be seen, and the fringe pattern
should appear centered in the exit pupil of the
telescope.
NOTE &-If there is any trace of roughness as the
contact is being made, remove the reference standard
and clean all surfaces again. More damage can be
done to the prism surface in this operation than in
weeks of use with liquids, if grit comes between the
two surfaces during this contact. The amount of
liquid should be just enough to fill the contact area
completely, leaving no liquid at the front edge of the
reference standard.
11.2 Set the instrument to the scale reading
corresponding to the refractive index engraved
on the solid reference standard. Rotate the
sodium lamp base while viewing the telescope
until a sharp vertical line appears in the illuminated
field and does not move with the
rotation of the lamp. Adjust the eyepiece of the
telescope to bring the cross hairs into sharp
focus.
11.3 Move the alidade by means of the hand
wheel until the critical line on the left side of
the band intersects the cross hairs, and read the
scale. Repeat the setting at least twice and,
between settings, shift the lamp slightly while
observing the critical line in order to make sure
a false line is not being observed. Average the
scale readings for all the settings.
11.4 Convert the average scale reading to
refractive index by means of the table for the
sodium D line. To give correct readings, without
application of corrections, the average
value obtained may differ from that engraved
on the test specimen by more than 0.00002.
11.5 If adjustment is necessary, set the scale
223

D 1218
to the reading corresponding to the value engraved
on the solid reference standard, by
means of the hand wheel on the side of the
instrument. If the critical line is to the left of
the intersection of the cross hairs, loosen the
small screw on the left of the telescope and
slowly tighten the one on the right until the
lines coincide; if the critical line is to the right
of the intersection, use the opposite procedure.
At the fmal adjustment both screws should be
snug but not tight. Again check the setting as
in 11.3.
12. Standardization with Reference Liquids
12.1 Measure the refractive indexes of each
of the primary liquid standards listed in 8.2 for
the D, F, and C lines, at the test temperature
20, 25, or 3OoC, following the procedure described
in Section 13. If the values obtained do
not agree with the certified values within
O.ooOo3, determine a correction curve for each
wavelength from an average of five independent
determinations on each of the three certified
liquid standards. A plot of the average error
against refractive index provides a correction
for all observed indexes between these points.
NOTE 5-This does not imply that the refractive
index engraved on the test specimen is necessarily
inaccurate, but tends to correct an error introduced
in the determination by the failure to obtain grazing
incidence in the case of liquid samples. This fault,
and other instrumental errors, if present, are inherent
in the refractomer design and their magnitude varies
with the refractive index of the liquid and different
instruments.
12.2 To observe any changes with time and
use in the relative positions of prism and alidade,
each operator shall check the instrument
with the calibrated solid reference standard
prior to his use of the instrument.
13. Procedure
13.1 Thoroughly clean the prism faces as
described in 10.2. Adjust the thermostat so that
the temperature indicated by the refractometer
thermometer is within 0.02"C of the desired
value.
13.2 In testing nonviscous liquid samples,
close the prism box and let stand for 4 to 5 min
to ensure temperature equilibrium between the
prisms and the circulating water. By means of
a small pipet or medicine dropper, introduce a
small quantity of sample into the tubulation
between the prism faces. Turn the knurled head
at the base of the telescope so as to bring the
auxiliary lens into the light path, and observe
through the face of the working prism. If the
space between the prisms is completely filled
with liquid, the field will be uniformly illuminated;
bubbles or unfdled spaces will appear
black. If the space is not completely filled, open
the prism box slightly several times and add
more liquid. Do not attempt to measure refractive
indexes until the space between the prisms
is completely fdled.
13.3 In testing viscous liquids, open the
prism box and apply the sample to the faces of
both prisms, spreading evenly with a round
wooden applicator stick. Never use metal or
glass for this purpose as these may scratch the
prism faces. Close the prism box slowly to avoid
straining the hinge and locking mechanism.
13.4 Adjust the illuminant to be in line with
the telescope and bring the border line approximately
to the reticle. While viewing the rear
prism face by means of the auxiliary lens, rotate
the lamp bracket to the right until only the
extreme left side of the prism appears to be
illuminated. If this rotation is camed too far,
vertical interference lines will appear in the
back face. These are generally irregular and
rather faint. The best adjustment for contrast
and illumination seems to be the point just
before these fringes become distinct.
13.5 Adjust the eyepiece of the telescope so
as to bring the cross hairs into sharp focus, set
the cross hairs on the critical edge and read the
scale of the instrument. Readjust the position
of the vapor lamp and repeat at least four times,
approaching from either side of the critical
edge, and record the average scale reading. (In
order to avoid the possibility of using a false
edge, it is best to adjust the position of the light
source each time a setting is made rather than
make four settings on one positioning of the
lamp.)
13.6 Without changing the position of the
prism assembly, place other desired light
sources into the angular position (with respect
to the rear face of the refracting prism) occupied
by the sodium lamp. Take average scale
readings for the desired lines in the manner
described in 13.4.
13.7 In testing volatile samples, clean the
prism faces without changing the position of
224

D 1218
the prism assembly or the lamp, recharge with
sample, and read immediately.
14. Calculation and Report
14.1 Convert the observed scale readings to
refractive indexes by use of the tables supplied
with the instrument and report these values and
the temperature at which the test was made,
distinguishing between the various spectral
lines used (for example, “ n ~ = 1.. -” or
66 1
n5 8 9 3 = 1. *”).
14.2 To obtain refractive dispersion, subtract,
nxz and nx,. Report the result and the
temperature at which the test was made (for
example “(nF - nc) x lo4 at t = * a” or “(ng
- no) x io4 at t = -”).
15. Precision and Accuracy
15.1 Results should not differ from the mean
by more than the following amounts:
Reproducibility
Repeatability Different Opera-
One Operator tors and Apand
Apparatus paratus
Refractive index 0.00006 0.00006
Refractive dispersion 0.000 I2 0.000 I2
15.2 Results should not differ from the true
value by more than the following amounts:
Accuracy
Refractive index 0.00006
Refractive dispersion
0.000 I2
NOTE 6-The Drecision for this method was not
obtained in accordance with RR:DO2- 1007.
L---
FIG. 1 Themmeter Holder
225

ANNEX
(Mandatory Information)
Al. PRECAUTIONARY STATEMENTS
Al.1 n-Pentane
Danger-Extremely flammable.
Harmful if inhaled. Vapors may cause flash fire.
Keep away from heat, sparks, and open flame.
Keep container closed.
Use with adequate ventilation.
Avoid buildup of vapors and eliminate all sources
of ignition, especially nonexplosion-proof electrical
apparatus and heaters.
Avoid prolonged breathing of vapor or spray mist.
Avoid prolonged or repeated skin contact.
A1.2 Toluene
Warning-Flammable. Vapor harmful.
Keep away from heat, sparks, and open flame.
Keep container closed.
Use with adequate ventilation.
bvoid breathing of vapor or spray mist.
Avoid prolonged or repeated contact with skin.
A1.3 Flammable Liquid
Warning- Flammable.
Keep away from heat, sparks, and open flame.
Keep container closed.
Use only with adequate ventilation.
Avoid prolonged breathing of vapor or spray mist.
Avoid prolonged or repeated contact with skin.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in
connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity
of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyfive years
and f not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive cireful consideration at a meeting of the
responsible technical commitree, which you may attend. If you feel that your comments have not received a fair hearing you should
makeyour views known to the ASTM Committee on Standards, I916 Race S!., Philadelphia, Pa. 19103,
226

ab
Designation: D 1259 - 85
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 49103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appeaf in the next edition.
Standard Test Methods for
NONVOLATILE CONTENT OF RESIN SOLUTIONS'
This standard is issued under the fixed designation D 1259; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 These test methods cover the determination
of nonvolatile content of solutions of resins
in volatile organic solvents.
1.2 Two methods are included as follows:
1.2.1 Method A-For solutions of nonheatreactive
resins. These solutions contain resins
that remain stable and release the solvent under
conditions of the test. Examples are ester gums
and alkyds.
1.2.2 Method B-For two types of solutions:
1.2.2.1 Solutions of heat-reactive resins. These
solutions contain resins that undergo condensation
or other reactions under the influence of
heat. Examples include the formaldehyde reaction
products of urea, melamine, and phenols,
and
1.2.2.2 Solutions that release solvent slowly.
Examples include epoxy resin solutions.
1.3 Methods A and B differ primarily in the
drying times and types of oven used.
1.4 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health practices
and determine the applicability of regulatory limiiaiions
p ~ i to ~ tlse. r
2. Summary of Methods
2.1 In both methods, a weighed specimen of
resin solution is spread under pressure between
two weighed sheets of aluminum or tin foil. The
coated foil sheets are separated and then dried.
The weight of residue is determined and the
nonvolatile content is calculated. The method is
unique in that it provides for drying of a very
thin film of resin, thus minimizing chances for
volatiles to be trapped and held during the heating
operation.
2.2 Either a gravity-convection or a forcedventilation
oven and a 30-min heating period at
105'C are used in Method A.
2.3 A forced-ventilation oven and a 2-h heating
period at 105°C are used in Method B.
3. Significance and Use
3.1 The nonvolatile content of resin solutions
is useful to coatings producers and users for the
determination of the total solids available for film
formation and for the estimation of the volatile
organic content.
METHOD A-NON-HEAT-REACTIVE
SOLUTIONS
RESIN-
4. Apparatus
4.1 Ovens:
4.1.1 Gravity-convection type, maintained at
105 f 2"C, with vents open.
4.1.2 Forced-ventilation type, maintained at
105 & 2°C. For ovens with adjustable air flow
rate, set the control damper at 50 %.
4.2 Aluminum or Tin Foil,2 from 0.0015 to
' These lesi methods zie under :he jurisdicricx of ASTM
Committee D-1 on Paint and Related Coatings and Materials
and are the direct responsibility of Subcommittee DO1.21 on
Paints and Paint Materials.
Current edition approved Nov. 29, 1985. Published January
1986. Originally published as D 1259 - 53. Last previousedition
D 1259-61 (1980)".
'Aluminum foil available from Thomas Scientific Co., P.O.
Box 99, Swedesboro, NJ 08085; or from Sargent and Welch
Scientific Co., 7300 North Linder Ave., Skokie, IL 60077 has
been found satisfactory.
Tin foil available from J. T. Baker Co., North Broad St.,
North Philipsburg, NJ 08865 has been found satisfactory.
227

~
0.0020 in. (38 to 50 pm) in thickness. Either one
piece 6 by 12 in. ( 150 by 300 mm), or two 6 by
6-in. (150 by 150-mm) pieces may be used. The
foil must be perfectly smooth; if it becomes wrinkled
during the initial handling, roll smooth as
directed in 5.2.
4.3 Plate Glass-Two pieces about 3/16 in. (5
mm) thick; one piece 5% by 5% in. (140 by 140
mm) and one piece 7 by 7 in. (1 80 by 180 mm).
4.4 Device for Weighing Specimens3-Apparatus
that will prevent loss of volatile matter
during the weighing operation such as any of the
following, or equivalent:
4.4.1 Syringe, Luer, 2 or 5-mL capacity,
4.4.2 Weighing Buret, Smith, 1 0-mL capacity,
or
4.4.3 Bulb Pipet, dropping, with 50-mL Erlenmeyer
flask.
4.5 Roller, for Smoothing Foil-Use a ground
and polished cylinder, preferably stainless steel,
approximately 7 in. ( 180 mm) long and 2 in. (50
mm) in diameter.
4.6 Foil Trays, two types as follows:
4.6.1 Trays measuring 6% by 12 in. (165 by
300 mm), for use with 6 by 12-in. foil, constructed
from No. 22-gage (0.6 mm) aluminum
sheet in accordance with dimensions shown in
Fig. 1. Several trays may be stacked in the oven
to permit running several specimens simultaneously.
4.6.2 Trays measuring 6l/2 by 6% in. (165 by
165 mm), for use with 6 by 6-in. foil, with holder,
shall be constructed from No. 22-gage aluminum
sheet, as shown in Fig. 2.
5. Procedure
5.1 Use the following procedure with the 6 by
12-in. foil sheets and the 6% by 12-in. trays.
Alternatively two 6 by 6-in. foil sheets may be
used in a similar manner with the 6% by 6Y2-h.
trays. In handling the foil, avoid wrinkling or
creasing the sheets until after the specimen has
been dried. Sheets may be rolled for convenience
of handling and making the initial weighing, but
must be kept smooth throughout the pressing
and drying operations.
5.2 Weigh the foil to 0.1 mg. Open and place
half the foil, with the shiny side up, on the 7 by
7-in. glass plate. If necessary, roll smooth with
the metal roller. By means of the weighing device,
weigh by difference a 0.9 to 1.1-g specimen of
the resin solution, to 0.1 mg. Place the specimen
D 1259
on the center of that area of the foil covering the
glass plate. Place the other half of the foil on top.
Covej the foil with the second glass plate, centering
the glass on the foil, and press down suficiently
to cause the specimen to spread uniformly
into a thin film, about 3 in. (75 mm) in diameter.
The pressure that must be exerted depends on
the viscosity of the sample. In case a specimen of
low viscosity should extend beyond the edge of
the foil, repeat the determination, allowing a few
minutes for a portion of the solvent to evaporate
from the weighed specimen before covering and
pressing it.
5.3 After pressing, open the foil to its full
length and place it in the foil tray. Place the tray
in either a gravity-convection or a forced-ventilation
oven at 105 & 2°C for 30 min.
5.4 Remove the tray from the oven and then
carefully remove the foil sheet from the tray.
Return the dried film surfaces to the face-to-face
position. While the foil is still warm, fold the
edges together to enclose completely the dried
film. Without undue delay, weigh to 0.1 mg.
6. Calculation
6.1 Calculate the nonvolatile content as follows:
Nonvolatile content, % = [(A - B) x lOO]/S
where:
A = weight of foil plus dried solids, g,
B = weight of foil, g, and
S = weight of sample taken, g.
7. Precision and Bias
7.1 The following criteria should be used for
judging the acceptability of results at the 95 %
confidence level:
7.1.1 Repeatability-The difference between
two results, each the mean of duplicate determinations
obtained by the same analyst is normally
ahnut 02 %, abso!u?e. Two such resu!?s should
be considered suspect if they differ by more than
0.5 %, absolute.
7.1.2 Reproducibility-The difference between
two results, each the mean of duplicate
determinations, obtained by analysts in different
laboratories is normally about 0.4 %, absolute.
A Smith weighing buret is available from Ace Glass Co.,
1430 Northwest Blvd., Vineland, NJ 08360. The bulb pipet is
available from Thomas Scientific Co., P.O. Box 99, Swedesboro,
NJ 08085 or from Fisher Scientific Co., 52 Fadem Rd., Springfield,
NJ 0708 1.
228

D 1259
Two such results should be considered suspect if
they differ by more than 1 .O %, absolute.
7.1.3 No bias has been determined for these
test methods.
METHOD B-HEAT-REACTIVE RESIN
SOLUTIONS AND SOLUTIONS THAT
RELEASE SOLVENT SLOWLY
8. Apparatus
8.1 Oven-Forced-ventilation type, maintained
at 105 f 2°C. For ovens with adjustable
air flow rate, set the control damper at 50 %.
8.2 The remainder of the apparatus is identical
with that given in 4.2 to 4.6.
9. Procedure
9.1 Weigh the specimen of resin solution and
press it between two sheets of foil as described in
5.1 and 5.2.
9.2 After pressing, open the foil to its full
length and place it in the foil tray. Then place
the tray in a forced-ventilation oven at 105 f
2°C for 2 h. When using 6'/2 by 6'/2-in. trays and
holder, place the assembly in the oven with the
open ends perpendicular to the direction of air
flow.
9.3 Complete the determination as described
in 5.4.
10. Calculation
10.1 Calculate the nonvoiatile content as described
in Section 6.
11. Precision and Bias
1 1.1 The following criteria should be used for
judging the acceptability of results at the 95 %
confidence level.
1 1.1.1 For Heat-Reactive Resin Solutions:
1 1.1.1.1 Repeatability-The difference between
two results, each the mean of duplicate
determinations, obtained by the same analyst is
normally about 0.3 %, absolute. Two such results
should be considered suspect if they differ by
more than 0.7 %, absolute.
1 1.1.1.2 Reproducibility-The difference between
two results, each the mean of duplicate
determinations, obtained by analysts in different
laboratories is normally about 0.7 %, absolute.
Two such results should be considered suspect if
they differ by more than 1.7 %, absolute.
1 1.1.1.3 No bias has been determined for this
test method.
1 1.1.2 For Solutions that Release Solvent
Slowly:
1 1.1.2.1 Repeatability-The average difference
between two results each the average of
duplicate determinations, obtained by the same
analyst is normally about 0.1 %, absolute. Two
such results should be considered suspect if they
differ by more than 0.3 %, absolute.
1 1.1.2.2 Reproducibility-The average difference
between two results obtained by analysts in
different laboratories will approximate 0.2 %.
Two such results should be considered suspect if
they differ by more than 0.5 %, absolute.
1 1.1.2.3 No bias has been determined for
these test methods.
229

D1259
Material: 22-Gage Aluminum
Sheet
1"
To Align with Pins
5Diam Holes
an I" Centers
~ d o o o o o o o o o o
1 %
_tl
U JJ T-
/
Pin, 2'' Diam
32
$ Long, 4 Req'd
NOTE-Millimetre dimensions appear in section on Apparatus.
FIG. 1 Tray for 6 by 12-in. Foil
230

FIG. 2 Trays and Holder for 6 by 6-in. Foil
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
nith any item mentioned in this standard. Users ofthis standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyfwe years and
not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed IO ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee. which you may attend. lf you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia. PA 19103.

dub
Designation: D 1308 - 79 (Reapproved 1981 )r’
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method For
EFFECT OF HOUSEHOLD CHEMICALS ON CLEAR AND
PIGMENTED ORGANIC FINISHES’
This standard is issued under the fixed designation D 1308; the number immediately following the designation indicates the
year of ori ‘nal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapprovafA superscript epsilon (E) indicates an editorial change since the last revision or reapproval.
This’method has been approved for use by agencies of the Department of Defense to replace Method 6011,6081 of Federal Test
Method Standard No. 141A and for listing in the DoD index of Specificationsand Standards.
~ ~~
“NoTE--Editorial changes were made throughout in August 1981.
1. scope
1.1 This method covers determination of the
effect of household chemicals on clear and
pigmented organic finishes, resulting in any
objectionable alteration in the surface, such as
discoloration, change in gloss, blistering,
softening, swelling, loss of adhesion, or special
phenomena.
2. Applicable Document
2.1 ASTM Standard
D 609 Preparation of Steel Panels for Testing
Paint Varnish, Lacquer, and Related Products*
3. Summary of Method
3.1 Three methods, each of which is particularly
applicable to individual reagents under
study, are described as follows:
3.1.1 Spot Test, Covered-The reagent is
placed on the test surface and immediately
covered with a watch glass.
3.1.2 Spot Test, Open-The test surface is
subjected directly to the effect of substance,
such as citrus fruit, oils, greases, beverages, etc.
3.1.3 Immersion Test-A suitably prepared
panel is immersed in the test reagent.
4. Test Panels
4.1 Steel Panels-See Section 4 of Method
D 609.
4.2 Other Metal Panels, as agreed upon by
the purchaser and the seller of the finish being
tested.
5. Reagents
5.1 The choice of reagent shall be governed
by ultimate coating use and by agreement between
the purchaser and the seller of the finish
being tested. The following reagents are sug-
gested:
5.1.1
5.1.2
5.1.3
5.1.4
5.1.5
5.1.6
5.1.7
5.1.8
5.1.9
agents.
Distilled Water, cold.
Distilled Water, hot.
Ethyl Alcohol (50 5% volume).
Vinegar (3 96 acetic acid).
Alkali Solution.
Acid Solution.
Soap Solution.
Detergent Solution.
Lighter Fluid and Other Volatile Re-
5.1.10 Fruit-Piece of cut fruit, with cut portion
placed face down on panel for time agreed
upon between the purchaser and the seller.
5.1.1 1 Oils and Fats-Butter, margarine,
lard, shortening, vegetable oils, etc.
5.1.12 Condiments-Mustard, catsup.
5.1.13 Beverages-Coffee, tea, cocoa.
5.1.14 Lubricating Oils and Greases.
5.1.15 Other Reagents, as agreed upon between
the purchaser and the seller.
’ This method is under the jurisdiction of ASTM Committee
D-I on Paint and Related Coatings and Materials and
is the direct responsibility of Subcommittee D01.55 on Factory-Applied
Coatings on Preformed Products.
Current edition approved May 25, 1979. Published July
1979. Originally published as D 1308-54T. Last previous
edition D 1308-57 (1978).
Annual Book of ASTM Standards, Part 21.
232

Dl308
6. Procedure
6.1 Panel Preparation-Spot and direct a p
plication tests may be carried out on the fabricated
article coated with the finishing system
under evaluation, if sufficient plane surface is
available. For immersion tests and tests where
the fmished article is not available, select panels
in accordance with Method D 609, or prepare
special metal panels according to agreement
between the purchaser and the seller of the
finish. Apply the fmish according to the method
and the schedule prescribed by the user of the
lacquer. This schedule includes number of
coats, frlm thickness, and other features. Allow
the finished panels to age 1 week at normal
room conditions, about 77°F (25°C) and 50 %
relative humidity, before testing.
6.2 Spot Test, Covered-Conduct the test at
73.5 * 3.5"F (23 k 2°C) and 50 f 5 % relative
humidity, or as agreed upon between the purchaser
and the seller. Using a 5-mL pipet graduated
in 0.1 mL, pipet onto the horizontal panel
1 mL of the reagents listed in Section 4 and
immediately cover with a watch glass. After an
interval agreed upon by the purchaser and the
seller, wipe the spot clean and examine immediately
for effects as listed in Section 1. Frequently
used intervals are 15 min, 1 h, and 16
h, or by agreement between the producer and
the user. If desired, allow the panel to recover
for a specified period, and examine for return
of original properties.
6.3 Spot Test, Open-Conduct the test at
73.5 f 3.5"F (23 f 2°C) and 50 f 5 % relative
humidity, or as agreed upon between the purchaser
and the seller. Place a small portion of
the reagent on a horizontal panel or surface,
with the exception of fruit juices, as mentioned
in 5.4.10. After a time interval, as agreed upon
between the purchaser and the seller, wipe the
spot clean and examine immediately for effects
as listed in Section 1. Frequently used inmvals
are 15 min, 1 4 and 16 4 or by agreement
between the producer and the user. If desired,
allow the panel to recover for a specified period
and examine for return of original properties.
6.4 Imersion-Immerse panels to a depth
of 50% in the specified reagents (5.1.1, 5.1.2,
5.1.5,5.1.6, 5.1.7, and 5.1.8) contained in beakers,
at a temperature and length of time agreed
upon between the purchaser and the seller.
Withdraw the panels, wash with distilled water,
and examine immediately for any of the effects
listed in Section 1. If desired, allow the panels
to recover for a specified period and examine
for return of the original properties. In general,
it will not be necessary to seal the edges of the
applied film. If the reagent effect is noted only
around the panel edges, the test should be
repeated using a suitable edge sealer. When
sealing of edges is required, the selection of the
sealer should be a matter of agreement between
the purchaser and the seller.
7. Report
7.1 The report shall include the following:
7.1.1 The system and the testing method
employed. The test conditions are an important
factor in the results obtained and, therefore,
should be defined in the report.
7.1.2 The type of the effect, if any (see Section
1).
a Precision
8.1 This test is designed to provide a working
procedure for examination of the effect of
household chemicals on clear and pigmented
organic finishes. The effects will be in terms of
appearance, and numerical values are assigned
ifa rating scale is used. No statement of precision,
therefore, can be made.
Tkc Ameiicmi Society for Testing and Materials taka ne position respecting ?he validity of any patent rights asserted LT
connection with any item mentioned in this stanaiud Users of this st&d die express+ advised that determination of rhe validity
of any such patent rights, and the risk of thfdgement of such rights, are entirely their own responsibiliy.
This stahrd is subject to revision at any time by the responsible technical commiltee and must be reviewed every five yean
and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this stanaiud or for oddtional
standards and should be &essed to ASTM Headpmers. Your comments will receive carejul coderation at a meetmg of the
responsible technical committee, which you may attend rfvou feel that your comments have not received a fair hearing you should
make your views known to the ASTM Commiltee on Stanaiud~, 1916 Race St., Philaahphio. Pa 19103. which will schedule a
further hearing regarding your comments. Failing satifaction there. you may appeal to the ASTM Board of Directors.
233

AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
A Reprint from Copyrighted ASTM Publications
Standard Method of Test for
FINENESS OF GRIND OF PRINTING INKS BY THE
PRODUCTION GRINDOMETER1
Scope
ASTM Designation : D 13 16 - 68 R 7 9
This Standard of the American Society for Testing and Materials is issued under
the fixed designation D 1316; the number immediately following the designation
indicates the year of original adoption or, in the case of revision, the year
of last revision. A number in parentheses indicates the year of last reapproval.
Samples
1. This method for determining the 4. When taking samples either from
fineness of grind of printing inks is a container or from the apron of a mill,
applicable to all pigmented inks with push aside the top layer and take the
vehicles which are essentially non- sample from below. This technique prevolatile
at room temperature and when vents any dust that may have settled on
the dispersion is fine enough to fall with- the surface from being transferred to the
in the range of the specified instrument. gage.
Deiinition
2. Fineness of Grind of a printing ink
is a measure of the size and prevalence
of oversize particles in the ink.
Apparatus
3. (a) Production Grindometer,2 with
Adco Scraper.
(b) Small Ink Kni'je.
(c) Lint-Free Rag and Sdvml, €GT
cleaning.
Under the standardiiation procedure of
the Society, this method is under the jurisdiction
of the ASTM Committee D-1 on Paint,
Varnish, Lacquer, and Related Products.
Current edition accepted Sept. 13, 1968. Originally
issued 1954. Replaces D 1316 - 54 T.
' The Production Grindometer. developed
by the National Printing Ink Research Institute,
may be obtained from the Precision Gage and
Tool Co., Dayton, Ohio.
Preparation and Standardization of
Apparatus
5. For a grindometer to function
properly, the following conditions must
be fulfilled:
(a) The scraper and the block must
be perfectly clean. Any dirt or lint
present will produce a scratch and
interfere with the readings.
(b) The scraper must wipe the center
and side areas clean. If these areas are
not wiped clean, the clearances between
the scraper and the bottoms of the paths
will not be correct (Note 1).
(c) Both the scraper and the block
must be dimensionally perfect. Proper
Derformance of "
hependent upon its dimensions
accurate within thirty millionths
the grindometer is
being
of an
10-68
30-11
234

FINENESS OP GRIND OF PRINTING INKS BY GRINDOMETER (D 1316)
inch. Deviations greater than this from
the specified groove depths or in the
linearity of the blade will produce readable
errors in the results (Note 1).
NOTE 1.-During the work on grindometers
at the National Printing Ink Research Institute,
a number of these imperfections have been observed.
They may be most readiy classified according
to their causes: warping of the parts,
normal wear, misuse, and rusting, as follows:
Warping has been noted in several of the
Institute's grindometer blocks. It is first indicated
by an inability to wipe clean either the
center or one of the sides of the block. In the
latter case there is also difficulty in getting
agreement between the readings from the two
paths. Warping is frequently caused by unrelieved
strains in the steel, and can be corrected
only by returning the instrument to the factory
for reannealing and regrinding. No scraper
warpage has been found to date.
NO" Wear.-Under steady usage over an
extended period of time, both scraper and block
will wear, but scraper wear is much more rapid
than block wear. Scraper wear can be checked
from time to time by repeating a drawdown,
using a new scraper. If the same reading is obtained
as with the first scraper blade, there has
been no appreciable blade wear. It is advisable
to keep a new scraper on hand for checking the
one in use. This extra scraper can then be put
into use when the first is returned to the factory
for refinishing. The refinished scraper can be
held in reserve for future checking. Each blade
of an Adco scraper should last for about two
months with steady use, and a block should last
for several years under these conditions.
Misuse will, of course, reduce the life of the
grindometer. The misuses usually encountered
are mechanical, such as chipping of the blade or
denting of the block. Such misuses involve
rather drastic treatment, and show up immediately
when the instrument is used.
Rusling.-The grindometer is made of carbon
steel and is subject to rusting; it is therefore
important that a coating of a rust-preventive be
kept on the gage when it is not in use.
No difficulty will be encountered if the above
points are recognized and a little care taken.
The Production Grindometer is a precision instrument
and must be treated as such.
Procedure
6. (a) Thoroughly clean the block
and scraper to assure perfect cleanliness
and freedom from dust and lint, or from
grease in which the instrument was
packed. The most effective cleaner is a
lint-free rag with a volatile solvent
such as mineral spirits or carbon tetrachloride.
(b) Place the samples of ink across the
deep end of the grooves about in.
from the end of the block. Approximately
0.5 ml of ink is suf?icient for a path
1 in. wide.
(c) Grasp the scraper in both hands
in a nearly vertical position and draw
down the ink on the block. Make the
drawdown by a smooth, steady stroke
that takes 7 to 10 sec to complete.
(d) Determine grittiness of the ink
films, as described in Section 7. Repeat
the entire procedure at least two more
times. If a reference standard is used in
one path for comparison, alternate its
position from side to side on the repeat
tests.
Calculation and Report
7. Determine and report the grittiness
of the ink by examination of the
scratches appearing in the ink films
(Note 2). A number of methods have
been suggested for the conversion of a
scratch pattern into a simple numerical
result (Note 3) but the following one
is simple and adequate:
(a) Find the first point at which there
are as many as four scratches, and read
off this point to the nearest half division
on the scale at the left of the gage block.
(b) Take a second reading at the point
at which there are as many as ten
scratches. The two figures thus obtained
are indicative of the grittiness of the Ira
in the path examined. The higher they
are, the grittier the ink; and the greater
the difference between them, the broader
the size-range of the largest particles.
NOTE 2.4n some quarters there is a preference
for examining the speckles which appear
on the surface of the drawdown due to protruding
pigment particle. These speckles always
30-53
235

FINENESS OF GRIND OF PRINTING INKS BY GRINDOMETER (D 1316)
appear at a greater path depth than do the
scrrtchcs. However, it is frequently difficult to
obtain agreement between operators on speckle
readings without a carefully set-up series of
standards (3);* and no such set of standards
has yet gained broad acceptance.
NOTE 3.-A preferred scale for reporting the
grittiness of an ink, or the fineness of grind, is in
microns. The approximate relationship between
a The boldface numbers in parentheses refer
to the references listed at the end of this method.
other scales and microns is shown in the following
example:
Depth of Groove, P
26 ...............
20 ...............
16 ...............
10 ...............
6 ...............
0 ...............
a To nearest tenth.
Depth of I NF’IRI
G ~ mils~ ~ Scalea ~ ~ ,
1 .o
0.8
0.6
0.4
0.2
0
9.8
7.9
6.9
2.9
2.0
0
REFERENCES
(1) W. C. Walker and A. C. Zettlemoyer, “The Ink Maker, Vol. 28, No. 7, pp. 31-34, 55,
NPIRI Production Grindometer,” American 57 (1950).
In& Maker, Vol. 27, No. 9, pp. 67-69, 93 (3) D. Doubleday and A. Barkman, “Reading
(1949). the Hegman Grind Gage,” OfiiuZ Digmi,
(2) W. C. Walker and A. C. Zettlemoyer, Federation of Paint and Varnish Production
“Grindometer Fundamentals,” Amaican Clubs, No. 307, August, 1950, pp. 598608.
236

Designation: D 1331 - 56 (Reapproved 1980)''
Reapproved
without change in
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. .19103
Reprinted from the Annual Book of AS7'WI Standards, Copyright ASTM
If not listed in-the current combined index, will appeai in the next edition.
Standard Test Methods for
SURFACE AND INTERFACIAL TENSION OF SOLUTIONS OF
SURFACE-ACTIVE AGENTS'
This standard is issued under the fixed designation D 1331; the number immediHtely following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon ( E) indicates an editorial change since the last revision or reapproval.
NoTE--Section 2 was added editorially and subsequent d ons renumbered May 1985.
1. scope
1.1 These test methods cover the determination
of surface tension and interfacial tension of
solutions of surface-active agents, as defined in
Definitions D 459. Two methods are covered as
follows:
Method A-Surface Tension.
Method B-Interfacial Tension.
1.2 Method A is written primarily to cover
aqueous solutions of surface-active agents, but is
also applicable to nonaqueous solutions and
mixed solvent solutions.
1.3 Method B is applicable to two-phase solutions.
More than one solute component may
be present, including solute components that are
not in themselves surface-active.
2. Applicable Document
2.1 ASTM Standard:
D 459 Definitions of Terms Relating to Soaps
and Other Detergents'
3. Apparatus
3.1 Tensiometer-Either the du Nouy precision
tensiometer or the du Nouy interfacial tensiometer,
equipped with either the 4 or the 6-cm
circumference platinum ring, as furnished by the
manufacturer, may be used. The tensiometer
shall be placed on a sturdy support that is free
from vibrations and other disturbances such as
wind, sunlight, and heat. The wire of the ring
shall be in one plane, free of bends or irregularities,
and circular. When set in the instrument,
the plane of the ring shall be horizontal, that is,
parallel to the surface plane of the liquid being
tested.
3.2 Sample Container-The vessel for holding
the liquid shall be not less than 6 cm in diameter,
and sufficiently large to ensure that the contact
angle between the ring and the interface is zero.
4. Preparation of Apparatus
4.1 Clean all glassware thoroughly. The use of
fresh chromic-sulfuric acid cleaning mixture, followed
by a thorough rinsing in distilled water. is
recommended.
4.2 Clean the platinum ring by rinsing thoroughly
in a suitable solvent and in distilled water,
before taking a set of measurements. Allow the
ring to dry, and then heat to white heat in the
oxidizing portion of a gas flame.
5. Calibration of Apparatus
5.1 The tensiometer is, in fact, a torsion balance,
and the absolute accuracy depends on the
length of the torsion arm, which is adjustable.
Torsion may be applied to the wire by means of
either the dial-adjusting screw (which controls
the dial reading) or a rear adjusting screw. Calibration
consists essentidly in adjusting the iength
of the torsion arm so that the dial scale will read
directly in dynes per centimetre. The precision
tensiometer shall be calibrated in accordance
' These methods are under the jurisdiction of ASTM Committee
D12 on Soaps and Other Detergents and is the direct
Responsibility of Subcommittee D 12.15 on Physical Testing.
Cumnt edition approved Sept. 10, 1956. Published November
1956. Originally published as D 1331 - 54 T. Last previous
editionsD 1331-54T.
Annual Book of ASTM Standards, Vol 15.04
237

~
with the following: 5.1.1 to 5.1.3; the interfacial
tensiometer shall be calibrated in accordance
with 5.1.1 to 5.1.4.
5.1.1 Level the tensiometer. A liquid level of
the type employed on analytical balances may be
used. Place the level on the table that holds the
sample for testing, and adjust the leg screws of
the tensiometer until the table is horizontal. Pull
the torsion wire taut by means of the tension
screw, and adjust the dial reading and the vernier
to zero. Insert the platinum ring in the holder,
and place a small piece of paper across the ring.
This will serve as a platform to hold the calibrating
weight. Turn the rear adjusting screw of the
torsion wire until the index level of the arm is
opposite the reference line of the mirror; this
automatically compensates for the weight of the
paper platform. Next, place an accurately standardized
weight of between 500 and 800 mg on
the paper platform and turn the dial-adjusting
screw until the index level of the arm is opposite
the reference line of the mirror. Record the dial
reading to 0.10 divison. Call this “gamma-c.”
5.1.2 Calculate what the reading “gamma-c”
obtained in 5.1.1 should be when the tensiometer
is properly adjusted, as follows (Note 1):
Yc = (M x g112L
where:
M = weight placed on the paper platform, g,
g = gravity constant (Note 2), cgs units, and
L = mean circumference of the ring (furnished
by the manufacturer with each ring).
If the recorded dial reading “gamma-c” is greater
than the calculated value, the torsion arm should
be shortened. If “gamma-c” is less than the calculated
value, the torsion arm should be
lengthened. Repeat the calibration procedure,
readjusting the zero position after each change in
the length of the torsion arm, until the dial
reading agrees with the calculated value. Each
unit of the sale now represents a puii on the ring
of 1 dyne/cm. Note that a conversion factor, F
(see 5. I .3), must be multiplied by the scale reading
to give corrected surface tension in dynes per
centimetre.
NOTE 1 Example-If M is exactly 0.600 g and L is
4.00 cm:
ye = (0.600 x 980.3)/(2 x 4.00) = 73.52 dynes/cm
NOTE 2-The gravity constant is 980.3 at Chicago;
in other localities it will differ very slightly from this
value.
D1331
5.1.3 After the tensiometer has been calibrated,
it is convenient to calculate the number
of grams total pull on the ring that is represented
by each scale divison. This is done simply by
dividing the scale reading into the weight used
for calibration (Note 3). This value is used in the
calculation of the conversion factor, F, mentioned
in 5.1.2
NOTE 3-In the example given in Note 1, each scale
unit after calibration represents:
0.600173.52 = 0.008 16 1 g
5.1.4 Interfacial Tensiometer-With the interfacial
tensiometer, the same principle of calibrating
by adjusting the length of the torsion arm
also applies. This instrument has, however, in
addition to the torsion arm, a torsion-arm counterbalance.
Adjust the length of this counterbalance
to coincide with that of the torsion arm
itself, in order that the vertical members of the
assembly may remain in line.
METHOD A-SURFACE
TENS103
6. Procedure
6.1 After the tensiometer has been calibrated,
check the level and insert the cleaned platinum
ring (Note 4) that will be used in the measurement.
Check the plane of the ring, and set the
dial and vernier at zero. Adjust the rear adjusting
screw so that the index level of the arm is opposite
the reference mark on the mirror, that is, the ri~g
system is at the zero position.
NOTE 4-Extreme care must be taken to have the
sample vessel and platinum ring clean. Contamination
of the liquid surface by dust or other atmospheric
impurities during measurement should be avoided.
6.2 Place the solution to be tested (Note 9,
contained in the thoroughly cleaned vessel (Note
4), on the sample platform. Raise the sample
platform by means of its adjusting screw until
the ring is just submerged.
NOTE 5-Since the surface tension of a solution is a
function of the concentration, care must be taken that
the concentration is adjusted and recorded within
known limits. The presence of solutes other than the
surface-active agent should be ascertained and reported
qualitatively and quantitatively, insofar as possible.
This includes hardness components in the water. Care
should be taken that the solution is physically homogeneous.
Measurements made near or above the cloud
point or other critical solubility points can be in serious
error. This is particularly true when the solute is a
surface-active material.
238

6.3 Lower the platform slowly, at the same
time applying torsion to the wire by means of
the dial-adjusting screw. These simultaneous adjustments
must be carefully proportioned so that
the ring system remains constantly in its zero
position. As the breaking point is approached,
the adjustments must be made more carefully
and more slowly. Record the dial reading when
the ring detaches from the surface.
6.4 Make at least two measurements. Additional
measurements shall be made if indicated
by the over-all variation obtained, the total number
of readings to be determined by the magnitude
of that variation.
6.5 Record the temperature of the solution
and the age of the surface at the time of testing.
Since the submerging of the ring (6.2) may constitute
a significant disturbance of the surface,
take the age as the dapsed time between submersion
and breakaway of the ring. The accuracy of
this time observation may be indicated in the
usual manner. In most cases an accuracy of +-5
s is reasonable, and sufficient for this method.
7. Calculation and Report
7.1 The dial reading, obtained from a measurement
carried out in the foregoing manner
with a calibrated instrument, is actually the pull
per linear centimetre on the ring (both inner and
outer circumference being considered) at the
break-point, expressed in dynes. This value,
called the uncorrected surface tension, must be
multiplied by a correcting factor, F, to give the
corrected surface tension. F is a function of the
contours of the liquid surface in the neighborhood
of the ring ai the instant of breakaway. It
can be numerically specified in terms of R, the
mean radius, in centimetres, of the ring; r, the
radius, in centimetres, of the wire from which
the ring is made; and V, the maximum volume
of !iquid e!evated above the free surface nf ?he
liquid. For liquids of low surface tension, such as
surface-active agen:s, F is, in general, appreciably
less than unity. It must, therefore, be ascertained
and applied. Values of F in terms of two compounded
parameters, R3/V and R/r have been
compiled and tabulated by Harkins and J~rdan.~
In order to look up F in the tables, the values of
these two parameters must be calculated. Values
for R and I are furnished by the manufacturer
with each ring. The value of Vis calculated from
D 1331
the following equation:
V = M/(D - d)
where:
M = weight of liquid raised above the free surface
of the liquid,
D = density of liquid, and
d = density of air saturated with vapor of the
liquid.
To calculate M, multiply the tensiometer dial
reading by the factor which converts this reading
into grams pull on the ring, as calculated in 5.1.3.
The factor D can be measured by the usual
procedures, and the value d can be obtained from
published data. The corrected surface tension in
dynes per centimetre is obtained by multiplying
the uncorrected surface tension value by F.
7.2 Unless specified, the surface tension values
reported shall be corrected values. Report
also the temperature at which the measurement
was made. If it is desired to report the surface
tension value of an aqueous solution at some
standard temperature, for example, 25'C, and
the measurement was actually made at a temperature
within about 3°C of this value (that is, 22
to 28'C), a correction factor of 0.14 dynes/cm.
'C may be used. Subtract this correction factor
from the surface tension when the temperature
of the test is lower than the reported temperature,
and add it to the surface tension when the temperature
of the test is higher than the reported
temperature. This value for the correction factor
is not valid for nonaqueous liquids, and should
be used only where the solvent is preponderantly
water.
METHOD LINTERFACIAL TENSION
8. Procedure
8.1 Determine interfacial tension as described
in Section 6 for surface tension, with the following
mdifica€ionsr
8. I. 1 Always move the ring from the aqueous
side of the interface through to the nonaqueous
side. With liquids lighter than water, it is accordingly
possible to use the precision tensiometer as
Harkins, W. D., and Jordan, H. F., "A Method for Determination
of Surface and Interfacial Tension from the Maximum
Pull on a Ring." Journal Am. Chemical Sac., Vol 52, 1930, p.
1751. These tables are also published in Physical Methods c,'
Organic Chemistry, Interscience Publishers, Inc., New York,
NY, VOI 1. 1945, p ~ 182-184. .
239

D 1331
well as the interfacial tensiometer. With liquids
heavier than water, where the ring must be
pushed downward, the interfacial tensiometer
should be used.
8.1.2 Use fresh solutions and a freshly cleaned
ring for each determination.
8.1.3 When operating with a liquid heavier
than the aqueous solution, place the two-layer
system in the sample vessel and place the ring in
the upper (aqueous) layer. Make the measurement
by turning the torsion wire counter-clockwise
and simultaneously keeping the ring system
in the zero position, as in the measurement of
surface tension, until the ring breaks through the
interface.
8.1.4 When operating with a liquid (oil)
lighter than the aqueous solution, first place the
aqueous solution in the sample vessel and immerse
the ring therein. Carefully pour the oil on
top of the aqueous solution to form the two-layer
system. Contact between the oil and the ring
should be avoided during this operation. After
allowing sufficient time for the interfacial tension
to come to its equilibrium value (Note 6), make
the measurement in the same manner as that
used for measuring surface tension.
NOTE 6-Since the interfacial energy of a newly
formed liquid-liquid interface generally requires some
time to reach its equilibrium value, it is advisable to
wait at least 5 min after the interface is formed before
taking a measurement.
9. Calculation and Report
9.1 As in the case of surface tension, a COK~Ction
factor, F, must be multiplied by the dial
reading (pull on the ring in dynes) in order to
obtain the corrected value for interfacial tension.
Values for F have been published by Zuidema
and Waters! The factor F is, in this case, a
function of the densities of the two liquids as well
as of R and r, the radius of the ring and that of
the wire, respectively.
9.2 Unless specified, interfacial tension values
reported shall be corrected values. Report and
adequately specify the nature of the nonaqueous
liquid (oil) used in the determination. Also report
the temperature at which the determination was
made. In contrast to surface tension values, interfacial
tension values cannot adequately be corrected
for small temperature deviations by means
of a simple formula.
'Zuidema, H. H., and Waters, G. W., "A Ring Method for
Determination of Interfacial Tension," Industrial and Engineering
Chemistry, Analytical Edition, Vol 13, 1941, p. 312.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this stadzrd. Users of this standard are expressly advised that determination of the validity of any such
pa&ent rights. and the risk of infringement of such rights, are entirely their own responsibility.
This stanahrd is subject to revision at any time by the responsible technical committee and must be reviewed every jive years and
fnot revised. either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be dressed to ASTM Headquarters. Your comments will receive car& consideration at a meeting of the
responsible technical committee, which you may attd. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.
240

4ib
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19105
Raprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Designation: D 1474 - 85
Standard Test Methods for
INDENTATION HARDNESS OF ORGANIC COATINGS’
This standard is issued under the fixed designation D 1474: the number immediately following the designation indicates the year of
original adoption or. in the case of revision. the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (6) indicates an editorial change since the last revision or reapproval.
Thew Iii.yI mi.rliod.v huve bivn upprovid ,/iw I I . bv ~ ugimii>.s qf [he Dipwtmcnr of Dil/irnsr 10 replucc Miithod 6212 of Fidiwl Test
Mi~lliod Slundurd No. 14lA undjiw lisling in Ihii DoD Index of Spi’c’(ficutions and Slundurds.
1. Scope
1.1 These test methods cover the determination
of the indentation hardness of organic materials
such as dried paint, varnish, and lacquer
coatings, when applied to an acceptable plane
rigid surface, for example, metal or glass.
I .2 Two methods are covered as follows:
Method A-Knoop
Method B-Pfund
Indentation Hardness
Indentation Hardness
Sections
6 to I2
13 to 19
1.3 Method A, which has the greater precision,
provides hardness values in terms of Knoop
Hardness Number (KHN). Method B provides
hardness in terms of Pfund Hardness Number
(PHN). Although the hardness value scales of
these methods differ, the methods agree in the
ranking of coating hardness.
I .4 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all qf‘the saj2t.v prob-
Ions associated with its use. It is the responsibility
of whocwr uses this standard to consult and
e.stablish appropriate s&ty and health practices
and determine the applicability Vf‘regulatorv limitations
prior to use.
2. Applicable Documents
2.1 ASTM Standards:
D823 Methods of Producing Films of Uniform
Thickness of Paint, Varnish, Lacquer,
and Related Products on Test Panels’
D 1005 Method for Measurement of Dry-Film
Thickness of Organic Coatings Using Micrometers*
D I I86 Methods for Nondestructive Measurement
of Dry-Film Thickness of Nonmag-
netic Coatings Applied to a Ferrous Base’
D 1400 Method for Nondestructive Measurement
of Dry-Film Thickness of Nonconductive
Coatings Applied to a Nonferrous BaseZ
3. Definitions
3.1 indentation hardness-the resistance to
penetration by an indenter.
3.2 Knoop indenter-a pyramidal diamond of
prescribed dimensions.
3.3 Pfund indenter-hemispherical quartz or
sapphire indenter of prescribed dimensions.
3.4 Knoop hardness number, KHN-the indentation
hardness determined with a Knoop
indenter, and calculated as follows:
KHN = L/A, = L/12Cp
where:
L = load applied to the indenter, kg,
I = measured length of long diagonal of the
indentation, mm,
C,, = indenter constant relating 1’ to A,,, and
A,, = projected area of indentation, mm2.
3.5 Pliind hardncw number, PHN-the indentation
hardness determined with a Pfund indenter,
and calculated as follows:
PHN = L/A = 4L/*d2 = 1.27 (L/d’)
’ These test methods are under the jurisdiction of ASTM
Committee D-I on Paint and Related Coatings and Materials
and are the direct responsibility of Subcommittee W1.23 on
Physical Properties of Applied Films.
Current edition approved Sept. 27, 1985. Published November
1985. Originally published as D 1474 - 57 T. Last previous
edition D 1474 - 68 (1979)“.
Annitul Book o/ASTM Stundurds, Vol 06.01.
24 1

D 1474
where:
L = load/kg applied to the indenter, kg,
A = area of projected indentation, mm2, and
d = diameter of projected indentation, mm.
4. Significance and Use
4.1 Identation hardness measurements have
proven to be useful in rating coatings on rigid
substrates for their resistance to mechanical
abuse, such as that produced by blows, gouging,
and scratching. These measurements do not necessarily
characterize the resistance to mechanical
abuse of coatings that are required to remain
intact when deformed.
5. Test Specimens
5.1 The substrate for the coating shall be an
acceptable plane rigid surface such as glass or
metal.
5.2 The coating thickness on any one panel
shall be uniform within 0.1 mil (3 pm). Coatings
to be compared shall be of equal thickness within
0.2 mil (5 pm). For maximum accuracy, the
minimum permissible coating thickness shall be
such that the depth of indentation does not exceed
three fourths of the coating thickness, to
minimize the effect of the substrate.
5.3 At least three replicate specimens shall be
tested for each coating to be evaluated.
5.4 Coatings should be applied in accordance
with Methods D 823 and their dry film thickness
should be measured in accordance with Methods
D 1005, D 1186, or D 1400.
METHOD A-KNOOP INDENTATION
HARDNESS
6. Summary of Method
6.1 This method consists of applying a load
to the surface of a coating by means of a pyramidal
shaped diamond having specified face angles,
and converting the measurements of the
resultant permanent impression to a hardness
number.
7. Apparatus
7.1 Hardness Te~ter,~ consisting of a load applicator,
a Knoop indenter, and a microscope
fitted with a movable micrometer stage. The
apparatus shall mechanically bring the indenter
into contact with the test surface with negligible
impact, apply the selected full load, maintain it
for 18 & 0.5 s, and withdraw the indenter.
7.2 Knoop Indenter-The Knoop indenter is
a pyramidal diamond with included longitudinal
angles of 172" 30' and included transverse angle
of 130" 0'.
NOTE I-The ratio of the long to the short diagonal
of the impression is approximately 7: 1 ; the ratio of the
long diagonal to the depth of penetration is approximately
30: 1.
7.3 Microscope-The microscope shall have a
filar micrometer eyepiece and sufficient objectives
to permit the measurement of the length of
impression to within &I %. The specimen shall
be firmly supported on a movable micrometer
stage attached to the microscope.
8. Calibration
8.1 Adjust the illumination in the microscope
to give maximum contrast when viewing an indentation.
8.2 By means of a calibrated scale, determine
the factor for each microscope objective that will
convert the filar scale units of the eyepiece to
millimetres.
8.3 With a 25-g load on the indenter, determine
the KHN of a calibrated standard (Note 2)
whose assigned value is not greater than 50 KHN.
If the obtained value is within &5 % of the assigned
value, the instrument is considered to be
in calibration.
NOTE 2-A suitable source of calibrated standards
in this hardness range is not available. Therefore, by
agreement of the parties concerned, a stable specimen
(such as an aged coating of a baked enamel applied to
a flat substrate) should be used to calibrate the participating
hardness testers.
9. Procedure
9.1 Unless otherwise specified, make the hardness
determinations at 73.5 & 3.50"F (23 & 2°C)
and 50 & 5 % relative humidity after equilibrating
the specimens cnder these cnnditinns fer at
least 24 h.
9.2 Rigidly attach the specimen to the movable
stage so that the surface to be measured is
normal to the direction of indentation.
NOTE 3-The panel should be so mounted that it
Among the hardness testers meeting the apparatus requirements
for this method are the Tukon Micro-hardness Tester
and the Riehle Kentron Micro-hardness Tester, available from
the Page-Wilson Measurement System Div., 929 Connecticut
Ave., Box 902 I , Bridgeport, CT 06602.
242

D 1474
cannot move with respect to the stage in any direction
during the course of the test.
9.3 Use the microscope to select an area of
the test specimen that is free of surface irregularities
and imperfections. Place this area under the
indenter by means of the movable micrometer
stage.
NOTE 4-If good impressions cannot be obtained
because of the roughness of the surface of the specimen,
gently polish the surface with No. 400 carborundum
and finish off with jewelers rouge before making the
impression.
9.4 Preset the apparatus to apply a 25-g load
and perform the test according to the manufacturer’s
instructions. Maintain the time the indenter
is in contact with the specimen for 18 f
0.5 s.
NOTE 5-For maximum accuracy, care must be
taken that the indenter does not penetrate the coating
to a depth beyond three fourths ofthe coating thickness.
This is necessary to eliminate any major substrate effect
on the hardness measurement.
9.5 Immediately after the completion of the
cycle, adjust the movable stage so that the indentation
is in the field of the microscope. Focus the
microscope on the indentation so that both extremities
of the long diagonal (that is, where the
upper edges of the indentation just converge) are
as sharp as possible. Measure the length of the
long diagonal of the impression with the filar
micrometer eyepiece.
NOTE 6-Select a microscope objective that will
cause the length of impression to be between 200 and
800 filar units to assure maximum accuracy in measurement.
9.6 From the measurements obtained in 9.5,
the information given in Note 1, and the measured
film thickness at the place of indentation,
calculate the depth of indenter penetration. If the
depth of penetration exceeds three-fourths of the
coating thickness, the results may be influenced
by substrate proximity. Therefore, for maximum
accuracy it is desirable to prepare thicker specimens
and repeat the test. Instead of this procedure,
at the option of purchaser and seller, an
indenter load of less than 25 g may be used.
9.7 Repeat the procedure described in 9.3,9.4,
and 9.5 until at least five impressions have been
made at widely spaced locations on the specimen.
10. Calculations
10.1 Calculate the mean indentation length in
filar units.
10.2 Convert this mean indentation length to
KHN by means of the appropriate tables supplied
with the instrument.
NOTE 7-If a conversion table is not available, the
KHN may be calculated as follows:
KHN = O.O25/l2CP
where:
0.025= load applied, kg, to the indenter,
1 = length of long diagonal of indentation,
mm, and
C, = indenter constant = 7.028 X lo-’.
11. Report
1 1.1 Report the following information:
11.1.1 Mean and range of KHN values obtained
for each specimen, stating the number of
indentations made and the indenter load used,
11.1.2 Mean film thickness of each specimen,
based on the measurements made at the points
of indentation,
11. I .3 Specimen preparation and conditioning
techniques used, and
11.1.4 Mean and range of KHN values of the
replicate panels.
12. Precision
12.1 On the basis of an interlaboratory test of
this method in which operators in six laboratories
tested seven coated panels having a broad range
of hardness, the within-laboratory coefficient of
variation was found to be 3 % with 2 1 degrees of
freedom and the between-laboratories coefficient
of variation 8 % with 30 degrees of freedom.
Based upon these coefficients, the following criteria
should be used for judging the acceptability
of results at the 95 % confidence level:
12.1.1 Repeatability-Two results, each the
mean of three determinations on a specimen,
obtained by the same operator should be considered
suspect if they differ by more than 9 % of
their mean va!ue.
12.1.2 Reproducibility-Two results, each the
mean of three determinations on a specimen,
obtained by operators in different laboratories
should be considered suspect if they differ by
more than 24 % of their mean value.
METHOD B-PFUND INDENTATION
HARDNESS
13. Summary of Method
13.1 This method consists of applying a load
to the surface of a coating, by means of a trans-
243

D 1474
parent colorless quartz or synthetic sapphire
hemisphere having a specified diameter, and converting
the measurement of the resultant observed
impression under load to a hardness number.
14. Apparatus
14.1 Hardness Testers-The hardness testers
used in this method shall consist of a load applicator,
a Pfund quartz or sapphire indenter, and
a microscope fitted with a stage. The apparatus
shall be constructed so as to permit the indenter
to be brought manually into contact with the
specimen surface with negligible impact.
14.2 Pfund Indentef-The Pfund indenter
(Fig. 1) is a transparent colorless quartz or synthetic
sapphire hemisphere with a spherical radius
of 0.125 in. (3.18 mm) and a maximum
spherical eccentricity of 0.002 in. (0.05 mm).
14.3 Microscope-The microscope shall have
a filar micrometer eyepiece and sufficient objectives
to permit the measurement of the diameter
of impression to within 21 %. The specimen
shall be rigidly supported on the microscope
stage.
14.4 Timer, capable of measuring a time interval
of 60 & 0.5 s.
15. Standardization
15.1 Adjust the illumination in the microscope
to give maximum contrast when viewing
an indentation.
15.2 By means of a calibrated scale, determine
the factor for each microscope objective that will
convert the filar scale units of the eyepiece to
millimetres.
15.3 With a 1 .O-kg load on the indenter, determine
the PHN of a calibrated standard (Note
2) with an assigned value not greater than 40
PHN. If the value obtained is within &5 ?6 of the
assigned value. the instrument shall be considered
to be in calibration.
16. Procedure
16.1 Unless otherwise specified, make the
hardness determination at 73.5 f 3.5"F (23 f
2°C) and 50 & 5 ?6 relative humidity, after holding
the specimens under these conditions for not
less than 24 h.
16.2 Rigidly attach the specimens to the instrument
stage such that the surface to be measured
is normal to the direction of indentation
(Note 3).
16.3 With a 1 .O-kg load on the indenter. carefully
bring the indenter into contact with the
specimen surface, apply the full load, and start
the timer. ~
16.4 At the end of 60 s, while still under full
load, rapidly measure the diameter of the circular
impression with the filar eyepiece of the microscope
(Note 6). It is very important that the
diameter measurements be made rapidly so that
the time the indenter is in contact with the specimen
is closely controlled.
16.5 From the measurements obtained in
16.4, the information given in 14.2, and the
measured film thickness at the place of indentation,
calculate the depth of indenter penetration.
If the depth of penetration exceeds three fourths
of the coating thickness, the results may be influenced
by substrate proximity. Therefore, for
maximum accuracy it may be desirable to prepare
thicker specimens and repeat the test.
16.6 Repeat the procedure in 16.3 and 16.4
until a total of at least five impressions have been
made at widely spaced locations on the specimen.
17. Calculations
17.1 Calculate the mean indentation diameter
in filar units.
17.2 Convert this mean indentation diameter
to millimetres using the appropriate factor determined
in 15.2.
17.3 Calculate the PHN as follows:
PHN = 1.27/d2
where:
d= mean indentation diameter, mm.
18. Report
18.1 Report the following:
18.1.1 Mean and range of PHN values obtained
for each specimen, stating the number of
indentations made.
18.1.2 Mean film thickness of the specimen,
based on measurements made near the points of
indentation,
18.1.3 Specimen preparation and conditioning
techniques used, and
18.1.4 Mean and range of PHN values of the
replicate panels.
A hardness tester meeting the apparatus requirements of
this method is the Pfund Indentation Hardness Tester. available
from the United States Testing Co.. 1415 Park Ave.. Hoboken.
NJ 07030.
244

Nb
Designation: D 1475 - 85
AMERICAN SOCIETY FOR TESTING AplD MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the Rext edition.
Standard Test Method For
DENSITY OF PAINT, VARNISH, LACQUER, AND RELATED
PRODUCTS’
This standard is issued under the fixed designation D 1475; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This method has been approved for use by agencies of the Departmeni of Defense to replace Meihod 4184.1 of Federal Tesi Meihod
Standard No. 141A and for lisiing in the DoD Index qfSpeclficaiions and Standards.
1. Scope
1.1 This test method covers the measurement
of density of paints, varnishes, lacquers, and
components thereof, other than pigments, when
in fluid form.
1.2 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health practices
and determine the applicability of regulatory limitations
prior to use.
2. Applicable Document
2.1 ASTM Standard:
E 380 Metric Practice2
3. Definition
3.1 density-the mass (weight in vacuum) of
a unit volume of the liquid at any given temperature.
In this method, it is expressed as the weight
in grams per millilitre, or as the weight in pounds
avoirdupois of one U. S. gallon, of the liquid at
the specified temperature; in the absence of other
temperature specification, 25°C is assumed.
4. Summary of Method
4.1 The accurately known absolute density of
distilled water at various temperatures (Table 1)
is used to calibrate the volume of a container.
The weight of the paint liquid contents of the
same container at the standard temperature
(25°C) or at an agreed-upon temperature is then
determined and density of the contents calcu-
lated in terms of grams per millilitre, or pounds
per gallon at the specified temperature.
5. Significance and Use
5.1 Density is weight per unit volume. It is a
key property in the identification, characterization,
and quality control of a wide range of
materials. Density measurements in terms of
weight per gallon are commonly used to check
paint quality. If the density is not within specification,
there is a good chance that there was a
mischarge or other serious problem.
5.2 This test method is suitable for the determination
of density of paint and related products
and components when in liquid form. It is particularly
applicable when the fluid has too high a
viscosity or when a component is too volatile for
a density balance determination.
5.3 This test method provides for the maximum
accuracy required for hiding power determinations.
It is equally suitable for work in which
less accuracy is required, by ignoring the directions
for recalibration and consideration of temperature
differentials, and using the container as
a “weight-per-gallon” cup.
6. Apparatus
6.1 Pycnometer-Any type, or weight-per-gal-
’ This test method is under the jurisdiction of ASTM Committee
D-l on Paint and Related Coatings and Materials and is
the direct responsibility of Subcommittee D01.24 on Physical
Properties of Liquid Paints and Paint Materials.
Current edition approved May 31, 1985. Published July
1985. Originally published as D 1475 - 57 T. Last previous edition
D 1475 - 60 (1980)“.
Annual Book ofASTM Standards, Vol 14.02.
245

D 1475
Ion cup, having a capacity of from 20 to 100 mL
may be used, provided that it may be filled
readily with a viscous liquid, adjusted to exact
volume, and covered to exclude loss of volatile
matter.
6.2 Thermometers, graduated in O.l"C, such
as are supplied with glass pycnometers.
6.3 Constant- Temperature Bath, held at
25 k 0.1"C is desirable.
6.4 Laboratory Analytical Balance.
NOTE 1 -The usual weight-per-gallon cup and similar
specialized pycnometers may have filled weights
that exceed the capacity of the usual laboratory analytical
balance. In such cases, use of a hanging pan, triplebeam
balance, with scales graduated to 0.01 g has been
found to provide results the mean of which was consistent
with the overall precision and accuracy of the
method.
6.5 Desiccator and Desiccated Balance, or a
room of reasonably constant temperature and
humidity are desirable.
7. Calibration of Pycnometer or Cup
7.1 Determine the volume of the container at
the specified temperature by employing the following
steps:
7.1.1 Clean and dry the container and bring
it to constant weight. Chromic acid (see 7.1.1.1)
cleaner and nonresidual solvents may be used
with glass containers and solvents with metal
containers. For maximum accuracy, continue
rinsing, drying, and weighing until the difference
between two successive weighings does not exceed
0.001 % of the weight of the container.
Fingerprints on the container will change the
weight and must be avoided. Record the weight,
M, in grams.
7.1.1.1 Chromic acid cleaning solution is corrosive
to skin, eyes and mucous membranes and
can cause severe burns. Avoid contact with eyes,
skin or clothing. In making dilute solution, always
add acid to water with care. In case of
contact, flush skin with water, using a shower if
exposure is severe. Flush eyes for 15 minutes
with copious amounts of water. Immediately call
a physician. Remove clothing immediately and
wash before reuse. Chromic acid cleaning solution
is a strong oxidizer. Avoid contact with
organic or reducing substances as a fire could
results. See supplier's Material Safety Data Sheet
for further information.
7.1.2 Fill the container with freshly boiled
distilled water at a temperature somewhat below
that specified. Cap the container, leaving the
overflow orifice open. Immediately remove excess
overflowed water or water held in depressions
by wiping dry with absorbent material.
Avoid occluding air bubbles in the container.
7.1.3 Bring the container and contents to the
specified temperature using the constant-temperature
bath or room if necessary. This will cause
further slight flow of water from the overflow
orifice due to the expansion of the water with the
rise of the temperature.
7.1.4 Remove the excess overflow by wiping
carefully with absorbent material, avoiding wicking
of water out of orifice, and immediately cap
the overflow tube where such has been provided.
Dry the outside of the container, if necessary, by
wiping with absorbent material. Do not remove
overflow that occurs subsequent to the first wiping
after attainment of the desired temperature
(Note 2). Immediately weigh the filled container
to the nearest 0.001 % of its weight (Note 3).
Record this weight, N, in grams.
NOTE 2-Handling the container with bare hands
will increase the temperature and cause more overflow
from the overflow orifice, and will also leave fingerprints;
hence, handling only with tongs and with hands
protected by clean, dry, absorbent material is recommended.
NOTE 3-Immediate and rapid weighing of the filled
container is recommended here to minimize loss of
weight due to evaporation of the water through orifices,
and from overflow subsequent to the first wiping after
attainment of temperature where this overflow is not
retained by a cap.
7.1.5 Calculate the container volume as follows:
V=(N-M)/p
where:
V = volume of container, mL,
N = weight of container and water, g (7.1.4),
M = weight of dry container, g (7.1.1), and
p = absolute density of water at specified temperature,
g/mL (see Table I).
7.1.6 Obtain the mean of at least three determinations.
8. Procedure
8.1 Repeat the steps in Section 7, substituting
the sample for the distilled water and a suitable
nonresidual solvent for the acetone or alcohol
(see 7.1.2 and Note 4). Record the weight of the
filled container, W, and the weight of the empty
container, w, in grams.
246

D 1475
NOTE 4-Trapping of paint liquids in ground glass
or metal joints is likely to result in high values of density
that appear to increase with the viscosity and density
of the material: such errors should be minimized by
firm seating of the joints.
8.2 Calculate the density in grams per millilitre
as follows:
where:
D,,, = density, g/mL.
D,,,=(W- W)/V
8.3 Calculate the density in pounds per gallon
as follows:
D=(W- w)K/V
where:
D = density, lb/gal,
K = 8.3454 (Note 5), and
I/ = volume of container, mL (see 7.1.6).
NOTE 5-The factor K, 8.3454, is calculated from
volume-weight relationship as follows:
8.345404 = [(2.54)" x (23 I .00)b]/(453.59237)c
(2.54)' is the conversion factor for millilitres to
cubic inches.
23 1 .OO is the conversion factor for cubic Aches to
gallons.
'453.59237 is the conversion factor for grams to
pounds.
9. Report
9. I In reporting the density, state the test temperature
to the nearest O.l"C, the units, and the
value calculated to the third place to the right of
the decimal point (for example, D = x.xxx Ib/gal
at 25°C); state the mean, the range, and the
number of replicate determinations.
10. Precision and Bias
10.1 The precision estimates are based on an
interlaboratory study in which one operator in
each of six different laboratories analyzed in duplicate
on two different days five samples of paint
ranging in density from 8.5 to 12.5 Ibs/gal. The
results were analyzed statistically in accordance
with Practice E 180. The within-laboratory coefficient
of variation was found to be 0.20 % relative
with 25 degrees of freedom and the betweenlaboratory
coefficient of variation was 0.6 1 %
relative with 20 degrees of freedom. Based on
these coefficients, the following criteria should be
used for judging the acceptability of results at the
95 % confidence level:
10.1.1 Repeatability-Two results, each the
mean of duplicate determinations, obtained by
the same operator on different days should be
considered suspect if they differ by more than
0.6 % relative.
10.1.2 Reproducibility-Two results, each the
mean of duplicate determinations, obtained by
operators in different laboratories should be considered
suspect if they differ by more than 1.8 %
relative.
10.2 No data on bias has been generated for
this method.
247

TABLE 1
Absolute Density of Water, g/mL
"C Density
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
0.999127
0.99897 I
0.998772
0.998623
0.998433
0.99823 1
0.998020
0.997798
0.997566
0.997324
0.997072
0.99681 1
0.996540
0.996260
0.995972
0.995684
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any irem mentioned in this standard. Users of this standard are expressly advised that determination ofthe validity qf any such
patent rights, and the risk of infringement cf such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every Jive years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting ofthe
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing voir should
makevour views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.
248

clSTb
Designation: D 1544 - 80
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
COLOR OF TRANSPARENT LIQUIDS (GARDNER COLOR
SCALE)'
This standard is issued under the fixed designation D 1544, the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval.
This method has been approved for use by agencies of the Department of Defense to replace Method 4248 of Federal Test Method
Standard No. 141A and for listing in the DoD Index of SpecPCations and Standards.
1. Scope
1.1 This method covers the measurement of
the color of transparent liquids by means of
comparison with arbitrarily numbered glass
standards. It applies to drying oils, varnishes,
fatty acids, polymerized fatty acids, and resin
solutions. Its application to other materials has
not been tested.
2. Applicable Documents
2.1 ASTM Standards:
D 1545 Test for Viscosity of Transparent Liquids
by Bubble Time Method2
E 308 Recommended Practice For Spectrophotometry
and Description of Color in
CIE 1931 Systems3
3. Apparatus
3.1 Glass Standards, 18, numbered separately,
and having the color characteristics
given in Table 1. A suitable procedure for their
calibration is contained in the Appendix. The
color shall be produced by the glass components
only.
3.2 Glass Tubes, c!ear, !Oh5 mm in inside
diameter and about 114 mm in outside length.
(Viscosity tubes, as described in Method
D 1545, are satisfactory.)
3.3 Suitable apparatus for comparing sample
and standard. The apparatus may be of any
design, but should have the following characteristics:
3.3.1 Illumination-CIF. Illuminant C.
3.3.2 Surrounding Field-The field should
not differ significantly in brightness from the
samples and standards and should be essentially
achromatic.
3.3.3 Field of View-The specimen and one
or more standards should subtend a visual angle
of about 2 deg and be in the field of view
simultaneously.
3.3.4 Separation of Standard and Specimen-
There should be a perceptible separation between
specimen and standard, but this should
be as small as is mechanically possible.
4. Procedure
4.1 Fill a glass tube with the material under
test. If the material is perceptibly cloudy, first
filter it.
4.2 Compare with glass standards, determining
which standard most closely matches the
specimen in brightness and saturation. Ignore
hue differences.
5. Report
5.1 Report the color as the number of the
standard most closely matching the specimen.
If more precise measurements are needed, report
as either matching a standard or lighter or
darker. Thus, between colors 5 and 6, the steps
will be 5, 5+, 5-, and 6.
' This method is under the jurisdiction of Committee D-1
on Paint and Related Coatings and is the direct responsibility
of Subcommittee DOI.33 on Varnish and Resins Including
Shellac.
Current edition approved March 10, 1980. Published May
1980. Originally published as D 1544 - 58 T. Last previous
edition D 1544- 68 (1974).
'Annual Book of ASTM Standards, Parts 27, 28, and 29.
'Annual Book of ASTM Standards, Parts 27 and 46.
249

D 1544
6. Precision
6.1 On the basis of a study in which one
observer at each of 80 laboratories made duplicate
determinations on four samples, the
"between" and "within" standard deviations
were found to be 0.5 and 0.1 color number,
respectively. Based on these standard deviations,
the following criteria should be used for
judging the acceptability of results at the 95 96
confidence level.
6.2 Repeatability-Two results obtained by
a single operator should be considered suspect
if they differ by more than two thirds of a color
number.
6.3 Reproducibility-Two results, each of the
mean of duplicate measurements, made by operators
in different laboratories should be considered
suspect if they differ by more than four-
thirds of a color number.
NOTE 1-If desired, liquid standards matching the
colors given in Table 1, in glass tubes similar to the
sample tubes may be used. These may be filled with
potassium chloroplatinate for the light colors and
solutions of ferric chloride and cobalt chloride in
hydrochloric acid for the darker colors. The specifications
and approximate composition of these solutions
are given in ASTM Method D I544 - 58 T, Test
for Color of Transparent Liquids (Gardner Color
Scale)." Many Glass Standards in current use do not
conform to the values of Table 1.
NOTE 2-The precision data were obtained using
an instrument in which two standards are viewed
simultaneously. There are other instruments available
for color matching which would be expected to
give similar results, but the statement above applies
only to the instrument checked.
' Discontinued, see 1961 Book of ASTM Standards, Part
8.
TABLE 1
Color Specifications of Reference Standards
Gard- Chromaticity Coordiner
nates"
Lumi- Trans-
Color
mittnous
Stand- Transmit- Talerance
ard
tance Y
Num-
X
Y
ance
(If-)
ber
I 0.3 I77 0.3303 80 7
2 0.3233 0.3352 79 7
3 0.3329 0.3452 76 6
4 0.3437 0.3644 75 5
5 0.3558 0.3840 74 4
6 0.3767 0.4061 71 4
7 0.4044 0.4352 67 4
8 0.4207 0.4498 64 4
9 0.4343 0.4640 61 4
IO 0.4503 0.4760 57 4
II 0.4842 0.48 I8 45 4
12 0.5077 0.4638 36 5
13 0.5392 0.4458 30 6
14 0.5646 0.4270 22 6
15 0.5857 0.4089 16 2
16 0.6047 0.3921 II I
17 0.6290 0.3701 6 1
18 0.6477 0.3521 4 1
a A duplicate standard shall have chromaticity coordinates
that differ from the reference standard by no more than one
third of the difference in x or ,P between adjacent reference
standards. In any one set, no two standards shall be closer
together than two thirds of the difference in x or ,p between
corresponding reference standards.
-
APPENDIX
Al. CALIBRATION OF GLASS REFERENCE STANDARDS
A I. 1 Select a dual beam spectrophotometer with
a sufficiently small light beam at the sample position
so that all rays will pass through the standards to be
calibrated. Alternatively equip the spectrophotometer
with a condensing lens to accomplish this purpose.
A1.2 Place the standards in turn in the sample
250

position of the spectrophotometer. If the comparator
is provided with a separate green filter in front of the
light source, place this filter in the reference beam of
the dual beam spectrophotometer during calibration
of each standard.
A1.3 Obtain spectral transmittance data for each
glass reference standard by following Recommended
Practice E 308.
A1.4 From the spectral transmittance data for
each reference standard calculate the CIE tristimulus
values, X, Y, Z, and the chromaticity coordinates, x,
y, for CIE Illuminant C (see Recommended Practice
E 308).
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in
connection with any item mentioned in this siandard. Users of this standard are expressly advised that determination of the va1idit.y
of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years
and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. Ifyou feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, Pa. 19103, which will schedule a
further hearing regarding your comments. Failing satisfaction there, you may appeal to the ASTM Board of Directors.
25 1

4Ib
Designation: D 1653 - 85
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Methods for
WATER VAPOR PERMEABILITY OF ORGANIC COATING
FILMS'
This standard is issued under the fixed designation D 1653; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
These test methods have been approved for use by agencies of the Department of Defense to replace Method 61 71 of Federal Test
Method Standard No. 141A and for listing in the DoD Index of SpeciJiations and Standards.
1. scope
1.1 These test methods cover the determination
of the rate at which water vapor passes
through films of paint, varnish, lacquer, and
other organic coatings. The films may be free
films or they may be on substrates such as plastic
film, glass cloth, paper, or thin plywood.
1.2 Two methods are covered as follows:
1.2.1 Method A-Wet Cup Method, and
1.2.2 Method B-Dry Cup Method.
1.3 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health practices
and determine the applicability of regulatory limitations
prior to use. Specific precautionary statements
are given in Section 8.
2. Applicable Documents
2.1 ASTM Standards:
D823 Methods of Producing Films of Uniform
Thickness of Paint, Varnish, Lacquer,
and Related Products on Test Panels'
D 1005 Test Method for Measurement of Dry-
Film Thickness of Organic Coatings Using
Micrometers2
D 1 193 Specification for Reagent Water3
E 96 Test Methods for Water Vapor Transmission
of Materials4
3. Descriptions of Terms Specific to This Standard
3.1 water vapor transmission rate, WVT-the
steady water vapor flow in unit time through unit
area of a body, between two specific parallel
surfaces, under specific conditions of temperature
and humidity at each surface. Accepted
inch-pound units are grains per square foot per
hour. Accepted SI units are grams per square
metre per 24 h.
3.2 water vaporpermeance, WVP-the steady
water vapor flow in unit time through unit area
of a body induced by unit vapor pressure difference
(Ap) between the two surfaces of the coating.
Therefore, WVP = WVT/Ap. Accepted inchpound
units are grains per square foot per hour
per inch of mercury (called a perm). Accepted SI
units are grams per square metre per 24 h per
millimetre of mercury (called a metric perm).
3.3 water vapor permeability, P-the permeance
through the total thickness of a body. Therefore,
P = (WVP).l, where 1 is thickness of body.
Accepted inch-pound units are grains per square
foot per hour per inch of mercury per mil of
thickness (called perm-mil). Accepted SI units
are grams per square metre per 24 h per millimetre
of mercury per centimetre of thickness
(called metric perm-centimetre).
'These test methods are under the jurisdiction of ASTM
Committee D-1 on Paint and Related Coatings and Materials
and are the direct responsibility of Subcommittee D01.23 on
Physical Properties and Applied Paint Films.
Current edition approved Sept. 27, 1985. Published November
1985. Originally published as D 1653 - 59 T. Last previous
edition D 1653 - 72 (1979)t'.
' Annual Book qf ASTM Standards, Vol06.0 I.
'Annual Book ufASTM Standards, Vol06.03.
Annual Book of ASTM Standards, Vol04.06.
252

D 1653
4. Summary of Method
4.1 In Method A (Wet Cup Method), the test
specimen is sealed to the open mouth of a cup
or dish containing distilled water, and the assembly
placed in a test chamber with a controlled
atmosphere. Two sets of exposure conditions are
recommended for this method:
4.1. I Condition A, consisting of very low relative
humidity at 73°F (23"C), and
4.1.2 Condition B, consisting of 50 % relative
humidity at 73°F (23°C). Periodic weighings of
the cup or dish are made to determine the rate
of water vapor movement through the specimen.
4.2 In Method B (Dry Cup Method) the test
specimen is sealed to the open mouth of a cup
or dish containing desiccant, and the assembly
placed in a test chamber with a controlled atmosphere.
Two sets of exposure conditions are
recommended for this method:
4.2.1 Condition B, consisting of 50 % relative
humidity at 73°F (23"C), and
4.2.2 Condition C, consisting of 90 % relative
humidity at 100°F (38°C). Periodic weighings of
the cup or dish are made to determine the rate
of water vapor movement through the specimen.
5. Significance And Use
5.1 One of the factors affecting the protection
provided by an organic coating is the resistance
of the coating to permeation by water vapor.
Hence, the permeability characteristics of coatings
are important in assessing their performance
in practical use.
5.2 The purpose of these test methods is to
obtain reliable values of water vapor transfer
through permeable and semipermeable organic
coatings. These values are for use in design, manufacture,
and marketing.
5.3 Water vapor transmission rate is not necessarily
a linear function of film thickness and is
not a linear function of temperature and relative
humidity. Therefore, a permeance value obtained
under one set of conditions may not indicate
what the value would be for a different set
of conditions. For this reason, the test conditions
should be selected that most closely approach the
conditions of use. While any set of conditions
may be used, standard conditions that have been
useful are given.
5.4 Values of water vapor transmission rate
(WVT) can be used in the relative rating of
coatings for permeance only if the coatings are
tested under the same closely controlled conditions
of temperature and relative humidity and
their film thicknesses are equal.
5.5 Values of water vapor permeance (WVP)
can be used for the comparison of materials of
equal thickness that have been tested under different
conditions of temperature and humidity.
6. Apparatus
6.1 Permeability Cup' or Dish (Note l), consisting
of a container made of noncorroding material,
impermeable to water or water vapor. It
should have a capacity of approximately 25 mL
and be of such dimensions and mass that it can
be weighed on an analytical balance. It should
have a mouth opening that will permit the exposure
of at least 25 cm2 of film to atmospheric
conditions.
NOTE I-If the cup or dish is made of aluminum,
it must be anodized or given a protective clear coating
to prevent corrosion.
6.1. I One type of cup that is suitable has a
flanged edge and is equipped with a separate
corresponding flange, so that the test specimen
can be held between them. The contacting faces
of the flanges shall be ground to such flatness
that when the film is in position, no moisture
can be lost from the cup, except through the
exposed area. For hard films, or films having a
very rough surface, a soft rubber gasket may be
inserted between the film and the flange. The
flanges shall be held together with suitable
clamps. A suitable cup of this type is the Gardner-
Park Permeability Cup shown in Fig. 1.
6.1.2 Another suitable cup is an open circular
dish to which the test specimen can be sealed
with wax.
6.2 Low-Humidity Chamber, consisting of a
standard glass desiccator or other suitable cabinet
in which a desiccant may be placed that will
produce a condition of very low (near zero) relative
humidity. Provision must be made to maintain
the desiccator or low-humidity chamber at
a uniform temperature to within 1°F (0.6"C) of
the desired temperature.
NOTE 2-The desiccant may be replaced with a salt
solution of known vapor pressure when a condition
higher than practically zero vapor pressure is required.
--
'The Gardner Permeability Cup, with test area of 25 cm2,
available from the Gardner/Neotec Division of the Pacific Scientific
Co., 1 100 East-West Highway, Silver Spring, MD 20910,
has been found satisfactory for this purpose. Other suitable types
of cups are described in the Appendix of Test Methods E 96.
25 3

D 1653
6.3 Test Chamber, with a controlled temperature
over the range from 70 to 1OO”F (20 to
40°C) and a controlled relative humidity over the
range from 50 to 90 %. The temperature shall be
maintained to within 1°F of the desired value
atd the relative humidity shall be maintained to
within 2 ?6 of the desired value. Air shall be
circulated continuously throughout the chamber
to maintain uniform conditions at all test locations.
6.4 Analytical Balance, having an adequate
capacity for the weight of the test cups and a
sensitivity of 1 mg.
7. Materials
7.1 Reagent Water (for the wet cup test), conforming
to Type IV of Specification D 1193.
7.2 Desiccant, consisting of either anhydrous
calcium chloride (Ca Clz) or anhydrous magnesium
perchlorate (Mg(C10&). (Caution-See
8.1 .) The calcium chloride shall be dried at 400°F
(200°C) before use.
7.3 Sealant, such as wax, for attaching the test
specimen to the top of the permeability cup. It
must be highly resistant to the passage of water
vapor (and water). It must not lose weight to, or
gain weight from, the atmosphere in an amount,
over the required period of time, that would
affect the test result by more than 2 %. It must
not affect the vapor pressure in a water-filled cup.
NOTE 3-Among acceptable sealants are ( I ) a 60:40
mixture of microcrystalline wax and refined crystalline
parafin wax, and (2) a 5050 mixture of beeswax and
rosin.
7.4 Film Support, providing support for free
films too brittle or otherwise unsatisfactory for
handling. Support materials of parchmentized
paper,6 filter paper, and glass cloth’ have been
found to be satisfactory in some instances. Such
support can have an effect on the test results.
8. Precautions
8.1 Use caution in handling magnesium perchlorate
because of possible violent chemical reaction
that may be produced if it comes in contact
with some organic materials.
9. Test Specimens
9.1 It is very important that the test specimens
be smooth, completely continuous films of uniform
thickness throughout the test area, and
entirely free of dust or other foreign matter.
Apply coatings to substrates by one of the auto-
matic-spray, dip, or doctor-blade methods described
in Methods D 823. However, special test
conditions may require that the coating be ap
plied by brushing, roller coating, or other special
methods. The thickness of the coating applied
shall be within normal range for the type of
material under test, and should not vary by more
than 5 % of total thickness in any test series.
NOTE 4-For coatings of low permeability, use the
same method of application when test results are to be
intercom pared.
9.2 Air dry or bake the coated material for a
specified time at a specified temperature, which
depends upon the requirements of the coating
under test. Permeability may vary with the baking
schedule or the time of air drying. If the
material is to be tested as a free film, remove it
from the substrate and allow the previously unexposed
surface free access to the air for at least 7
days in the case of air-drying materials.
9.3 Cut a circular disk from the conditionedfree
film or coated support by placing the cup on
the material and cutting around the outside edge
with a razor blade. Measure the thickness of the
disk at several places with a micrometer using
the procedures in Test Method D 1005. The
thickness may also be calculated from the relationship
between the area of the disk, weight of
the disk, and density of the film. With supported
films the weight of the support must be subtracted
from the total weight of the disk. The
amount of film in the area under test may be
calculated from the ratio of the total area of the
disk to the exposed area.
NOTE 5-Wherever possible, use unsupported films
to eliminate the potential interferences of substrates.
9.4 When coatings are applied to only one
side of a support, the coated side of the test
specimen should be placed toward the water in
the cup and the uncoated side exposed to the dry
air of the desiccator. Coatings should not be
applied to both sides of a support that will absorb
water, such as paper, because they will show
abnormally high permeability due to the swelling
of the support and consequent distention of the
film. Coatings applied to a fine grade of glass
cloth do not show this distention because there
Payne, H. F., “Permeability Measurements,” Paint and
Varnish Proceedings, Scientific Section, National Paint, Varnish,
and Lacquer Assoc., 1938.
’ Payne, H. F., “Permeability to Moisture of Organic Surface
Coatings,” Industrial and Engineering Chemistry, Analytical
Edition, Vol I I, 1939, p. 453.
254

D 1653
is no swelling of the fibers during this test. Glass
cloth is preferred for coatings that are cured by
baking and subsequent testing. The best method
of application to glass cloth is by the automatic
dipping apparatus, where the rate of withdrawal
is such as to provide a film of uniform thickness.
METHOD A-WET
10. Test Conditions
CUP METHOD
10. I Unless other conditions are agreed upon
by the purchaser and the seller, the tests shall be
performed under one or more of the following
conditions:
10.1. I Condition A-Test chamber maintained
at 73°F (23°C) and very low (near zero)
relative humidity.
10.1.2 Condition B-Test chamber maintained
at 73°F (23°C) and 50 % relative humidity.
11. Procedure
1 I. 1 Prepare at least two and preferably three
test cups for each test material as follows:
1 1.1. I Pour from 6 to 8 mL of distilled water
in the permeability cup.
11.1.2 If the cup is equipped with flanges,
place the test specimen over the opening of the
cup between the flanges and adjust the clamps to
hold it firmly in position. If the coating is on a
substrate or support, place the coated side toward
the water in the cup.
I 1. I .3 If the cup is not equipped with flanges,
seal the test specimen to the top edge of the cup
with wax:
11.1.3.1 First place the test specimen, cut to
the size of the cup, carefully on a thin cardboard
ring soaked in molten wax. Equilibrate with vapor
at the desired relative humidity and temperature.
I 1. I .3.2 Then place the specimen-covered
ring over the mouth of the cup, taking care that
the film does not touch the water. Thoroughly
seal the ring to the edge of the cup at the temperature
to be used in the test. Make certain that
a film area of at least 25 cm2 is exposed for the
transmission of vapor.
NOTE 6-Imperfections in the film that are not readily
visible will produce a very high loss rate; consequently
the test should always be run in duplicate, and
preferably in triplicate.
I I .4 Weigh the loaded cups to 1 mg and place
them in the test chamber.
11.5 Remove the cups for periodic weighing
to determine the loss in weight. In general, the
cups should be weighed every 24 h for a period
of I week, or until the loss rate has become
constant. For some very permeable coatings, it
may be necessary to make weighings at shorter
time intervals.
NOTE 7-If the cup must be removed from the test
chamber for weighing, then weigh the cup immediately
after removal and return the cup to the test chamber
immediately.
METHOD B-DRY
CUP METHOD
12. Test Conditions
12. I Unless other conditions are agreed upon
by the purchaser and the seller, the tests shall be
performed under one or more of the following
conditions:
12. I . I Condition B-Test chamber maintained
at 73°F (23°C) and 50 % relative humidity.
12. I .2 Condition C-Test chamber maintained
at 100°F (38°C) and 90 % relative humidity.
13. Procedure
13.1 Prepare at least two and preferably three
test cups for each test material as follows:
13. I. 1 Fill the permeability cup with desiccant
to within '/4 in. (6 mm) of the top edge.
13.1.2 If the permeability cup is equipped
with flanges, place the test specimen between the
flanges and adjust the clamps to hold it firmly in
position.
13.1.3 If the permeability cup is not equipped
with flanges, seal the test specimen to the top
edge of the cup with wax in accordance with the
procedures in 1 1.1.3.1 and 1 1.1.3.2.
13.1.4 Weigh the loaded cups to I mg and
place them in the test chambers.
13. I .5 Remove the cups for periodic weighing
to determine the increase in weight. In general,
the cups should be weighed every 24 h for a
period of I week. or until the rate of weight
increase has become constant. For some very
permeable coatings, it may be necessary to make
weighings at shorter time intervals (Note 7).
14. Calculations
14.1 For each material tested, determine the
mean values for the replicate cup weighings in
milligrams.
14.2 Plot the mean values for successive
weighings against elapsed time and draw a
smooth curve through the plotted points. When
a straight line adequately fits the plot of four
255

D 1653
successive 24 h spaced points, a nominally steady
state exists. Determine the slope of the straight
line which is the rate of vapor transmission, T,
in terms of weight change in milligrams per hour.
14.3 Calculate one or more of the following,
depending on the permeability characteristics to
be determined:
14.3.1 Calculate the water vapor transmission
rate, WVT:
14.3.1.1 In inch-pound units as follows:
WVT = (G/t)/A = grains per square foot per I h
where:
G = weight change, grains (from the straight
line),
t = time during which G occurred, h, and
A = test area, ft2.
1 g = 15.43 grains
14.3.1.2 In metric units as follows:
WVT = (G/t)/A = grams per mz per 24 h
where:
G = weight change, g (from straight line),
t = time during which G occurred, h, and
A = test area, mz.
14.3.2 Calculate the permeance, WVP:
14.3.2.1 In inch-pounds units as follows:
WVP = WVT/Ap = grains per foot per I h
per inch of mercury (perms)
where:
AP = S(RI - &),
S = in. Hg (saturation vapor pressure at test
temperature),
RI = relative humidity at vapor source, and
R2 = relative humidity at vapor sink.
14.3.2.2 In metric units as follows:
WVP = WVT/Ap = grams per square metre per 24 h
per millimetre of mercury, (metric perms)
where:
AP = ~(RI-Rz),
S = mm Hg (saturation vapor pressure at test
temperature),
RI = relative humidity at vapor source, and
R2 = relative humidity at vapor sink.
14.3.3 Calculate the permeability coefficient,
p:
14.3.3.1 In inch-pounds as follows:
P = (WVP)-l = grains per ft2 per 1 h
per inch of mercury per mil thickness (perm-mils)
where:
I = film thickness, mils.
14.3.3.2 In metric units as follows:
P = (WVP). 1 = grams per square metre per 24 h
per millimetre of mercury per centimetre of thickness
(metric perm-centimetre)
where:
1 = film thickness, cm.
NOTE 8-Examples of calculations: In a dry cup test
that ran 288 h (1 2 days) on a I .5-mil film with exposed
area of 3.88 in? (25 cm2), it was found that the rate of
gain was substantially constant after 48 h and during
the subsequent 240 h, the weight gain was 500 mg. The
controlled chamber conditions were measured to be
89.O’F (3 1.7”C) and 49 % relative humidity.
(a) Calculate in inch-pound units as follows:
G/t = (0.5.15.43)/240 = 0.032 grains/h (15.43 is conversion
from grams to grains),
A = 3.88/144 = 0.027 ftz,
then WVT = 0.032/0.027 = 1.19 grains/ft2 in 1 h,
S = 1.378 in. Hg (saturation vapor pressure at 89”F),
RI = 0.49 (in chamber),
RZ = 0.00 (in cup),
Ap = S (RI- R2) = 1.378 (0.49- 0.00) = 0.675 in.
Hg,
then WVP =
WVP =
WVT/Ap = 1.1910.675,
1.76 grains per square foot per 1 h per
inch of mercury, and
WVP = 1.76 perms.
P = (WVP).I,
P = 1.76.1.5 = 2.6,
P = 2.6 grains per square foot per 1 h per inch of
mercury per mil thickness, and
P = 2.6 perm-mils.
(b) Calculate in metric units as follows:
G/t = 0.5/10 = 0.05 g/24 h,
A = 0.225/104 = 0.0025 m,
then WVT = 0.5/0.0025 = 20 g/m2 in 24 h,
S = 35 mm Hg (saturation vapor pressure at 89”F),
R1 = 0.49 (in chamber),
R2 = 0.00(incup),
Ap = S (RI- R2) = 35 (0.49 - 0.00) = 17.15 mm
HI?,
then WVP = WVT/Ap = 20117.15,
WVP = 1.16 g per square metre per 24 h per milk
metre of mercury,
WVP = 1.16 metric perm,
P
P
P
= (WVP).I,
= 16.0.0044 = O.OOO18 g per square metre per
24 h per millimetre of mercury per cm thickness,
and
15. Report
= 4.4 x !0-3 metric *m-centirnet.e.
15.1 Report the following information:
15.1.1 Method of coating application and curing
procedure used.
15.1.2 Mean film thickness of the test specimens
for each material.
15.1.3 Type of film support used, if any.
15.1.4 Method used (Method A (Wet Cup) or
Method B (Dry Cup).
15.1.5 Which face of the test specimen was
256

D 1653
exposed to the higher humidity.
15.1.6 Test temperature and relative humidity
in the test chamber.
15.1.7 Computed rate of water vapor transmission
(WVT), either in inch-pound or in metric
units.
15. I .8 The computed permeance in terms of
both perms and metric units.
16. Precision
16. I Results obtained by any one procedure
on several test specimens from the same sample
may differ as much as 10 % from their average.
Careful attention to all aspects of the procedures
is required in order to obtain test results of acceptable
precision.
NOTE 9-Some
are:
factors producing a lack of precision
(a) Area of film transmission encroached upon by
seal.
(b) Splashing of film by water in wet cup method.
(c) Variation in air gap under film.
(d) Faulty control of temperature or humidity, or
both.
(e) Removal time ofcups from test conditions during
weighing.
(J) Leakage of seal.
257

D1653
I
I
Metric Equivalents
in. 3% 3 '%6 '/32
mm 82.6 76.2 17.5 2.4
1 -Cap, Top
2-Washer
3-Gasket
4-Base, Cup
5--Dowel, %z
in. in Diameter
FIG. 1 Gardner-Park Permeability Cup
The American Society,for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination ofthe validity of any such
patent rights, and the risk of infn'ngement of such rights, are entirely their own responsibi1i;y.
This standard is subjecl[o revision at any time by the responsible technical committee and must be reviewed everyjive years and
iJ not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.
258

Wb
Designation: D 1876 - 72 (Reapproved 1978)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not'listed in the current combined index, will appear in the next edition.
VWTHOUT CHANGE IN
1983
An American National Standard
Standard Test Method for
PEEL RESISTANCE OF ADHESIVES
(T-PEEL TEST)'
This standard is issued under the fixed designation D 1876; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This meihod has been approved for use by agencies of ihe Deparimeni of Defense as pari of Federal Test Method Standard
No. I75a andfor lisiing in ihe DoD Index of Specijicaiions and Standards.
1. Scope
INTRODUCTION
The accuracy of the results of strength tests of adhesive bonds will depend on the
conditions under which the bonding process is carried out. Unless otherwise agreed
upon by the manufacturer and the purchaser, the bonding conditions shall be prescribed
by the manufacturer of the adhesive. In order to ensure that complete information
is available to the individual conducting the tests, the manufacturer of the
adhesive shall furnish numerical values and other specific information for each of the
following variables:
(I) Procedure for preparation of the surfaces prior to application of the adhesive,
the cleaning and drying of metal surfaces, and special surface treatments such as
sanding, which are not specifically limited by the pertinent test method.
(2) Complete mixing directions for the adhesive.
(3) Conditions for application of the adhesive, including the rate of spread or
thickness of film, number of coats to be applied, whether to be applied to one or both
surfaces, and the conditions of drying where more than one coat is required.
(4) Assembly conditions before application of pressure, including the room temperature,
length of time, and whether open or closed assembly is to be used.
(5) Curing conditions, including the amount of pressure to be applied, the length
of time under pressure, and the temperature of the assembly when under pressure.
It should be stated whether this temperature is that of the glue line, or of the atmosphere
at which the assembly is to be maintained.
(6) Conditioning procedure before testing, unless a standard procedure is specified,
including the length of time, temperature, and relative humidity.
A range may be prescribed for any variable by the manufacturer of the adhesive,
if it can be assumed by the test operator that any arbitrarily chosen value within
such a range or any combination of such values for several variables will be acceptable
to both the manufacturer and the purchaser of the adhesive.
1.1 This method is primarily intended for
determining the relative peel resistance of
adhesive bonds between flexible adherends by
means of a T-type specimen.
2. Description of Terms
2.1 T-peel Srrengrh is the average load per previous edition D 1876 69
unit width of bond line required to produce
progressive separation of two bonded, flexible
adherends, under conditions designated in
' This method is under the jurisdiction of ASTM Committee
D-14 on Adhesives
Current edition approved July 28, 1972 Published OC-
tober 1972 Origindlly published as D 1876
61 T Last
259

___I
D 1876
this method.
2.2 Flexible-as used in this method, indicates
that the adherends shall have such dimensions
and physical properties as to permit
bending them through any angle up to 90 deg
without breaking or cracking.
3. Apparatus
3.1 Tension Testing Machine, capable 01
applying a tensile load having the following
prescribed conditions:
3.1.1 The machine and loading range shall
be so selected that the maximum load on the
specimen falls between 15 and 85 percent of
the upper limit of the loading range.
3.1.2 The rate of movement between heads
shall remain essentially constant under fluctuating
loads.
NOTE 1-It is difficult to meet this requirement
when loads are measured with a spring-type or
pendulum-type weighing device.
3.1.3 The machine shall be equipped with
suitable grips capable of clamping the specimens
firmly and without slippage throughout
the tests.
3.1.4 The machine shall be autographic,
giving a chart that can be read in terms of
inches of separation as one coordinate and
applied load as the other coordinate.
3.1.5 The applied tension as measured and
recorded shall be accurate within &I percent.
3.2 Conditioning Room or Desiccators-
The conditioning room or desiccators (Note 2)
shall be capable of maintaining a relative humidity
of 50 f 2 percent at 23 f 1 C (73.4 f
1.8 F).
NOTE 2-A saturated solution of calcium nitrate
will give approximately 51 percent relative humidity
at the testing temperature.
4. Test Specimen
4.: Laiiiinated test pneis (see Fig. i) shaii
consist of two flexible adherends properly
prepared and bonded together in accordance
with the adhesive manufacturer’s recommendations.
Specially prepared test panels shall
be 152 mm (6 in.) wide by 305 mm (12 in.)
long, but shall be bonded only over approximately
241 mm (9 in.) of their length. Test
panels of these same dimensions may also be
cut from larger, fully laminated panels.
NOTE 3-Direct comparisons of different adhesives
can be made only when specimen construc-
tion and test conditions are identical.
NOTE 4-Clad aluminum alloy 0.81 mm (0.032
in.) thick conforming to ASTM Specification
B 209, for Aluminum-Alloy Sheet and Plate,* Alloy
2024-T3, has been found satisfactory as an adherend
for structural adhesives. Canvas, coated fabrics,
plastics films, and metal foils have also proven
to be satisfactory adherends for use with specific
adhesives.
NOTE 5-It is not essential that the two adherends
be alike, either in material or thickness. They
shall, however, be capable of being bent through
any angle up to 90 deg without breaking.
4.2 The bonded panels shall be cut into 25-
mm (1-in.) wide test specimens (see Fig. 1)
by a means that is not deleterious to the bond.
The 76-mm (3411.) long unbonded ends shall
be bent apart, perpendicular to the glue line,
for clamping in the grips of the testing machine.
4.3 At least ten test specimens shall be
tested for each adhesive.
NOTE 6-Within the limitations imposed by
Note 3, other specimen widths may be used, provided
the test machine grips are of ample width to
apply the load uniformly across the width of the
adherends.
NOTE 7-For obtaining a gripping area on specimens
that are completely bonded, one end of the
bonded specimen may be chilled in dry ice until
the adhesive becomes brittle, and then the adherends
may be carefully pried apart. This technique
will not work for all adhesives and adherends.
5. Conditioning
5.1 Condition specimens for 7 days at a
relative humidity of 50 f 2 percent at 23 f
1 C (73.4 f 1.8 F), except where the adhesive
manufacturer may specify such an aging
period to be unnecessary or a shorter period
to be adequate.
NOTE 8-Conditioning is not required for laminated
assemblies containing only metal adherends,
unless specified as a part of the bonding procedure
by the manufacturer of the adhesive.
6, Procedure
6.1 Clamp the bent. unbonded ends of the
test specimen in the test grips of the tension
testing machine. Apply the load at a constant
head speed of 254 mm (10 in.)/min.
NOTE 9-This speed will cause separation of the
bond at a rate of 127 mm (5 in.)/min.
6.2 During the peel test make an autographic
recording of load versus head move-
1983 Annual Book ofASTM Standards, Vol02.02.
260

D 1876
ment or load versus distance peeled.
6.3 Determine the peel resistance over at
least a 127-mm (Sin.) length of the bond line
after the initial peak.
7. Calculation
7.1 Determine from the autographic curve
for the first 127 mm (5 in.) of peeling after
the initial peak the average peeling load in
pounds per inch of the specimen width required
to separate the adherends. It is preferred
that the average be determined from
the curve with the use of a planimeter.
NOTE 10-In case a planimeter is not used, the
average may be calculated as the average of load
readings taken at fixed increments of crosshead
motion. For example, the load may be recorded at
each 25” (1-in.) interval of head motion (or
each 12.7 mm (0.5 in.) interval of bond separation)
following the initial peak, until at least ten readings
have been obtained.
8. Report
8.1 The report shall include the following:
8.1.1 Complete identification of the adhesive
tested, including type, source, manufacturer’s
code number, batch or lot number,
form, etc.,
8.1.2 Complete identification of adherends
used, including material, thickness, surface
preparation, and orientation,
8.1.3 Description of bonding process, including
method of application of adhesive,
glue-line thickness, drying or precuring conditions
(where applicable), curing time, temperature,
and pressure,
8.1.4 Average thickness of adhesive layer
after formation of the joint, within 0.001 in.
The method of obtaining the thickness of the
adhesive layer shall be described including
procedure, location of measurement, and
range of measurements.
8.1.5 Complete description of the test specimens,
including dimensions and construction
of the test specimens, conditions used for cutting
individual test specimens, number of test
panels represented, and number of individual
test specimens,
8.1.6 Conditioning procedure prior to testing,
8.1.7 Type of test machine and crosshead
separation rate used,
8.1.8 Method of recording load and determining
average load,
8. I .9 Average, maximum, and minimum
peeling load values for each individual specimen,
8.1.10 Average T-peel strength in pounds
per inch of width for each combination of
materials and constructions under test, and
8.1.1 1 Type of failure, that is, cohesive
failure within the adhesive or adherend, adhesion
to the adherend, or combinations
thereof, for each individual specimen.
26 I

4- SPECIMEN pull
METRIC EQUIVALENTS
in. 1 3 6 9 12
mm 25 76 152 229 305
FIG. 1 Test Panel and Test Specimen
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in
connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity
of any such patent rights, and the risk of infringement of such rights, ore entiret) their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyfive years
and if not revised, either reapproved or withdrawn. Your comments are invited eitherfor revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. Ifyou feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, Pa. 19103.
262

(Sib
Designation: D 2095 - 72 ~ 8 3
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa., 19103
Reprinted from the Annual Book ot ASTM Standards, Copyright ASTM
Standard Method of Test for
TENSILE STRENGTH OF ADHESIVES BY
MEANS OF BAR AND ROD SPECIMENS'
This Standard is issued under the fixed designation D 2095; the number immediately following the designation indicates
the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the
year of last reapproval.
1. scope
1.1 This method covers the determination
of the relative tensile strength of adhesives
by the use of bar- and rod-shaped butt-joined
specimens under defined conditions of preparation,
conditioning, and testing. The method
is applicable to the testing of adhesives with
various adherend materials in either similar
or dissimilar combinations.
NOTE I-Alternative test methods for determining
the tensile strength of adhesives are as follows:
ASTM Method D g97, Test for Tensile Properties
of Adhesive Bonds,-
ASTM Method D 1344, Testing Cross-Lay
Specimens for Tensile Properties of Adhesives;
and
ASTM Methods D 1205, Testing Adhesives for
Brake Lining and Other Friction Materials.'
2. Significance
2.1 Tension tests provide reasonably accurate
information with regard to the tensile
strength of adhesives. Tensile strength data
may be suitable for specification acceptance,
service evaluation, manufacturing control,
research, and development. Tension tests are
not considered significant for applications
differing widely from the test in rate, direction,
and type of loading.
3. Description of Term
3.1 The tensile strength of an adhesive is
the maximum tensile stress which it is capable
of sustaining. Tensile strength is calculated
from the maximum load during a tension
test carried to rupture and the original crosssectional
area of the specimen (see ASTM
Definitions E 6, Terms Relating to Methods
of Mechanical Testing)."
4. Apparatus
4.1 Testing Machine-A testing machine
capable of maintaining a specified rate of
loading and in which the error for indicated
loads that are to be measured shall not exceed
f 1 percent. The load-indicating mechanism
shall be essentially free of inertial lag
at a specified rate of loading. The accuracy of
the testing machine shall be verified in accordance
with ASTM Methods E 4, Verification
of Testing Machines.4 The testing machine
shall be provided with the following:
4.1.1 Fixed Member-A fixed or essentially
stationary member carrying one attachment
fixture.
4.1.2 Movable Member-A movable member
carrying a second attachment fixture.
4.1.3 Attachment Fixtures-Fixtures for
holding a test specimen between the fixed
member and the movable member. These
shall be of the self-aligning type. The fixtures
shall be attached to the fixed and movable
members and to the test specimen in such a
way that they will move into alignment as
soon as load is applied, so that the long axis
of the test specimen will coincide with the
direction of the applied load. A design for
fixtures that has proven satisfactory is shown
in Figs. 1 and 2.
4.2 Conditioning Room or Desiccators-
A conditioning room capable of maintaining a
' This method is under the jurisdiction of ASTM
Committee D-14 on Adhesives.
Current edition approved July 28, 1972. Published October
1972. Originally published D 2095 - 62 T. Last previous
edition D 2095 - 69.
-Annual Book ofASTMStandards, Part 16.
' Annual Book of ASTM Standards, Part 3 1.
Annual Book ofASTM Standards, Part 30.
263

elative humidity of 50 f 2 percent at 23 +
1 C (73.4 f 1.8 F) or desiccators containing
a saturated salt solution (Note 2) to give the
same relative humidity and temperature.
NOTE 2-A saturated salt solution of calcium
nitrate will give approximately 51 percent relative
humidity at 24.5 C (see ASTM Recommended
Practice E 104, Maintaining Constant Relative
Humidity by Means of Aqueous Solutions).4
5. Test Specimens
5.1 Description and Preparation-Bar- or
rod-type specimens shall be used in this test
method. The design of the specimens and
procedures used in preparing them shall be
in accordance with ASTM Recommended
Practice D 2094, Preparation of Bar and
Rod Specimens for Adhesion Tests.2
5.2 Number of Specimens-A minimum
of five specimens shall be tested for each
test condition.
6. Conditioning
6.1 All specimens, except those in which
both adherends are metals, shall be conditioned
prior to testing for at least 40 h at 50 f
1 C (73.4 f 1.8 F). Metal-to-metal bonds can
be tested as soon as the specimen has reached
an equilibrium temperature of 23 f 1 C
(73.4 f 1.8 F) after curing.
6.2 Special conditioning procedures may
be used by agreement between the purchaser
and the manufacturer when the tensile
strength of the adhesive at other conditions
is to be determined.
7. Procedure
7.1 Place the specimen in the testing machine
(see Fig. 2), using steel dowel pins and
fixtures such as those described in 4.1.3 and
start the loading. Conduct tests at other than
room temperature with a suitable temperature-controlled
test chamber enclosing the
fixtures and test specimen while assembled
in the testing machine.
7.2 Speed of Testing-Apply the load to
the specimen at the rate of 170 to 195 kg/cm’
(2400 to 2800 psi) of bond area per min, or,
if rate of loading is measured as crosshead
motion, set the testing machine to obtain the
foregoing rate of loading.
7.3 Record-Record the maximum load
carried by the specimen at failure. Estimate
D 2095
the percentage cohesion failure, adhesion
failure, contact failure, and adherend failure
on the basis of bond area by visual inspection
and record. If dissimilar adherends are used,
estimate and record the percentage adhesion
failure for each material. Discard specimens
that break at some obvious flaw and retest,
unless such flaws constitute a variable the
effect of which it is desired to study.
8. Calculations
8.1 Calculate the tensile strength by dividing
the breaking load by the area of the
bonded surface. Express this result in kilograms
per square centimeter (pounds per
square inch) and, if possible, report to three
significant figures.
8.2 For each series of tests, calculate the
arithmetic mean of all values obtained and
report this value as the average tensile
strength. This value shall be a result of no
fewer than five tests.
8.3 If it is desired to determine the standard
deviation and coefficient of variation, calculate
these values as follows and report to
two significant figures:
s = 4 (ZX2 - nX”)/(n - 1)
u = lOOs/R
where:
s = estimated standard deviation,
X = value of a single observation,
n = number of observations,
X = arithmetic mean of the set of observations,
and
u = estimated coefficient of variation.
9. Report
9.1 The report shall include the following:
9.1.1 Complete identification of the adhesive
tested, including type, sourcel manufacturer’s
code number, form, etc.,
9.1.2 Identification of materials used as
adherends and method of surface preparation
used,
9.1.3 Type of specimen (rod or bar) used
and dimensions of inserted sheet material, if
any,
9.1.4 Method of application of adhesive
and drying, precure and cure conditions used,
9.1.5 Average thickness of adhesive layer
after formation of the joint, within 0.001 in.
264

The method of obtaining the thickness of the
adhesive layer shall be described including
9.1.8 Test room conditions and temperature
of specimens at time of test,
procedure, location of measurements, and 9.1.9 Number of specimens tested,
range of measurements.
9.1.10 Speed of testing, and
9.1.6 Whether or not flash was removed 9.1.11 An average value of the tensile
and method employed, if any,
strength. Also, an average value of the per-
9.1.7 Conditioning procedure used, centage of each type of failure, that is, adhesion,
cohesion, contact, or adherend failure.
I
- I 31.75 t .13 mm. DU.
(1.250-i .005")
FIG. 1 Test Specimen and Attachment Fixtures.
265

D 2095
FIG. 2 Test Specimen with Attachment
Fixtures Assembled in Tension Testing Machine.
By publication of this standard no position is taken with respect to the validity of any patent rights in connection therewith,
and the American Society for Testing and Materials does not undertake to insure anyone utilizing the standard
against liability for infringement of any Letters Patent nor assume any such liability.
266

AMERICAN NATIONAL
STANDARD
ASTM D 2134 - 66 (Reapproved 1980)'
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
SOFTENING OF ORGANIC COATINGS BY PLASTIC
COMPOSITIONS'
This standard is issued under the fixed designation D 2134 the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval.
' NoTE-Editofial changes were made throughout in November 1980.
1. scope
1.1 This method covers the determination of
the relative degree of surface softening of organic
coating by plastic compositions under
specified exposure conditions.
1.2 This method is not applicable to plastic
compositions that may spew plasticizer under
the test conditions, as this will lead to spurious
results. The spewed plasticizer will slow the
rocker, yet the organic coating may be unaffected.
With unfamiliar plastic compositions a
microscopic examination of the organic coating
for possible spewing is recommended.
1.3 The values stated in SI units are to be
regarded as the standard.
2. Applicable Documents
2.1 ASTM Standards:
D 618 Conditioning Plastics and Electrical
Insulating Materials for Testing'
D 823 Producing Films of Uniform Thickness
of Paint, Varnish, Lacquer, and Related
Products on Test Panels3
3. Significance
3.i Organic coaihgs may be ~~~&p:ib!e to
softening as a result of contact by plastic compositions.
Plasticizer migration from the plastic
composition into the organic coating may cause
surface softening. The test result is significant
only for the specific surfaces in contact with
each other.
3.2 One important case of surface softening
is that which takes place when plasticized
poly(viny1 chloride) comes in contact with nitrocellulose
coatings. The degree of softening is
dependent on the plasticizer, the plasticizer
concentration, and the nitrocellulose lacquer
formulation.
4. Apparatus
4.1 Hardness Tester4-The hardness tester
shall consist of two flat, chromium-plated
bronze rings fmed together by a rack which
supports two bubble tube-type levels and
equipped with a vertical screw mounted from
the top of the rings. The levels are used to
measure the amplitude of the oscillations of the
hardness tester. The rate of change in amplitude
is used as a measure of the softness of the
test surface. The hardness tester shall meet the
following definitive characteris tics:
Weight
Diameter
Width between rings
Period
loof log
IO cm (4 in.)
2.5 cm (1 in.)
50 swings on glass plate in
60.0 f 0.5 s
Calibration Decrease in amplitude of 6
deg, taken between approximately
22 and 16 deg
from the vertical, after 50
swings on glass
The hardness tester should be equipped with a
clear cctiei to pioieet it from air cirrents dur;ig
operation. A suitable tester is illustrated in Fig.
1.
This method is under the jurisdiction of ASTM Committee
D-20 on Plastics and is the direct responsibility of
Subcommittee D20.15 on Thermoplastic Materials.
Current edition effective Sept. 20, 1966. Originally issued
1962. Replaced D 2134 - 62 T.
Annual Book of ASTM Standards, Parts 22,35, and 39.
Annual Book of ASTM Standards, Part 21.
The Sward Hardness Rocker, Model C, available from
Gardner Laboratory, Bethesda, Md., has been found satisfactory
for this purpose.
267

4.2 Glass Plates-Glass panels approximately
15 cm square and a minimum of 2 mm
thick are required. Preferably these should be
plate glass; however, carefully inspected window
glass without irregularities may be substituted.
4.3 Cushioning Material- Sponge rubber or
flexible urethane foam 1 to 2 cm thick and 15
cm square is required for even distribution of
the weight on the sample.
4.4 Barrier Material-Aluminum foil of any
commercial wrapping grade or other flexible,
impervious film can be used to prevent contamination
of the rubber or foam by plasticizer
migration.
4.5 Weights-Weights of 900 g (nominal 2
lb) including the top cover glass.
4.6 Photographic Roller-A hard rubber
roller approximately 100 mm in length is required
for pressing the plastic to the organic
coating.
4.7 Oven, laboratory-type, maintained at
50°C.
5. Test Specimens
5.1 The plastic specimen shall be a 50 by
100 by 0.25-mm (nominal 2 by 4 by 0.01-in.)
piece cut from a smooth uniform sheet. Embossed
or nonuniform samples may be remolded
to form smooth sheets.
5.2 The organic coating specimen shall be a
thin film on a glass panel with a dry thickness
of 0.025 to 0.05 mm (1 to 2 mils). See Appendix
for a suitable formulation for evaluation of
softening.
5.3 The film shall be dried or cured, or both,
using recommended conditions dependent
upon the type of organic coating. Only coatings
visually free of holes, craters, orange peel, or
other irregularities shall be used for this test.
6. Calibration of Hardness Tester
6.1 Calibrate the hardness tester on plate
glass placed on a leveling table. After the tester
is leveled, start oscillation of the tester so that
the bubble in the left-hand tube slightly overlaps
the mark. Place the cover in position and
start the count (beginning with zero) when the
bubble in the left-hand tube just fails to reach
the mark. Stop the count when the bubble in
the right-hand tube just fails to reach the mark.
6.2 The hardness tester shall make 50 com-
D 2134
plete oscillations in 60 0.5 s. If the number
of swings is not 50, adjust the angle of the lefthand
bubble tube to give the correct value. The
time for 50 swings can be changed by adjustments
in the position of the weight on the
vertical screw.
7. Conditioning
7.1 Conditioning-Condition the test specimens
at 23 k 2°C (73.4 k 3.6"F) and 50 & 5
% relative humidity for not less than 40 h prior
to test in accordance with Procedure A of Methods
D 618, for those tests where conditioning
is required. In cases of disagreement, the tolerances
shall be 1°C (&l.S"F) and 22 %
relative humidity.
7.2 Test Conditions-Conduct tests in the
Standard Laboratory Atmosphere of 23 * 2°C
(73.4 f 3.6"F) and 50 f 5 9% relative humidity,
unless otherwise specified in the test methods
or in this specification. In cases of disagreement,
the tolerances shall be * 1 "C (* 1.8"F)
and +2 9% relative humidity.
8. Procedure
8.1 Prepare two panels of the organic coatings
for each plastic composition to be tested.
Prior to testing, condition the panels for 7 days
at the conditions specified in Section 7.
8.2 Determine the initial hardness of the
coated panel in duplicate, using the procedure
in Section 6, measuring parallel to the long
direction of the coating. The number of complete
oscillations multiplied by 2 gives the hardness
value.
NOTE 1-The rings of the hardness tester should
be cleaned after each measurement with acetone or
other suitable solvent and polished with a dry cloth.
8.3 Heat the coated panel and plastic specimen
in an oven at 50°C for 30 min and place
the warm plastic specimen carefully on the
organic coating surface, using the roller to ensure
uniform contact between the specimen and
panel. Use extreme care to prevent entrapment
of air or dust particles under the plastic specimen.
NOTE 2-With clear organic coatings inspect the
panel from the back side to determine if uniform
contact has been made.
8.4 Cover the plastic specimen with the barrier
material, sponge rubber, and the cover
plate in that order, and add sufficient weight to
-
268

D 2134
make 900 g (including top cover plate). To
expedite attainment of temperature equilibrium
in the mass, precondition the weight and
cover glass at 50°C for a minimum of 1 h
immediately before use.
8.5 Place the sandwich in the 50°C oven for
4 h. At the end of this time, disassemble the
sandwich retaining the plastic specimen in a
dust-free atmosphere.
8.6 Condition the coated panel as in Section
7 for a period of 4 to 24 h. Determine the
hardness as in Section 6.
8.7 Reassemble the sandwich, return to the
oven for an additional 20-h exposure, and repeat
the hardness measurement.
9. Calculations
9.1 Calculate the average initial hardness
and hardness after 4 and 24-h exposures.
9.2 Compute the percentage softening as follows:
Softening, % = [(Ifo - H)/Ho] X 100
where:
Ho = hardness on unexposed panel, and
H = hardness on exposed panel.
10. Report
10.1 The report shall include the following:
10.1.1 Identification of the plastic specimen,
10.1.2 Identification of the organic coating,
and
10.1.3 Average percentage softening for
each contact time.
11. Precision
11.1 Inter- and intralaboratory tests in the
range from 30 to 80 % softening may be expected
to give 95 % confidence limits of the
order f 10 %. Limits for the 4-h test may be
expected to be somewhat higher than those for
the 24-h test.
FIG. 1 Rocker Hardness Tester
APPENDIX
XI. LACQUER FQR EVALUATION OF SOFTENING
X1.1 Formulation
Xl.l.1 For evaluation of softening of nitrocellulose
lacquer by poly(viny1 chloride) film, the following
lacquer formulation has been found to be suitable
when freshly prepared (Note Xl):
Parts by
Weight
%-s nitrocellulose (30 % butyl wet)
110.0
Alkyd resin (60% in xylene)A 131.0
Raw castor oilB 18.5
Dioctyl phthalate 18.0
Methyl ethyl ketone 55.0
Methyl isobutyl ketone 169.0
Diisobutyl ketone 22.0
Isopropyl alcohol 53.2
Xylene 38.2
Toluene 143.5
Ethylene glycol monobutyl ether - 15.2
113.6
A Duraplex ND-77B made by the Rohm and Haas Co.,
Philadelphia, Pa., or equivalent, has been found satisfactory
269

for this purpose.
* Bakers AA made by the Baker Castor Oil co., Bayonne.
N. J., or equivalent, has been found satisfactory for this
purpose.
NOTE X1-Methods D 823, outlines detailed procedures
for producing uniform films of lacquers.
X1.2 Application
XI .2.1 A 0.075-” (3”ii) wet film of the above
lacquer shall be applied to a glass panel by blade
application. The film shall be dried for 24 h at room
temperature, followed by 2 h at 60°C and then
conditioned as prescribed in Section 7.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in
conneciion with any iiem mentioned in this standard. Users of this standard are expressly advised that determination of the validity
of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyjve years
and ynot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of ihe
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, Pa. 19103, which will schedule a
further hearing regarding your comments. Failing satisfaction there, you may appeal to the ASTM Board of Directors.
270

Designation: D 2196 - 86
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St. Philadelphia. Pa 19103
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
If not listed in the current combined index will appear in the next edition
Standard Test Methods for
RHEOLOGICAL PROPERTIES OF NON-NEWTONIAN
MATERIALS BY ROTATIONAL (BROOKFIELD) VISCOMETER'
This standard is issued under the fixed designation D 2 196: the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (t) indicates an editorial change since the last revision or reapproval.
Thiw iiw mi.rhod.v havc hcvn upprond.li)r iisi' by uginc~ii>s i?/'/hc Dqurimcvii (!/'Dc:livsi~ io ripla~i~ .Wihod 4 37 o/' Fdcrul 7iw
Merhtd Siandard No. 141.4 und,/i)r lisring in ihcp DoD 1ndi.r c?/Spi~c~/ic~urions and Siundurds.
1. Scope
1.1 These test methods cover the determination
of the apparent viscosity and the shear thinning
and thixotropic properties of non-Newtonian
materials in the shear rate range from 0.1 to
50 s-I.
I .2 This standard may involw hazardoirs marcv-ials.
oprvutions, and cqiqlripmcwt. This standard
does no[ purport to address all qftiic sqfi.ry proh-
1cm.s associarcJd with its use. It is the rc~sponsibility
of'Ihc usor ofthis standard to establish appro-
priatc sufiyv and hdh practices and dctijrminc'
rhc upplicabiliry oJ'rcJgirlulory limitations prior IO
l(SC.
2. Referenced Document
2.1 ASTM Standard:
E I Specification for ASTM Thermometers'
3. Summary of Test Methods
3.1 Test Method A consists of determining
the apparent viscosity of coatings and related
materials by measuring the torque on a spindle
rotating at a constant speed in the material.
3.2 Test Methods B and C consist of determining
the shear thinning and thixotropic (timedependent)
rheological properties of the materials.'
The viscosities of these materials are determined
at a series of prescribed speeds of a rotational-type
viscometer. The agitation of the material
immediately preceding the viscosity measurements
is carefully controlled.
4. Significance and Use
4.1 Test Method A is used for determining
the apparent viscosity at a given rotational speed,
although viscosities at two or more speeds better
characterize a non-Newtonian material than does
the single viscosity measurement.
4.2 With Test Methods B and C. the extent of
shear thinning is indicated by the drop in viscosity
with increasing viscometer speed. The degree
of thixotropy is indicated by comparison of viscosities
at increasing and decreasing viscometer
speeds (Test Method B). viscosity recovery (Test
Method B), or viscosities before and after high
shear (combination of Test Methods B and C).
The high-shear treatment in Test Method C approximates
shearing during paint application.
The viscosity behavior measured after high shear
is indicative of the characteristics of the paint
soon after application.
5. Apparatus
5. I Rotational-type viscometers having at
least four speeds, such as:
5.1 . I Brookfirld I 'isc*omc~ter.'' Model LVF.
having four rotational speeds, or Model LVT
ha. ing eight rotational speeds, with set of four
spindles; or
5.1.2 Brookfidd Viscwmc~ter, Model RVF,
having !-mi. ;ota:iona! speeds. or Mode! R!'T
' These test methods are under the jurisdiction of ASTM
Committee D-l on Paint and Related Coatings and Materials
and are the direct responsibility of Subcommittee DO1.24 on
Physical Properties of Liquid Paints and Paint Materials.
Current edition approved Aug. 29. 1986. Published October
1986. Originally published as D 2 I96 - 63 7'. Last previous edition
D 2196 - XI.
* ..inmu/ Rook 0/':1S7"'t4 L%ndurd.s. Vol I4.01.
' Pierce. P. E., "Measurement of Rheology of Thixotropic
Organic Coatings and Resins with the Brookfield Viscometer."
Joftrnul o/'/'uin~ 1i.c~hnolog.r. Vol 43. No. 557. 197 I , pp. 35-43.
' Brookfield viscometers are availablc from the Hrooklicld
Engineering Laboratories. Inc.. 240 Cushing St.. Stoughton. MA
02072.
27 I

D 2196
having eight rotational speeds, with set of seven
spindles.
5.2 T~~crinotni~li~r-ASTM thermometer having
a range from 20 to 70°C and conforming to
the requirements for Thermometer 49C as prescribed
in Specification E I.
5.3 C'onrainiw, round I-pt (0.5-L) can, 3% in.
(85 mm) in diameter, or I-qt (I-L) can, 4 in. (100
mm) in diameter.
5.4 Shaker,' or equivalent machine capable of
vigorously shaking the test specimen.
6. Materials
6. I Siandard Oils,6 calibrated in absolute viscosity,
millipascal seconds.
7. Calibration of Apparatus
7. I Select at least two standard oils of viscosities
differing by at least 5 P (0.5 Pa.s) within the
viscosity range of the material being measured
and in the range of the viscometer. Condition
the oils as closely as possible to 25.0"C (or other
agreed-upon temperature) for I h in a I-pt (0.5-
L) can, 3% in. (85 mm) in diameter. Measure
the viscosities of each oil as described in Test
Method B (Section 13) taking readings only at
increasing speeds (13.7). Make certain that the
spindle is centered in the container prior to taking
measurements.
Nore I-The Brookfield LV and RV series viscometersare
equipped with a spindle guard leg. The spindle/
speed multiplying factors (Table I ) are designed for use
with the guard leg in place except for the following
conditions: RV series when the factors are the same
with or without the guard leg for spindles No. 3 through
7; or LV series when the factors are the same with or
without the guard leg for spindles No. 3 and 4.
7.1.1 Calibration in a I-pt (0.5-L) can is always
possible with the LV series viscometer with
the guard leg attached. Calibration of the RV
series viscometer in the I-pt can must be done
with spind!es No. 3 through 7 without the guard
leg. If the No. 1 or No. 2 spindles are to be used,
calibration is carried out in the I-qt (I-L) can
with the guard leg attached.
7.2 Combining the tolerance of the viscometer
(k 1 %, equal to the spindle/speed factor) and the
tolerance of the temperature control (typically f
0.5"C at 25°C) it is reasonable to assume that a
viscometer is calibrated if the calculated viscosities
are within +_5 % of the stated values (see
Table 2 for examples of the considerable change
in viscosity with temperature exhibited by stand-
ard oils). If measurements are not made at 25°C'.
then the stated viscosities should be corrected to
the temperature at which they are measured. If
the viscosities determined in 7. I differ from the
stated values of the viscosity standard by more
than 5 %, calculate new factors for each spindle/
speed combination as follows:
1 = 1 (1)
where:
1' = new factor for converting scale reading to
viscosity, CP (mPa.s),
1' = viscosity of standard oil. mPa.s, and
s = scale reading of the viscometer.
7.3 Prepare a table of new factors similar to
that furnished with the viscometer (Table I) for
the spindle/speed combinations worked out in
7.2. Spindle/speed factors vary inversely with
speed.
8. Preparation of Specimen
8.1 Fill a I-pt or I-qt can with samplc to
within 1 in. (25 mm) of the top with the sample
and bring it as close as possible to a temperature
of 25°C or other agreed-upon temperature prior
to test.
8.2 Vigorously shake the specimen on the
shaker or equivalent for 10 min, remove it from
the shaker, and allow it to stand undisturbed for
60 min at 25°C prior to testing (Note 2). Start
the test no later than 65 min after removing the
can from the shaker. Do not transfer the specimen
from the container in which it was shaken.
Noli 2-Shake time may be reduced if necessary.
or as agreed upon between the purchaser and manufacturer,
but, in any case. should not be less than 3 min.
IESI' MFrHOL) A-APPARENT
VISCOSI'I'Y
9. Procedure
9.1 Make all measurements as close as possib!e
to 25°C. or other agreed-upo:: temperatiire.
9.2 Place the instrument on the adjustable
stand. Lower the viscometer to a level that will
immerse the spindle to the proper depth. Level
the instrument using the attached spirit level.
9.3 Tilt the selected spindle (Note 3). insert it
A reciprocating shaker may be obtained from the Ked Devil
Tools. 2400 Vauxhall Rd.. Union. NJ 07083.
Absolute viscosity standards arc availahle in I-pt samples
from The Cannon Instrument Co.. P.O. Box 16. State College.
PA 16801. or Brooklield Engineering Laboratories. Inc., 240
Cushing SI.. Stoughton. MA 02072.
272

0 2196
into one side of the center of the surface of the
material. and attach the spindle to the instrument
as follows: Firmly hold the upper shaft coupling
with thumb and forefinger: screw left-hand
thread spindle coupling securely to the upper
shaft coupling being very careful when connecting
to avoid undue side pressure which might
affect alignment. Avoid rotating the dial so that
pointer touches the stops at either extreme ofthe
scale.
NOTI: 3-Select the spindle/speed combination that
will give a minimum scale reading of IO but preferably
in the middle or upper portion of the scale. The speed
and spindle to be used may differ from this by agreement
between user and producer.
9.4 Lower the viscometer until the groove
(immersion mark) on the shaft just touches the
material. Adjust the viscometer level if necessary.
Move the container slowly in a horizontal plane
until the spindle is located in approximately the
center ofthe container so that the test will be run
in a region undisturbed by the lowering of the
spindle.
9.5 Turn on the viscometer. Adjust the viscometer
to the rpm selected (Note 3) for the
material under test. Allow the viscometer to run
until the pointer has stabilized (Note 4). After
the pointer has stabilized. depress the clutch and
switch ofT the motor so that when it stops, the
pointer will bc in view (Note 5).
No~ir 4-In thixotropic paints. the pointer does not
always stabilize. On occasion it reaches a peak and then
gradually declines as the structure is broken down. In
these cases. the time of rotation or number of revolutions
prior to reading the viscometcr should hc agreed
to between user and manufacturer.
Noli: 5-Always release the clutch while the spindle
is still immersed so that the pointer will float. rather
than snap back to zero.
10. Calculation
10.1 Calculate the apparent viscosity at each
speed, as foliows:
1,' = ,/.v
where:
1' = viscosity of sample in centipoises, mPa.s,
,/' = scale factor furnished with instrument (see
Table I), and
.Y = scale reading of viscometer.
11. Report
I 1. I Report the following information:
1 I. I. 1 The Brookfield viscometer model and
spindle,
I I. 1.2 The viscosity at the spindle/speed utilized.
1 I. 1.3 The specinien temperature in degrees
celsius, and
I I. I .4 The shake time and rest period, if other
than specified.
12. Precision and Bias
12. I t'rc~c'isior+--See Section 23 for precision.
including that for measurement at a single speed.
12.2 Bia.v-No statement of bias is possible
with this test method.
'IES'I' $1 ET1 10D B--VISCOSIT\' 1N DER
CIiANGINC; SPEED CONDITIONS, DECREE
OF SIIEAR 'I'I1INNINC AND THISO?'ROP\'
13. Procedure
13. I Make all measurements with the Brookfield
viscometer as close as possible to 3°C. or
ot her agreed upon tempera t u rc.
13.2 Adjust thc instrument and attach the
spindle as in 9.2 through 9.4.
13.3 Set the viscometer at the slowest rotational
speed (Notes 5 and 6). Start the viscometer
and record the scale reading after ten revolutions
(or other agreed-upon number of revolutions).
Noli: 6-When the eight speed viscometers (RVT
and LVT) are used. lower or higher speeds than that
permitted by the four speed viscometers may be used
upon agreement between producer and user.
13.4 Increase the viscometer speed stepwise
and record the scale reading after ten revolutions
(or equivalent time for each spindle/speed combination)
at each speed. After an observation has
been made at the top speed. decrease the speed
in steps to the slowest speed. recording the scale
reading after ten revolutions (or equivalent time)
at each speed.
NOTI: 7-11 is preferable to change speed when the
motor is running.
13.5 After the last reading has been taken at
the slowest speed, shut off the viscometer and
allow it and the specimen to stand undisturbed
for an agreed-upon rest period. At the end of the
rest period, start the viscometer at the slowest
speed and record the scale reading after ten revolutions
(or other agreed-upon number of revolutions).
14. Calculations and Interpretation of Results
14. I Calculate the apparent viscosity at each
273

D 2196
speed as shown in Section 9.
14.2 If desired, determine the degree of shzar
thinning by the following method:
14.2.1 Shear Thinning Index (sometimes erroneously
called the thixotropic index)-Divide
the apparent viscosity at a low rotational speed
by the viscosity at a speed ten times higher.
Typical speed combinations are 2 and 20 rpm, 5
and 50 rpm, 6 and 60 rpm but selection is subject
to agreement between producer and user. The
resultant viscosity ratio is an index of the degree
of shear thinning over that range of rotational
speed with higher ratios indicating greater shear
thinning.
14.2.2 A regular or log-log plot of viscosity
versus viscometer speed in rpm may also be
useful in characterizing the shear-thinning behavior
of the material. Such plots may be used for
making comparisons between paints or other
materials.
14.3 If desired, estimate the degree of thixotropy
(under conditions of limited sheanng-out
of structure) by one of the following methods:
14.3.1 Calculate the ratio of the slowest speed
viscosity taken with increasing speed to that with
decreasing speed. The higher the ratio, the greater
the thixotropy.
14.3.2 Calculate the ratio of the slowest speed
viscosity taken after the rest period to that before
the rest period. The higher the ratio, the greater
the thixotropy.
15. Report
15.1 Report the following information:
15. I . 1 The Brookfield viscometer and spindle,
I 5.1.2 The viscosities at increasing and decreasing
spindle speeds,
15.1.3 The rest period time and the viscosity
at the end of that time.
15.1.4 The specimen temperature in degrees
Celsius; and
15. I .5 The shake time if other than that specified.
15.2 Optionul Reporting:
15.2.1 Degree ofshear Thinning-Shear thinning
index and speeds over which it was measured
(14.2).
15.2.2 Esrimated Degree qf Thixorrop-v (under
conditions of limited shearing-out of structure)-
Ratio of the lowest speed viscosities, for both
increasing and decreasing speeds; or ratio of the
lowest speed viscosities before and after the rest
period, and speed at which they were measured
(14.3).
16. Precision and Bias
16.1 Precision-See Section 23 for precision,
including that for measurement of the shear thinning
index (ratio of viscosity at 5 r/min to that
at 50 r/min). It has not been possible to devise a
method for determining precision for viscosities
at increasing and decreasing speeds other than as
individual measurements. No attempt was made
to determine the precision of the measurement
of the degree of thixotropy because this parameter
is dependent on the material, the time of the
test, and other variables.
16.2 Bias-No statement of bias is possible
with this test method.
TEST METHOD c-vIscosrrY AND SHEAR
THINNING OF A SHEARED MATERIAL
17. Apparatus
17.1 High-speed laboratory stirrer with speeds
of at least 2000 rpm and equipped with a 2-in.
(50-mm) diameter circular dispersion blade.'
18. Preparation of Specimen
18.1 Insert the 241-1. (SO-mm) blade into the
center of the can (4.3) so that the blade is about
I in. (25 mm) from the bottom. Run the mixer
at 2000 rpm (Note 8) for 1 min.
NOTE &-Materials may be sheared at other speeds
using other size blades upon agreement between producer
and user.
19. Procedure
19.1 Immediately insert the same spindle used
in Test Method B into the sheared material in
the same manner as in Section 9.
19.2 Start the viscometer and adjust to the
highest speed used in Test Method B (13.5).
R~CGK! the ~ a!e reading after ten r ~ d i i t(ai
i ~ ~
other agreed-upon number of revolutions).
19.3 Decrease the viscometer speed (Note 7)
step-wise and record the scale readings at each
speed down to the lowest speed used in Test
Method B, recording the scale reading after ten
revolutions at each speed (or other agreed-upon
number of revol ut ions).
-~ .
'Cowles or Shar type mixer/disperser
274

D 2196
20. Calculations and Interpretation of Results
20.1 As in Test Method B. calculate the viscosities
at each decreasing speed.
20.2 If desired. calculate the degree of shear
thinning by the method given in Test Method B,
14.2. The measured viscosity behavior after
shearing is essentially that of the paint immediately
after application (disregarding changes in
solids).
20.3 If desired. estimate the degree of thixotropy
(under conditions of cotnplufc shearing-out
of structure) by calculating the ratio of the lowest
speed viscosities before and after shear. The lowest
speed before-shear viscosity is taken from Test
Method B. 14.1. at the lowest increasing speed.
The lowest speed after-shear viscosity is taken
from 20. I. The higher the ratio. the greater the
thixotropy.
21. Report
2 1. I Report the following information:
2 1.1.1 The Brookfield viscometer model and
spindle,
2 I. 1.2 The viscosities at decreasing spindle
speeds.
2 I . I .3 The specimen temperature in degrees
Celsius. and
2 1. I .4 The speed of the high-speed mixer. size
of blade. and time of mixing if different from
method.
2 1.2 Optioml Rcportin&y:
2 I 2.1 Dqrw of'Siiwr 77iirrtiiu,q--Shear thinning
index and speed over which it was measured
(14.1).
2 1.2.2 E.vlirnuttd 7/ii.\-orro~pl.-Ratio of lowest
speed viscosities before and after shear and
the speed at which they were measured.
22. Precision and Bias
22. I frc.cSi.sion--The precision for individual
viscosity measurements is the same as for Test
Method A in Section 23. No attempt has been
made to determine the precision of the shear
thinning index or degree of thixotropy for Test
Method C for the reasons given in 16.1.
22.2 Bias-No statement of bias is possible
with this test method.
23. Summary of Precision
23. I In an interlaboratoq study of Test Methods
A and B. eight operators in six laboratories
measured on two days the viscosities of four
architectural paints comprising a latex flat. a
latex semi-gloss. a water-reducible gloss enamel.
and an alkyd semi-gloss. that cobered a reasonable
range in viscosities and were shear thinning.
Measurements at increasing speeds of 5. 10. 30.
and SO r/min (equivalent to eight operators testing
16 samples) were used to obtain the precision
of Test Method A. The within-laboratory coetlicient
of variation for Tesr Method A (single
speed) was found to be 3.49 % with I I! I degrees
of freedom and for Test Method B (Shear Thinning
Index) 3 3 with 31 degrees of freedom.
T tie corresponding between-laboratories coe t?icicnts
are 7.68 CO with 105 degrees of freedom
and 7.63 % with 27 degrees of freedom. Based
on these coefficients the following criteria should
be used for judging the acceptability of results at
the 95 7; confidence level:
23. I . 1 R~J/~~i~ilti/Ji/ir~-TWO results obtained
by thc same operator at different times should be
considered suspect if they differ by more than
7 "0 relative for single speed viscosity and 9.5 5;
relative for shear thinning index.
23. I .2 Riprc,dirc.ihi/ifl.-Two results obtained
by operators in different laboratories should be
considered suspect if they differ by more than
21.6 and 22.1 9; relative. respectively. for the
same two test methods.
275

D 2196
TABLE 1 Factors for Converting Brookfield Dial Readings
to Centipoises (MillipascPI seconds)
NOTE-M = 1000.
RV Series Factors Spindles
Speed'rpm I 2 3 4 5 6 7
0.5 200 800 2000 4000 8000 20M 80M
I 100 400 1000 2000 4OOO IOM 40M
2 50 200 500 1000 2000 5M 20M
2.5 40 160 400 800 1600 4M 16M
4 25 100 250 500 1000 2.5M IOM
5 20 80 200 400 800 2M 8M
IO IO 40 100 200 400 IM 4M
20 5 20 50 100 200 500 2M
50 2 8 20 40 80 200 800
100 I 4 IO 20 40 100 400
Speed. rpm
0.3
0.6
1.5
3.0
6
12
30
60
LV Series Factors Spindles
I 2 3 4
200 1000
100 500
40 200
20 100
IO 50
5 25
2 IO
I 5
4000
2000
800
400
200
100
40
20
20M
1 OM
4M
2M
IM
500
200
100
TABLE 2 Viscosity Variation of Cannon Viscosity
Standards About the 25°C Temperature Point
Cannon Viscosity
Standard
Viscosity at Viscosity Change With
25°C. CP + I'C at 25'C. CP
(m Pa. s) (mPa.s)
s-600 I 400 87.7 (6.26 96)
s-2Ooo 4 900 332 (6.77 %)
S-8000 20 000 1462.3 (7.31 %)
The American Societyji)r Testing and Materials tuk1.s no position rtqmting the validity (!/'any putivt rights assc~rtc~d in conncr'tion
with any item mentioned in this standard. Users of this standard are expriwly advised that determination o/'ihc salidity of any .sidi
parent rights, and the risk if infringement of such rights. are entire1.v their own re.~pon.sihility.
This standwd is suhject to revision at any time by the responsible. tcvhnical committee and must he rtviiwed evc~rv,fiw .wars and
if not revised, either reapproved or withdrawn. Your comments are invited (.ither ,J>r revision of this standard or ji)r additional
standards and should be addwssed to ASTM Headquarters. Your comments will rcwive careful tnnsidi~ration at a mcvting of thc~
ri~.spon,sible technical committee, which you may attend. (f,vou!&el that your commmts have not received a ,/air hmring ,you should
make your views known to the ASTM Committee on Standards. 1916 Raw St., Philadelphia. PA 19103.
276

4sIE,
Designation: D 2240 - 86
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
RUBBER PROPERTY-DUROMETER
HARDNESS'
This standard is issued under the fixed designation D 2240 the number immediately following the designation indicates the year of
original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (6) indicates an editorial change since the last revision or reapproval.
This iwthod hus hivn upprovi~d,fi)r usi' hr ugiwcies o?/'~hi~ Diymtmiwr ((Di:/i*n.si, IO rcpluiv mi*thid.v 531 1. I and 5321 in Fivhd
T~w .tli~lliod Slundurd 6001 und mchd 1084 of Frdc.rcrl TiW Mi~~litd Stundurd 406. and 1i)r listing in !hi. DoD Inder 4'
.Spir.ilii~utions und 9undard.s.
1. Scope
1.1 This test method covers two types of durometers,
A and D, and the procedure for determining
the indentation hardness of homogeneous
materials ranging from soft vulcanized rubber
to some rigid plastics.
1.2 This test method is not applicable to the
testing of coated fabrics.
1.3 The values stated in SI units are to be
regarded as the standard.
1.4 This stundurd muy involvc huzurdoirs mutcvkds.
operutions. und eyiripmcnt. This stundurd
doe.s not purport to uddrcss all ofthc safi>tp prohkms
u.s.sociutid with its IISY. It is thc~ responsibilit!.
of' whocwr irws this standard to consrrlt und
cstuhlish uppropriuto .safi,ry and hcwlth pruct ices
unddctrrminc. the upplicuhility qfrquiutor.v limitutions
prior to iise
2. Applicable Documents
2.1 ASTM Stundurd.s:
D530 Methods of Testing Hard Rubber
Products2
D 618 Methods for Conditioning Plastics and
Electrical Insulating Materials for Testing3
D 785 Test Method for Rockwell Hardness of
Plastics and Electrical Insulating Materials3
D 1349 Practice for Rubber-Standard Temperatures
and Atmospheres for Testing and
C~nditioning~.~
D 1415 Test Method for Rubber Property-
International Hardness*
D 3040 Practice for Preparing Precision Statements
for Standards Related to Rubber and
Rubber
NOTE I-The specific dated edition of Practice
D 3040 that prevails in this document is referenced in
the Precision section.
3. Summary of Methods
3.1 The Type A durometer is used for measuring
softer materials, and the Type D for harder
materials (see Note 6. Section 9). This test
method permits hardness measurements based
on either initial indentation or indentation after
specified periods of time, or both.
4. Significance and Use
4.1 This test method is based on the penetration
of a specified indentor forced into the material
under specified conditions. The indentation
hardness is inversely related to the penetration
and is dependent on the elastic modulus and
viscoelastic behavior of the material. The shape
of the indentor and the force applied to it influence
the results obtained so that there may be no
simple relationship between the results obtained
with one type of durometer and those obtained
with either another type of durometer or another
instrument for measuring hardness. This test
method is an empirical test intended primarily
for control purposes. No simple relationship exists
between indentation hardness determined by
' This test method is under the jurisdiction of ASTM Committee
D-l I on Rubber and is the direct responsibility of Subcomittee
DI I. IO on Physical Tests.
Current edition approved March 27, 1986. Published May
1986. Originally published as D2240-64 T. Last previous
edition D 2240 - 85.
Annual Book of ASTM Slundards. Vol09.0 I.
'Annual Book of ASTM Standards. Vol08.0 I.
'Annual Book ofASTM Standard.% Vol 09.02.
277

this test method and any fundamental propert)
of the material tested. For specifcation purposes,
it is recommended that Method D 14 I5 be used
for soft materials and Method A of Method
D 530 or Method D 785 be used for hard materials.
5. Apparatus
5.1 Hardness-measuring apparatus or durometer
consisting of the following components:
5.1.1 Pressor Foot with a hole having a diameter
between 2.5 and 3.2 mm (0. IO and 0.13
in.) centered at least 6 mm (0.25 in.) from any
edge of the foot.
5. I .2 Indentor formed from hardened steel
rod with a diameter between 1.15 and 1.40 mm
(0.045 and 0.055 in.) to the shape and dimensions
shown in Fig. I for Type A durometers or
Fig. 2 for Type D durometers.
5.1.3 Indicating Device on which the amount
of extension of the point of indentor may be read
in terms of graduations ranging from zero for full
extension of 2.46 to 2.54 mm (0.097 to 0.100
in.) (Note I) to 100 for zero extension obtained
by placing presser foot and indentor in firm
contact with a flat piece of glass.
NOTE 2-Type A Shore Durometers serial numbers
I through 16 300 and 16 351 through 16 900
and Type A-2 Shore Durometers numbers I through
8077 do not meet the requirement of 2.46 to 2.54 mm
(0.097 to 0.100 in.) extension of the indentor at zero
reading. These durometers will give readings which are
low by amounts ranging from 3 units at 30 hardness to
I unit at 90 hardness.
5. I .4 Calibrated Spring for applying force to
the indentor in accordance with one of the following
equations:
Force. N = 0.550 + 0.075 HA (1)
where HA is the hardness reading on a Type A
durometer, and
Force, N = 0.4445HD (2)
where HD is the hardness reading on a Type D
durometer.
6. Test Specimen
6.1 The test specimen shall be at least 6 mm
(0.25 in.) in thickness unless it is known that
identical results are obtained with a thinner specimen
(Note 2).A specimen may be composed of
plied pieces to obtain the necessary thickness, but
determinations made on such specimens may
not agree with those made on solid specimens
because the surfaces between plies may not be in
complete contact. The lateral dimensions of the
specimen shall be sufficient to permit measurements
at least 12 mm (0.5 in.) from any edge
unless it is known that identical results are obtained
when measurements are made at a lesser
distance from an edge. The surface of the specimen
shall be flat over sufficient area to permit
the presser foot to contact the specimen over an
area having a radius of at least 6 mm (0.25 in.)
from the indentor point. A suitable hardness
determination cannot be made on a rounded,
uneven, or rough surface.
NOTE 3-The minimum requirement for the thickness
of the specimen is dependent on the extent of
penetration of the indentor into the specimen; that is.
thinner specimens may be used for materials having
hardness values at the upper end of the scale. The
minimum distance from the edge at which measurements
may be made likewise decreases as the hardness
increases. For materials having hardness values above
50 Type D durometer. the thickness of the specimen
should be at least 3 mm (0. I2 in.) and measurements
should not be made closer than 6 mm (0.25 in.) to any
edge.
7. Calibration
7.1 The spring can be calibrated by supporting
the durometer in a vertical position and resting
the point of the indentor on a small spacer at the
center of one pan of a balance as shown in Fig.
3 in order to prevent interference between presser
foot and pan (Note 3). The spacer shall have a
small cylindrical stem approximately 2.5 mm
(0.1 in.) in height and 1.25 mm (0.05 in.) in
diameter, and shall be slightly cupped on top to
accommodate the indentor point. Balance the
mass of the spacer by a tare on the opposite pan
of the balance. Add known masses to the opposite
pan to balance the force on the indentor at
various scale readings. The measured force (9.8
x mass in kilograms) shall equal the force a!-
culated by either Eq I within +. 0.08 N or Eq 2
within & 0.44 N.
NOTE 4-Instruments specifically designed for calibration
of durometers may be used. Zwick & co..
Control Equipment 7501, can be used for calibration
as it is capable of measuring or applying a force on the
point of the indentor within 0.004 N for a Type A
durometer and within 0.02 N for a Type D durometer.
Zwick Control Equipment 7501 with serial numbers
higher than WA-20301 are satisfactory for this work.
Instruments with lower serial numbers must be modified.
278

eb
7.2 Frequent checks in between calibrations
in accordance with 7. I, of the indentor by means
of a test block supplied by the manufacturer
should be made to monitor the condition of the
indentor relative to possible wear or damage.
8. Conditioning
8.1 Tests shall be made at 23 f 2°C (73.4 f
3.6’F) if the temperature of test is not specified.
When tests are made at other temperatures, it is
recommended that they be made at one or more
of the standard temperatures given in Practice
D 1349 or Procedure A of Method D618. The
specimens shall be conditioned at the temperature
of test for at least I h before test for materials
whose hardness is not dependent on the relative
humidity. For materials whose hardness is dependent
on the relative humidity, the specimens
shall be conditioned in accordance with Procedure
A of Method D 6 I8 and tested at the same
conditions.
9. Procedure
9.1 Place the specimen on a hard, horizontal
surface. Hold the durometer in a vertical position
with the point of the indentor at least 12 mm
(0.5 in.) from any edge of the specimen, unless it
is known that identical results are obtained when
measurements are made with the indentor at a
lesser distance. Apply the pressor foot to the
specimen as rapidly as possible without shock,
keeping the foot parallel to the surface of the
specimen. Apply just sufficient pressure to obtain
firm contact between pressor foot and specimen.
NOTE 5-Better reproducibility may be obtained by
using either a durometer stand or a mass centered
on the axis of the indentor or both to apply the presser
foot to the specimen. Recommended masses are I kg
for the Type A durometer and 5 kg for the Type D
durometer.
9.2 Unless otherwise specified,
. .
read the scale
ratory program with three materials of varying
within i s ;after the ~ ~TSSH f30: is ifi firm c~nta~c!
with the specimen, unless the durometer has a
maximum indicator, in which case the maximum
reading is taken. If a reading after a time interval
is specified, hold the presser foot in contact with
the specimen without change in position or pressure
and read the scale after the period specified.
NOTE 6-Durometers having only a maximum indicator
cannot be used to obtain hardness values at
various time intervals, nor in testing vinyl plastics which
require the reading to be taken at I5 s.
9.3 Make five measurements of hardness at
D 2240
different positions on the specimen at least 6 mm
(0.25 in.) apart and determine the median value
or the arithmetic mean.
NOTE 7-It is recommended that measurements
be made with the Type D durometer when values above
90 are obtained with the Type A durometer and that
measurements be made with the Type A durometer
when values less than 20 are obtained with the Type D
durometer. Values below IO Type A are inexact and
should not be reported.
10. Report
10.1 The report shall include the following:
10. I. 1 The hardness value obtained.
IO. I .2 Complete identification of material
tested, including date of vulcanization,
IO. I .3 Description of specimen, including
thickness and number of pieces plied. if less than
6 mm (0.25 in.).
IO. I .4 Temperature of test if other than 23°C.
and relative humidity when hardness of material
is dependent on humidity.
10.1.5 Type and manufacture of durometer,
IO. I .6 Indentation hardness time interval at
which reading was taken (Note 7). and
IO. 1.7 Date of test.
NOTI 8-Readings may be reported in the form: A/
45/15 where A is the type of durometer. 45 the reading.
and I5 the time in seconds that the pressure foot is in
firm contact with the specimen. Similarly. D/60/1 indicates
a reading of 60 on the Type D durometer
obtained either within I s or from a maximum indicator.
11. Precision and Bias’
I 1.1 These precision and bias statements have
been prepared in accordance with Practice
D 3040 - 8 I. Refer to Practice D 3040 for terminology
and other testing and statistical concepts.
I 1.2 The LQC precision for both Type A and
D methods was determined from an interlabo-
hardness, in each range, with SIX participating
laboratories. Tests were conducted on two separate
days in each laboratory for both the A and
D programs. All materials were supplied from a
single source.
1 1.3 A test result for hardness (both A and D)
was the median of five individual hardness readings
on each day in each laboratory.
11.4 Table 1 gives the precision results for
’ Supporting data have been tiled at ASTM Headquarters.
1916 RaceSt., Philadelphia, PA 19103. Request RR:DI 1-1029.
279

~~
D2240
Type A method. Table 2 gives the precision
results for Type D method.
11.5 Repeatability refers to within laboratory
precision; reproducibility refers to among (between)
laboratory precision.
1 I .6 Bias-In test method statistical termi-
nology, bias is the difference between an average
test value and the reference or true test property
value. Reference values do not exist for this test
method since the value or level of the test property
is exclusively defined by the test method.
Bias, therefore, can not be determined.
Material
Mean
Level
TABLE 1 LQC Hardness Precision Data-Type A
Within Laboratories
Among Laboratories
S cv S cv
I 51.4 0.646 0.0 I3 I .56 0.030
2 65.3 0.878 0.014 2.14 0.333
3 68.0 0.433 0.0064 2.28 0.034
Average or Pooled Values 0.677 0.01 I8 2.018 0.0323
Repeatability
Reproducibility
Standard Deviation, (S)" 0.677 2.045
CoeFficient of Variation. (CV) 0.01 18 0.0325
Least Significant Difference, (LSD)' 3.29 % 9.20 %
A An average value. the value of S varies with mean level.
'LSD based on 95 % confidence level; two results are considered significantly different if their difference, expressed as a
percentage of their average, exceeds the stated percent value.
Material
I
2
3
TABLE 2 LQC Hardness Precision Data-Type D"
Mean Within Laboratories Among Laboratories
Level s cv S cv
42.6 0.316 0.0080 2.8 I5 0.066 I
54.5 0.79 I 0.0 I50 3.536 0.0649
82.3 1.012 0.0 I30 3.544 0.043 1
~~~~~~ ~
Average or Pooled Values 0.762 0.0 I22 3.316 0.0590
Repeatability
Reproducibility
Standard Deviation, (S)' 0.762 3.359
CoeFficient of Variation. (CV) 0.0122 0.0596
Least Significant Difference, (LSD)' 3.45 % 16.85 %
A One laboratory did not report data. The results are based on five laboratories.
'An average value, the value of S varies with mean level.
'LSD based on 95 % confidence level: two results are considered significantly different if their difference. expressed as a
percentage of their average, exceeds the stated percent level.
280

D2240
Q 35.2 5
-OramiW
I*
0.79 ZOO3 mm
FIG. 1 Indentor for Type A Durometer
2. 5010.04~0m
,o
FIG. 2 Indentor for Type D Durometer
Rod. 0.100~~012 mm
The .4merican Sotietyji)r Testing and Materials takes no position respecting the validity ofany patent rights asserted in iwmection
with uny item mentioned in this standard. Users (?/‘this standard are expressly advised that determination of the validity of any such
puieni rights. and the risk of infringement of such rights. are entirely their own responsibility.
This standard is suhject to revision at any time by the responsible technical committee and must be reviewed every,five .wars and
If not revised. either reapproved or withdrawn. Your comments are invited either for revision of this standard or ,for additional
.standurd.v und should be uddressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting (f the
re.sponsihle technical 1-ommittee. which ~vou may attend. If you .bel that your comments have not received a ,fair heuring you should
muke your views know to the ASTM Committee on Standards. 1916 Race St.. Philadelphia, Pa. 19103.
28 1

em
Designation: D 2293 - 69 (Reapproved 1980)"
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Raw St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appmr in the next edition.
Standard Test Method for
CREEP PROPERTIES OF ADHESIVES IN SHEAR BY
COMPRESSION LOADING (METAL-TO-METAL)'
This standard is issued under the fixed designation D 2293; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parenthesa indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change Since the last revision or rcapproval.
'' Note in Section 2 was added editoriallv and subuent sections renumbmd in Ami1 1985.
1. scope
I. 1 This test method covers the determination
of the creep properties of adhesives for bonding
metals when tested on a standard specimen and
subjected to certain conditions of temperature
and compressive stress in a spring-loaded testing
apparatus.
2. Applicable Document
2.1 ASTM Standard:
D 1002 Test Method for Strength Properties
of Adhesives in Shear by Tension Loading
(Metal-to-Metal?
3. Apparatus
3.1 Compression Creep Test Apparatus, as
shown in Figs. 1 and 2.
3.2 Microscope, calibrated, with Filar microeyepiece
and l OX objective lens.
4. Test Specimens
4.1 Test specimens shall conform to the form
and dimensions shown in Fig. 3. These specimens
are similar to the tension lap shear specimens
described in Test Method D 1002, except
that the length of either side of the shear area
shall be 6.35 mm (Vi in.) rather than 88.9 mm
(3% in.) minimum.
4.2 A complete description of these specimens
and the method of preparation is given in Sections
3,4, and 5 of Test Method D 1002.
4.3 Each test specimen shall have the edges of
the bond area polished and scribed with three
fine lines across the glueline for creep measurement.
5. Procedure
5.1 To conduct a creep test, center the specimen
within the slot between the washer and
bushing of the apparatus as shown in Fig. 1.
Compress the spring between the two bushings
to the desired load by tightening the nut. The
correct load can be applied by deflecting the
spring a given measured amount as determined
from a calibration curve.
5.2 To measure total deflection, observe the
average displacement of fine razor scratches
across the centers of both sides of the lap joints
with a calibrated microscope having a Filar microeyepiece
and a lox objective lens.
5.3 If the spring load is allowed to continue
to compress the specimen, the observed initial
deflection will be followed by a continued increasing
deflection with time. To provide a complete
history of creep behavior, measure these
deflections periodically with the calibrated microscope
for as long as the test is allowed to
continue or until the adhesive joint fails.
5.4 If a creep curve at other than room temperature
is required, perform both the specimen
loading and its subsequent exposure while holding
the specimen to the desired temperature. A
suitable oven or cold box may be used for this
purpose. Under these conditions, the actual creep
measurements are more difficult to obtain. This
' This test method is under the jurisdiction of ASTM Committee
D-14 on Adhesives and is the direct responsibility of
Suhmitteee D14.80 on Metal Bonding Adhesives.
Current edition approved May 9, 1969. Pulbished July 1969.
Originally published as D2293 - 64 T. Last previous edition
D 2293 - 64 T.
Annual Book ofASTM Standards, Vol 15.06.
282

can be done, however, in one of two ways. The
microscopic measurements can be made quickly
and the specimen and its apparatus returned to
its temperature box before its test temperature
has changed appreciably. Or, periodically, additional
fine scribe lines can be added adjacent to
the original scratches across the centers of both
sides of the lap joints and all of the displacements
measured and calculated in terms of differences
from the original scratches at the conclusion of
the test. If final scratches are made just before
the specimen is removed from the temperature
box, the displacement measurements can be
made at room temperature and with the specimen
unloaded if desired. Furthermore, relaxation
of the specimen after unloading can also be
measured if the displacement readings are continued.
5.5 If buckling of the specimen occurs due to
compressive creep of the metal, discount the test
and redesign the specimen.
5.6 Record the total observed average deflection,
the magnitude and duration of the compressive
stress, and the test temperature for each
specimen.
6. Report
6.1 The report shall include the following
6.1.1 Complete description of materials and
procedures used and dimensions of the specimen,
6.1.2 Creep of specimen defined as the quotient
of the total measured deflection and the
bondline thickness, expressed in &metres per
,millimetre(or inches per inch),
6.1.3 Magnitude and duration of the compressive
stress and the test temperature, and
6.1.4 Nature of the failure if it occurs before
the creep test is completed.
283

@ D2293
1
3
3.97 mm
(5132")
7
63.5 mm
( 2 -I /2")
1
6.35
f
1905 mm(3/4") I ' I
L'
-12.7 mm (1/2")
20 NF Threod
50.8 mm (2")long
I
A-slotted bdt
&Bushing
C-Sprhg-piano wire cylindrical helical compression
spring with six active coils, eight total coils, wound closed,
ground quam, and cadmium plated
D-Washer-22.25 mm ('h in.) OD, 12.7 mm (% in.) ID,
1.6 mm (%6 in.) thick
E-Nut-12.7 mm ('h in.)-20 NF
F-T- specimen
Bolt 12.7 mm (1/2")
20NFx130 mm
(5-3/32") long
@
FIG. 2 Compression Creep Test Appmtm, Deenils
FIG. 1 Compression Creep Test Apparatus, Assembly
284

1.6 mm (0.064")
1
Bondline
TMochine oll edges
flat and square
t
25.4 mm
6.35 mm 6.35"
( I /4" 1 ( 1/4"
FIG. 3 Form and Dimeasions of Test Specimen
The American Scxiety for Testing and Materials takes no position respecting the validity o$any patent rights asserted in conrrortion
with any item mentioned in this standard. Users o$this standard are expressly advised that determination of the validity o$any such
went rights, and the risk of infingement of such rights, are entirely their own responsibility.
This standard is subject to revision a! any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision os this standard or for additid
statduds and should be addressed to ASTM Headquarters. Your comments will receive carefil consideration at a meeting ofthe
respnsible technical committee, which you may attend. I$ you feel that your comments have not received a jhir hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.
285

Lbsignatim 0 2294 - 69 (Reapproved 198Or'
AMERICAN SOClETV FOR TESTING AND MATERIALS
1916 Raw St., Phikblphb, Pa. 1910d
R~primd from the Annual Book of ASTM Standads, Wright ASrM
in the current canbind index. will appmr in the mt edition.
If not I ii
Standard Test Method for
CREEP PROPERTIES OF ADHESIVES IN SHEAR BY
TENSION LOADING (METAL-TO-METAL)'
This standard is issued under the fixed desigaation D 2294, the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last mvision or reapproval.
" No~ESeCtion 2 WBS added editohlly and suhpequent SC&XIS renumbered h A@ 1985.
1. scope
1. I This test method covers the determination
of the creep properties of adhesives for bonding
metals when tested on a standard specimen and
subjected to certain conditions of temperature
and tensile stress in a spring-loaded testing ap
paratus.
1.2 This test method is applicable to the temperature
range from -55 to +26OoC (-67 to
+5WF).
2. Applicable Documents
2. I ASTM Standards..
D638 Test Method for Tensile Properties of
Plastics2
D 1002 Test Method for Strength Properties of
Adhesives in Shear By Tension Loading
(Metal-t~-Metal)~
3. Apparatus
3.1 Tension Creep Test Apparatus, as shown
in Fig. It shall consist of a hollow loading
chamber, a solid extension rod with provisions
for attachment of test specimens, and a hightemperature
resistant spring.' A testing machine
conforming to the requirements of Test Method
D 638 shall be used as a loading mechanism.
3.2 Microscope, calibrated, having loOX magnification.
4. Test Specimens
4.1 Test specimens shall conform to the shape
and dimensions shown in Fig. 2. These specimens
are similar to the tension lap shear speci-
mens described in Test Method D 1002, except
for the holes as shown in Fig. 2:
4.2 At least three specimens shall be tested for
each set of standard conditions of load, time, and
temperature.
4.3 A complete description of these specimens
and the method of preparation is given in Sections
3,4, and 5 of Test Method D 1002.
4.4 Each test specimen shall have the 12.7-
mm (%in.) edges of the bond area polished and
scribed with three fine lines across the glueline
(Fig. 1) for creep measurement.
5. Procedure
5.1 Attach the test apparatus to a testing machine
and condition to a prescribed test temperature.
Place a specimen within the load chamber
of the test apparatus (Fig. 2), and attach to the
chamber and load shaft by means of pins.
5.2 Apply the load by the test machine at a
rate 80 to 100 kgf/cm2/min (1200 to 1400 psi/
min). After reaching the desired load turn up the
knurled supporting ring to make contact with
! This test method, is under the jurisdiction of ASTM Committee
D-14 on Adhesives and is the direct responsibility of
Subcommittee D14.80 on Metal Bonding Adhesives.
Current edition approved May 9, 1969. Published July 1969.
Onginally published as D2294 - 64T. Last previous edition
D 2294 - 64T.
' Annual Book of ASTM Standards, Vol08.0 1.
'Annual Book of ASTM Standards, Vol 15.06.
' Detailed working drawings for the construction of the tensile
creep test apparatus are available at a nominal cost from the
ASTM, 1916 Race St., Philadelphia, PA 19103. Request Adjunct
No. 12-422940-00.
' Springs suitable for this apparatus may be obtained from
the \N. D. Gibson Co., Chicago, IL.
286

the disk (that is, touch plus Y4 turn) supporting
the compressed Spring. Unload the testing machine,
remove the entire creep test apparatus
(except the loading yoke) from the testing machine,
and place it in the desired environment.
5.3 To measure total deflection, observe the
displacement of fine razor marks across both
sides of the bond area with a calibrated microscope
having lOOx magnification.
5.4 To measure deflection at various times
during the test, especially when the environment
is other than room temperature, fine scribe lines
may be added periodically adjacent to the original
mark across the edge of the joint. Make a
final mark just before the specimen is removed
from the temperature-conditioned area and the
load removed. The relative displacement measurements,
which may then be made at any time
thereafter, will indicate the amount of creep deflection
at the various time intervals. Suggested
time intervals are 1, 3, 5, 10, 30, 50, 100, 300,
500, 1O00, etc., min, as these yield approximately
equally spaced points when plotted on a log scale.
If desired, readings of the changes in displacement
can be continued even after the specimen
is unloaded. These provide a measure of the
relaxation.
5.5 Record the deflection at periodic intervals
during the test, the total deflection, the magnitude
and duration of the tensile stress, and the
test temperature for each specimen. Express all
loads in kilograms per square centimetre (or
pounds per square inch) and, if possible, report
to three significant figures.
6. Report
6.1 The report shall include the following:
6.1.1 Complete identification of the materials
and procedures used and dimensions of the bond
area including width and length k2.54 mm (0.0 1
in.) and bondline thickness kO.0 127 mm (0.0005
in.),
6.1.2 Creep deflection of the specimens shown
as total measured deflection,
6.1.3 Magnitude and duration of the tensile
stress, test temperature, and any environmental
conditions,
6.1.4 Conditioning procedure used for specimens
prior to testing,
6.1.5 Number of specimens tested, and
6.1.6 Nature of the failure (that is, percent
adhesive or cohesive) if it occurs before the creep
test is completed.
287

LT
FIG. 1 Tc~~sion Creep Test Apparalvs
288

The American Sbciety for Testingand Materials takes no position respecting the validity ofany patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
went rights. and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyfive years and
$not revised. either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additiona2
standards and sholrld be addressed to ASTM Headquarters. Your comments will receive car& consideration at a meeting of the
responsible technical committee, which you may attend. rf you fwl that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Stanhrds. 1916 Race St.. Philadelphia, PA 19103.
289

4slb
Designation:
D 2556 - 69 386
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa., 19103
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
AMERICAN NATIONAL STANDARD 2201.1-1970
AMERICAN NATIONAL STANDARDS INSTITUTE
Standard Method of Test for
APPARENT VISCOSITY OF ADHESIVES
HAVING SHEAR-RATE-DEPENDENT
FLOW PRO PE RTI ES
This Standard is issued under the fixed designation D '556: the number immediately following the designation indicates
the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the
year of last reapproval.
1. scope
1 .I This method covers the measurement of
the apparent viscosity of shear-rate-dependent
adhesives.
5.2 The principle of measurement is based
upon a reversible isothermal change in apparent
viscosity with change in rate of shear.
1.3 Measurement is performed with a spindle,
disk, T-bar, or coaxial cylinder rotational
viscometer under standardized conditions with
rigid control of the time intervals of measurement.
Readings are obtained on the viscometer
dial scale at the end of 1 min for each rotational
speed. Changes from the lowest speed
to the highest speed, and return to the lowest
speed, are made without stopping the instruffient.
2. Apparatus
2 I Viscometer-The apparatus shall consist
of a spindle,2 disk,2 T-bar,2 or coaxial-type"
viscometer with appropriate spindles, disks,
T-bars, or cylinders. A scored, warped, or
~ther~ise damaged spid!t, disk, T-bai, oi
cylinder shall not be used. Except when using
the coaxial cylinder-type viscometer, the size
of container to be used wall be determined by
mutual agreement. Some instruments have
two concentric scales, and care should be
taken to read the pointer on the correct scale.
2.2 Supporting Stand'-The support for
the viscometer shall consist of a suitable stand
with a supporting arm which shall be capable
of being lowered or raised either manually or
mechanically.
2.3 Thermometer-A precision thermome-
290
ter, with graduations not greater than 0.2 C
(0.5 F), shall be used for temperature measurements.
3. Conditioning
3.1 Condition the adhesive sample and instrument
at 23 f 0.5 C (73.4 f 1.0 F) (or
other temperature agreed upon by the adhesive
vendor and purchaser) at least 16 h. If
special conditioning methods are necessary,
such as the use of a circulating water bath,
they shall be noted in the report, see 4.1.4.
4. Procedure
4.1 Select a viscometer and spindle (see
Table AI), disk, T-bar, or cylinder suited to
the viscosity range of the material such that
the model-speed-rotational element combination
will give dial readings between 20 and 80
percent of the full-scale reading. Firmly fit the
rotational element into the shaft extension
which goes down through the center of the
dial casing. Place the viscometer on the supporting
stand so that the rotational element is
vertical. Slowly immerse the rotational ele-
' This method is under the jurisdiction of ASTM Committee
D-14 on Adhesives. A list of members may be found
in the ASTM Yearbook.
Current edition effective May 9. 1969. Originally issued
1966. Replaces D 2556 66 T.
- The Brookfield Synchro-Lectric Viscometers. Models
LV, RV, or HV have been found satisfactory for this purpose
and are available from the Brookfield Engineering
Laboratories, Stoughton, Mass.
' The Ferranti Portable Viscometers, Models VL, VM,
or VH have been found satisfactory for this test and are
available from Ferranti Electric Inc.. Plainview. Long Is-
Ian!. N. Y.
The Brookfield Helipath Stand or other commercially
available stands may be used.

D 2556
ment in the sample to the depth recommended
by the manufacturer of the apparatus or,
where this is not clearly indicated, to a depth
agreed upon by the adhesive vendor and purchaser.
Take care as the rotational element is
lowered into the solution to ensure that no air
is trapped under or around it. See Appendix
A 1 for example or spindle selection.
4.2 With the rotational element immersed
n the adhesive, start the motor of the viscometer
at the lowest rotational speed. Maintain
this speed for exactly 1 min. Without stopping
the motor, increase the speed to the next indicated
measure of rotation, etc., at I-min (*2
s) intervals, until the maximum readable rotation
has been achieved. At the end of 1 min at
thih speed, decrease the revolutions per minute
in I-min intervals until the lowest speed
ha5 been reached. Record dial readings at the
end of each minute.
4.3 A plot of rotational speed versus apparent
viscosity as determined from the dial
readings provides evidence as to shear-rate
dependency of the material. A value of apparent
viscosity may be obtained from any point
on the curve.
5. Report
5.1 The report shall include the following:
5.1.1 Date of test and complete identifica-
tion of the adhesive tested, including type,
source, manufacturer’s code numbers,, form,
date of manufacture,
5.1.2 Name and model number of the instrument
used,
5.1.3 Number and type of rotational element
used,
5.1.4 Conditioning procedure employed in
preparation of the adhesive for testing, including
dimensions of the test container,
5.1.5 Time elapsed between various operations
in preparation of the adhesive mix and
between rotational element immersion and
start of test,
5.1.6 Temperature of the sample during
test,
5.1.7 Depth of immersion of rotating element
(if depth not standard), and
5.1.8 Apparent viscosity in poises or equivalent
units associated with the particular
equipment at one or more selected rotational
speeds and whether obtained while increasing
or decreasing the rotational speeds.
NOTE-The shear-rate-dependent characteristics
of a sample under test may be defined by a so-called
“thixotropic index,” which is the ratio of apparent
viscosities at two different speeds. For example:
apparent viscosity at speed 2
~
apparent viscosity at speed 20
= 80,000 ~P/20.000 CP = 4
REFERENCES
Eirich. F. K., Rheolog.i,, Academic Press, I1 1 5th
Ave., New York, N. Y., 1960.
Green, Henry, Industrial Rheo1og.r and Rheological
Structures, John Wiley and Sons, New York,
N. Y., 1949.
29 1

APPENDIX
Al. EXAMPLE OF TABLE FOR VISCOMETER AND SPINDLE SELECTION
TABLE A1
Recommended Spindles for Brookfield RVF Viecometer
Range, cP" Spindle Speed, rpm Factor'
100 to 400
400 to 800
800 to 1 600
1600to3 200
3 2OOto4OOO
4OOOto8000
8 OOO to 16 OOO
16 OOO to 20 000
20 OOO to 40 OOO
40 OOO to 80 GOO
80 000 to 160 OOO
160 000 to 200 OOO
200 000 to 400 OOO
400 000 to 800 OOO
800 OOO to 2 000 OOO
1
1
2
2
3
4
4
3
4
4
5
6
6
7
7
20
IO
20
10
20
20
IO
4
4
2
2
4
2
4
2
5
10
20
40
50
100
200
250
500
1000
2000
2500
5000
IO 000
20 000
a If the scale reading is below 20 or above 80, move to the spindle and speed recommended for the next lower
or higher viscosity-range
* To obtain the viscosity in centipoises, multiply the reading on the "100' scale by the factor for the given
spindle and speed
292

(ISTE,
Designation: D 2849 - 69 (Reapproved 1980)''
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition
Standard Methods of Testing
URETHANE FOAM POLYOL RAW MATERIALS'
An American National Standard
This standard is issued under the fixed designation D 2849; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (c) indicates an editorial change since the last revision or reapproval.
'' NoTE-Mion 2 was added editorially and subsequent sections renumbered in August 1985.
1. scope
1.1 These methods cover the testing of poly01
raw materials used in preparing urethane foams,
including both polyesters and polyethers containing
carboxyl, primary or secondary hydroxyl
groups, or both.
NOTE 1-Urethane foams are cellular products that
vary from soft resilient types to those which are hard
and rigid. These foams are made by the interaction of
polyhydroxy compounds, water, and an organic polyisocyanate.
The reactions involved in the manufacture
of these foams can be modified in many ways. Basic
materials, especially tertiary amines, act as catalysts and
accelerate the reaction, whereas acidic materials retard
it. The uniformity and size of the cells are affected by
the addition of surface-active agents. Usually nonionic
or cationic surfactants are employed. Fillers, plasticizers,
and colors are also added in many cases to give
specific properties to the foam.
1.2 The procedures appear in the following
order:
Sections
Sampling ........................... 4
Sodium and Potassium ................ 6 to 20
Acid and Alkalinity Numbers ...........21 to 30
Hydroxyl Number ....................31 to 52
Unsaturation ....................... .53 to 60
Water ............................. .61 to 70
Suspended Matter ....................71 to 73
Specific Gravity . . . . . . . . . . 74 io 79
Viscosity . . . . . . . . . . . . . . . 80 to 91
Color .......................... 92 to 103
1.3 The values stated in SI units are to be
regarded as the standard.
2. Applicable Documents
2. I ASTM S "k:
D 6 18 Method for Conditioning Plastics and
Electrical lnsulating Materials for Testing'
D I 193 Specification for Reagent Water3
D 1209 Test Method for Color of Clear Liquids
(Platinum-Cobalt Scale)4
E 1 Specification for ASTM Thermometers'
E 200 Methods for Preparation, Standardization,
and Storage of Standard Solutions for
Chemical Analysis6
E 203 Test Method for Water Using the Karl
Fischer Reagent6
E 308 Method for Computing the Colors of
Objects by Using the CIE System'
3. Purity of Reagents
3.1 Purity of Reagents-Reagent grade chemicals
shall be used in all tests. Unless otherwise
indicated, it is intended that all reagents shall
conform to the specifications of the Committee
on Analytical Reagents of the Amencan Chemical
Society, where such specifications are available.*
Other grades may be used, provided it is
first ascertained that the reagent is of sufficiently
high punty to permit its use without lessening
the accuracy of the determination.
3.2 Purity of Water-Unless otherwise indi-
I These methods are under the jurisdiction of ASTM Committee
D-20 on Plastics and are the direct responsibility of
Subcommittee D20.22 on Cellular Plastics.
Current edition approied Dec. I Q. 1964 Puhli\IiL,.: I :vtiJr\
1970.
* .-II1/711U/ Book o/ .I.W\f .StU//t/Ud\. 1'01 ox 01
'. lrlrllru/ Book o/ .1S%\f.s/u//durt/\.
1'L)l I I (1 I
.lr1r7//~/ Book o/ .I.ST.\I S/ur/durd\. 1

D 2849
cated, references to water shall be understood to
mean water conforming to Specification D 1 193.
4. Sampling
4. I Polyesters and polyethers usually contain
molecules covering an appreciable range of molecular
weights. These have a tendency to fractionate
during solidification. Unless the material
is a finely-ground solid it is necessary to melt
(using no higher temperature than necessary) and
mix the resin well before removing a sample for
analysis. Many polyols are hygroscopic and care
should be taken to provide minimum exposure
to atmospheric moisture during the sampling.
5. Conditioning
5.1 Conditioning-Condition the test specimens
at 23 f 2°C (73.4 f 3.6"F) and 50 f 5 %
relative humidity for not less than 40 h prior to
test in accordance with Procedure A of Method
D 618 for those tests where conditioning is required.
In cases of disagreement, the tolerances
shall be f 1 "C (f 1.8"F) and +2 % relative humidity.
5.2 Test Conditions-Conduct tests in the
Standard Laboratory Atmosphere of 23 f 2°C
(73.4 f 3.6"F) and 50 & 5 % relative humidity,
unless otherwise specified in the test methods or
in this specification. In cases of disagreement, the
tolerances shall be floc (fl.8"F) and f2 % relative
humidity.
SODIUM AND POTASSIUM
6. Scope and Application
6.1 This method covers the determination of
sodium and potassium in all types of polyols
containing from 0 to 10 ppm of sodium or potassium,
or both. Polyols having larger sodium
or potassium concentrations can be analyzed by
employiiig ~iie of the fg:l~~iiig mobifications:
6.1.1 Decreasing the sample size,
6.1.2 Diluting the ash solution, and
6.1.3 Extending the calibration curve to
higher concentration.
7. Summary of Method
7.1 This method is based on a flame photometric
analysis of the ash derived from the sample.
8. Apparatus
8. I Flame Photometer.'
8.2 Metal Sheet, 1.6 by 152 by 152 mm (l/16
by 6 by 6 in.), or asbestos slate of similar dimensions,
with a hole 38 mm ( 1.5 in.) in diameter in
the center.
8.3 Polyethylene Bottles, 470-cm3 (I-pt) capacity.
8.4 Sample Holders, for vaporizing solution
into the flame.
8.5 Funnel, 50-mm, having short stem and
drawn to a point.
9. Reagents
9.1 Potassium Carbonate, Potassium Chloride,
or Potassium Acetate, Stock Solution
(0.1000 g K/ 1000 mL, IO0 ppm K)-Prepare an
aqueous solution of potassium carbonate
(K2C03), potassium chloride (KCl), or potassium
acetate (KC2H302) containing 0.1000 g of potassium/lOOO
mL (100 ppm potassium). Store in a
polyethylene bottle. Prepare standard aqueous
solutions containing 1,2, 3, and 5 ppm of potassium
from the above 100 ppm stock solution and
store in a polyethylene bottle.
9.2 Sodium Carbonate, Sodium Chloride, or
Sodium Acetate, Stock Solution (0.1000 g Na/
1000 mL, 100 ppm Na)-Prepare an aqueous
solution of sodium carbonate (Na2C03), sodium
chloride (NaCl), or sodium acetate (NaC2H302)
containing 0.1000 g of sodium/l000 mL (100
ppm sodium). Store in a polyethylene bottle.
Prepare standard aqueous solutions containing
1, 2, 3, and 5 ppm of sodium from the 100 ppm
stock solution and store in a polyethylene bottle.
9.3 Water, freshly distilled, stored in a polyethylene
bottle.
10. Special Precautions
10.1 An extra effort must be made to avoid
contamination during the entire procedure. 'The
environment should be free of dust and cigarette
smoke. Boiling of exposed salt solutions of calcium,
sodium, and potassium near the sample
can significantly affect the result. Fingers should
never contact solutions and the inside of containers.
All containers should be rinsed before
use with freshly distilled water which is stored in
The Beckman DU with flame photometer accessory, or the
equivalent, has been found satisfactory for this purpose.
294

D 2849
a closed chemical-resistant glass or polyethylene
bottle. Water contained in a polyethylene
squeeze type wash bottle should be changed frequently
since the air returning to the bottle after
use can readily introduce sodium or potassium
from the atmosphere. Filter paper must not be
used in the analysis since it could either absorb
or contribute sodium ion. The sample ash solution
should be read in the flame photometer the
same day it is prepared. Glass stoppers should be
inserted in the volumetric flasks without twisting
action. The platinum dishes should be perfectly
clean, have a shiny and smooth inner surface,
and should be reserved for this analysis.
11. Sample Ashing
11.1 Weigh 20 f 0.1 g of the sample into a
platinum dish. Place the dish with its contents in
the center of a metal or asbestos sheet that is
supported by a ring stand and located above a
bunsen or Meker burner. Light the burner and
carefully heat the sample below its ignition point
so that nonspattering steams of bubbles rise from
the sample (Note 2). After the sample has been
reduced to a tarry or coke-like residue (approximately
40 min), ignite it by passing the flame
over the dish. Turn the burner off and allow the
residue to burn out. Transfer the dish to a mume
furnace at 525 to 550°C (above 550°C a loss of
sodium or potassium could occur) and complete
the ashing to a carbon-free residue (Note 3).
Remove the dish from the furnace and allow to
cool to room temperature in a desiccator.
NOTE 2-If the sample has a low volatility, the
burner flame should touch the platinum dish directly;
or, alternatively, the sample may be ignited and allowed
to bum with a small flame that contains a minimum
number of white-hot streamers.
NOTE 3-The carbonaceous residue of some products
may resist oxidation in the muffle furnace. If the
carbon particles have not disappeared after 60 min, the
cooled residue may be treated with a few drops of
concentrated sulfunc acid. The acidified residue shaii
then be heated slowly and carefully with a burner to an
absence of white fumes and then returned to the mume
furnace. One acid treatment will usually decompose
the carbon particles in the ash. If acid treatment is
necessary, a blank determination shall be made, using
the same amount of the same lot of acid.
1 1.2 Dissolve and ash in about four successive
10-mL portions of warm water and quantitatively
transfer each portion through a funnel to
a 50-mL flask that has been freshly rinsed with
water. Rinse the funnel with water and add each
rinse to the volumetric flask until the liquid is at
the 50-mL mark. Mist the contents of the flask
and analyze with the flame photometer as directed.
12. Flame Photometer Adjustment''
12.1 Turn on the oxygen and acetylene supplies.
Set the tank reducing and panel valves in
accordance with the instrument manufacturer's
instructions (Note 4). Light the burner. Adjust
the spectrophotometer to the following settings:
NOTE 4-The slit width and optimum oxygen and
acetylene pressure settings vary with the burner. When
a new burner is installed, the settings must be reestablished
according to the instructions of the instrument
manual.
Wavelength set at maximum deflection near
766 nm for potassium or 589
nm for sodium
0.1
3 (IO 000 MQ)
Selector switch
Phototube load resistor
Filter slide
Phototube housing
knob
Shutter
Sensitivity and slit
in.
in.
open
adjust for optimum sensitivity
and maximum response
SODIUM
13. Calibration
13.1 Rinse and fill a sample holder with
freshly distilled water. (Note 5). Cover the holder
with a 150-mL beaker. This is for use to establish
background correction.
NOTE 5-For increased accuracy the same lot of
water should be used for background correction, solution
of sample, and the standards. Experimental results,
however, indicate that mixed lots do not significantly
increase the error of the procedure. A check on the
calibration curve with a new lot of water used to correct
for background should verify the suitability of the water,
provided no instrument changes have taken place.
!3.2 Rinse 2nd f! tWO samp!e hn!den with
the sodium solution (5 ppm Na). Cover each
holder with a 150-mL beaker to minimize evaporation
and possible dust contamination.
13.3 Aspirate rinsing water in the flame for
about 15 s and replace with the water used for
background correction. Set the transmittance
scale to 0 76. Rotate the dark current knob until
"The adjustments described in Section 12 apply to the
Beckman DU flame photometer. Comparable adjustments must
be made if another type of instrument is used.
295

the galvanometer needle is constant at zero.
About 15 s are required before the radiant power
becomes steady.
13.4 Replace the aspirating background water
with sodium solution (5 ppm Na). Set the transmittance
scale to 100 % and turn the slit knob
until the galvanometer needle is at zero. Do not
change this slit width during a run of determinations.
13.5 Remove the sodium solution from the
burner. Aspirate cleaning water for at least 15 s
and remove,
13.6 Remove the water from the burner and
introduce one of the two holders containing sodium
solution. Set the transmittance dial to
100 % T and rotate the sensitivity knob until the
galvanometer reads zero. Do not change this
sensitivity setting during a run of determinations.
13.7 Replace the holder at the burner with the
other holder containing sodium solution. Rotate
the transmittance knob until the galvanometer
again reads zero. The average of two readings
should be 100 f 0.5 % on the transmittance
scale. If the deviation is more than 0.5 (probably
due to contamination) repeat 13.5 through 13.7
with fresh portions of sodium solution (5 ppm
Na) until the desired reading is obtained.
13.8 Remove the standard solution from the
burner and aspirate cleaning water.
13.9 Establish transmittance readings between
0 and 100% by aspirating the sodium
solutions containing 1, 2, and 3 ppm sodium.
13.10 Prepare a calibration curve by plotting
transmittance reading versus parts per million of
sodium on linear graph paper.
14. Procedure
14.1 Rinse the burner with water and introduce
a cell containing sample ash solution. Record
the reading on the transmittance scale. If the
meter indicates that the reading is more than
100 %, dilute an appropriate aliquot of the solution
with water until a reading can be made at
approximately 50 ?6 transmittance.
14.2 Remove the solution from the burner
and aspirate a second portion of the sample
solution. Take readings as before. The average
should not differ more than f 1 % absolute from
that given in 14.1. If the difference is greater,
repeat 14.1 and 14.2 with fresh portions of sample
ash solution until a satisfactory check is obtained.
14.3 Remove the sample from the burner and
aspirate water. If more samples are to be analyzed,
repeat 14. l and 14.2. If there are any delays
between tests, close the shutter until work is
resumed. If there are any prolonged delays between
sample determinations on a given day,
check one point on the calibration curve to ensure
that no change has occurred in the instrument.
14.4 When a run is completed, thoroughly
rinse the burner by aspirating with water. Wait
about 30 s and then turn off the acetylene valves
.first. After the flame is extinguished, turn off the
oxygen valves and the switches on the instrument.
15. Calculation
15.1 Convert the transmittance scale reading
to parts per million of sodium by comparison
with the sodium calibration curve. Calculate the
parts per million of sodium in the sample as
follows:
Sodium, ppm = A X 2.5 x F
where:
A = parts per million of sodium from the calibration
curve,
2.5 = dilution factor for method as written, and
F = dilution factor if further sample dilution
is necessary.
16. Precision
16.1 The following data should be used for
judging the acceptability of results (95 ?6 confidence
limits). I I
1 5.1.1 Repeatability-Duplicate results by
the same operator should not be considered suspect
unless they differ by more than 0.5 ppm of
sodium.
16.1.2 Reproducibility-The average result
reported by one laboratry should not be considered
suspect unless it differs from that of another
laboratory by more than 2.0 ppm of sodium.
POTASSIUM
17. Calibration
17.1 Prepare a calibration curve for potassium
in accordance with the procedure described for
sodium in Section 13, using the proper wave-
" These precision data are approximations based on limited
data, but they provide a reasonable basis for judging the significance
of the results.
296

D 2849
length setting (Section 12) and the potassium
standards instead of the sodium standards.
18. Analysis
18.1 Analyze the sample ash solution in accordance
with Section 14 using the proper wavelength
setting (Section 12).
19. Calculation
19. I Convert the transmittance scale reading
to parts per million of potassium by comparison
with the potassium calibration curve. Calculate
the parts per million of potassium in the sample
as follows:
Potassium, ppm = A x 2.5 x F
where:
A = parts per million of potassium from the
calibration curve,
2.5 = dilution factor for method as written, and
F = dilution factor if further sample dilution
is necessary.
20. Precision
20.1 The following data should be used for
judging the acceptability of results (95 % confidence
limits). I I
20.1.1 Repeatability-Duplicate results by
the same operator should not be considered suspect
unless they differ by more than 0.5 ppm of
potassium.
20. I .2 Reproducibility-The average result
reported by one laboratory should not be considered
suspect unless it differs from that of another
laboratory by more than 2.0 ppm of potassium.
ACID AND ALKALINITY NUMBERS
21. Scope and Application
2 I. 1 This method is intended for determination
of acidic or basic constituents in resins and
other materials soluble in mixtures of benzene
and denatured ethyl alcohol. This method is not
applicable to pol yethers.
2 1.2 This method is useful as an indication of
the extent of a reaction involving acids. The
results are a measure of batch-to-batch uniformity
and are used as correction factors in calculating
true hydroxyl number.
22. Definitions
22.1 acid number-the quantity of base, expressed
in milligrams of potassium hydroxide,
that is required to titrate acidic constituents present
in 1 g of sample.
22.2 alkalinity number-the quantity of base,
expressed as milligrams of potassium hydroxide,
present in 1 g of sample.
23. Summary of Method
23.1 The sample is dissolved in a mixture of
benzene and denatured ethyl alcohol, and the
resulting single-phase solution is titrated at room
temperature with alcoholic potassium hydroxide
solution, to the end point indicated by the color
change of the added phenolphthalein. Alkalinity
numbers are determined by back-titration after
adding excess hydrochloric acid.
24. Reagents
24. I Ethyl Alcohol, Denatured-Ethyl alcohol
conforming to either Formula No. 2B or 3A of
the U. S. Bureau of Internal Revenue.
24.2 Hydrochloric Acid (0.1 N)-Prepare a
0.1 N solution of hydrochloric acid (HC1). Standardization
is unnecessary.
24.3 Phenolphthalein Indicator Solution-
Dissolve 0.5 g of phenolphthalein in 100 mL of
a mixture of equal volumes of water and denatured
ethyl alcohol. Add a slight excess of 0.1 N
NaOH solution (pink color) and then just neutralize
(colorless) with 0.1 N HCl.
24.4 Potassium Hydroxide, Standard Alcoholic
Solution (0.1 N)-Dissolve 5.6 I g of potassium
hydroxide (KOH) in 10 mL of carbon
dioxide-free water and dilute to I L with denatured
ethyl alcohol. Store the solution in a chemical-resistant
dispensing bottle out of contact with
cork, rubber, or saponifiable stopcock lubricant
and protected by a guard tube containing sodalime
or soda-asbestos (Ascarite). Standardize frequently
enough to detect changes of 0.0005 N,
preferably against pure potassium acid phthalate
(KHC8H404, 0 8 to 0.9 g) in about 100 mL of
carbon dioxide-free water, using phenolphthalein
to detect the end point.
24.5 Sodium Hydroxide, Standard Solution
(0.1 N)-Prepare and standardize a 0.1 N solution
of sodium hydroxide (NaOH).
24.6 Titration Solvent-Mix equal volumes of
benzene and denatured ethyl alcohol.
ACID NUMBER
25. Procedure
25.1 Into a 250-mL Erlenmeyer flask, intro-
297

D 2849
duce a weighed quantity of the sample (Note 6).
Add 50 mL of the titration solvent and 0.5 mL
of the indicator solution. and swirl until the
sample is entirely dissolved by the solvent (heat
only if necessary, and do not boil).
NOTE 6-For samples with an acid number of less
than 7.0. use 6 to 8 g of sample. If the acid number is
expected to exceed 7.0. choose an amount of sample
that will contain 0.7 to 0.9 milliequivalents of acid. If
the sample is not sufficiently soluble to enable use of
the above amounts, decrease the sample size as necessary.
Samples exceeding I .O g should be weighed to the
nearest 1 mg. Smaller samples should be weighed to
the nearest 0.1 mg.
25.2 Titrate immediately with 0.1 N KOH
solution at a temperature below 30°C, using a
1 0-mL buret to add the KOH solution and using
phenolphthalein as the indicator. Swirl the solution
vigorously and add the KOH solution dropwise
when approaching the end point. Consider
the end point definite if the color change persists
for 15 s or if it reverses with 2 drops of 0.1 N
HCI .
25.3 Make a blank titration on 50 mL of the
titration solvent and 0.5 mL of the indicator
solution, in the same manner as the sample was
titrated. Record the quantity of 0.1 N KOH
solution required to reach the phenolphthalein
end point.
26. Calculation
26.1 Calculate the acid number, in terms of
milligrams of KOH per gram of sample, as follows:
Acid number = [(A - B)N x 56.l]/W
where:
A = millilitres of KOH solution required for
titration of the sample,
B = millilitres of KOH solution required for
titration of the blank,
N = normality of the KOH solution, and
W- = grams of sample used.
ALKALINITY NUMBER
27. Procedure
27.1 Proceed as directed in Section 25. If the
sample solution is alkaline to phenolphthalein,
add 0.1 N HCI from a 10-mL buret until the
solution is colorless; then add 1.0 mL excess.
Back-titrate to the end point with 0.1 N NaOH
solution from a IO-mL buret. Titrate a blank
containing the same amount of added 0.1 N HC1.
28. Calculation
28.1 Calculate the alkalinity number, in terms
of milligrams of KOH per gram of sample, as
follows:
Alkalinity number = [(B - A )N X 56.1]/U'
where the terms are defined as in Section 26.
29. Report
29.1 For acid and alkalinity numbers below
7.0, report the value to the nearest 0.01.
29.2 For acid or alkalinity numbers of 7.0 or
over, report the value to the nearest 0.1.
30. Precision
30.1 The following data should be used for
judging the acceptability of results (95 % confidence
limits)."
30.1.1 Repeatability-Duplicate results by
the same operator should not be considered suspect
unless they differ by more than the following
amounts:
Acid or
Alkalinity Number
Less than 7.0
7.0 and over
Repeatability
0.1 number
I %
30.1.2 Reproducibility-The average result
reported by one laboratory should not be considered
suspect unless it differs from that of another
laboratory by more than the following amounts:
Acid or
Alkalinity Number
Reproducibility
Less than 7.0
0.3 number
7.0 and over 4%
HYDROXYL NUMBER
31. Scope
31.1 These methods describe the determination
of hydroxyl groups in polymeric glycols and
esters. They may be app!ied, 2s we!!, to the determination
of the hydroxyl function in many
other substances.
31.1.1 Method A-Acetic Anhydride Pressure
Bottle, recommended for polyesters and polyols
used for rigid polyurethane foams.
31.1.2 Method B-Phthalic Anhydride Pressure
Bottle, recommended for polyols used for
flexible and rigid polyurethane foams.
31.1.3 Method C-Phthalic Anhydride Reflux,
recommended for polyols used for flexible
and rigid polyurethane foams.
298

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32. Definition
32.1 hydroxyl number-the number of milligrams
of potassium hydroxide equivalent to the
hydroxyl content of 1 g of the sample.
33. Summary of Methods
33.1 Method A-The sample is acetylated
with a solution of acetic anhydride (Caution, see
Note 7) in pyridine in a pressure bottle at 98°C.
The excess reagent is hydrolyzed with water and
the acetic acid is titrated with standard sodium
hydroxide solution. The hydroxyl content is calculated
from the difference in titration of the
blank and sample solutions.
NOTE 7: Caution-Acetic anhydride and pyridine
are toxic and flammable. In addition, acetic anhydride
is corrosive. Proper precautions should be taken in
handling these reagents.
33.2 Method B-The hydroxyl group is esterified
with a solution of phthalic anhydride in
pyridine in a pressure bottle at 98°C. The excess
reagent is titrated with standard sodium hydroxide
solution.
33.3 Method C-The hydroxyl group is esterified
with a solution of phthalic anhydride in
pyridine under reflux conditions at 1 15°C. The
excess reagent is titrated with standard sodium
hydroxide solution.
34. Interferences
34.1 Excessive amounts of water in the sample
will interfere by destruction of the esterification
reagents. If the water content of the sample exceeds
0.2 %, it is recommended that the sample
be dried.
34.2 Primary and secondary amines and
higher fatty acids react with the reagent to form
stable compounds and would be included in the
analysis.
METHOD A-HYDROXYL NUMBER BY
ACETYLATION
35. Apparatus
35.1 Bag, heavy fabric, with draw string, to
hold bottle (35.2). As an alternative stainless steel
mesh jacket fitted to cover the bottle may be
used.
35.2 Bottle, pressure, heat-resistant, approximately
350-mL.I2
35.3 Buret, 100-mL total capacity, range of
graduated portion 50 mL, 0.1 mL graduation.
NOTE 8-As a substitute. if the 100-mL buret is not
available, the first 50 mL of titrant may be added by
pipet (uniform drainage time for all aliquots) and the
titration completed with a 50-mL buret.
35.4 Steam Bath, 98 k 2"C, containing
enough water to cover the liquid in the sample
bottles. It is critical that the water level be as
prescribed and that the temperature be within
the prescribed range and uniform throughout the
bath.
36. Reagents
36.1 Acetic Anhydride.
36.2 Acetylation Reagent-Mix 127 mL of
acetic anhydride with 1000 mL of pyridine
(36.5). The reagent shall be prepared fresh daily
and kept in a dark bottle. It should not be used
if darker than a pale yellow color.
36.3 Hydrochloric Acid, Standard (0.5 N)-
Prepare and standardize in accordance with Section
18 to 22 of Methods E 200. Determine and
record the temperature at which the standardization
was performed. The concentration of the
solution shall be corrected to the temperature at
which the determination is performed as described
in 36.6. The factor for the thermal expansion
of this solution is 0.00014. This solution is
required only if a correction is to be applied for
presence of strong base in the sample being analyzed.
36.4 Phenolphthalein Indicator Solution-
Dissolve 1 g of phenolphthalein in 100 mL of
pyridine.
36.5 Pyridine, containing 0.30 to 0.45 % wa-
ter-Determine the water content of the pyridine
using Test Method E 203, and add the required
amount of water. The volume of water to add
per litre of pyridine may be calculated as follows:
Water to add, mL = 4.0 - 9A
where A = % water in pyridine.
36.6 Sodium Hydroxide, Standard Solution
(0.5 Xj-Prepare and standardize iri accoidiiiice
with Sections 12 to 17 of Methods E 200. Determine
and record the temperature at which the
standardization was performed. The factor for
thermal expansion of this solution is 0.00014.
For calculation of the hydroxyl content, the normality
of the solution shall be corrected to the
temperature at which the determination is performed
by the following:
"A suitable bottle is available from B. Preiser Co., Inc.,
Catalog No. 10-5485; Chemical Rubber Co., Catalog No.
33052A; and Scientific Glass Co., Catalog No. B-53 17.
299

D 2849
where:
Ntl =
Nt2 =
tl =
t2 =
F =
normality when standardized,
normality during analysis of samples,
temperature of solution ("C) during standardization,
temperature of solution ("C) during analysis
of samples, and
factor to correct for thermal expansion
of the solution (see each solution for
appropriate factor).
37. Procedure
37.1 To each of a sufficient number of pressure
bottles to make all blank and sample determinations
in duplicate, pipet 20.0 mL of the
acetylation reagent. A uniform drainage time
must be used for all aliquots.
37.2 Reserve two of the bottles for the blank
determination. Into the other bottles introduce
an appropriate weight of sample. Determine the
sample weight as follows and weigh to the nearest
0.1 mg.
Sample weight, g
= (56 1 x 0.98)/approximate hydroxyl number
Since the calculated weight will be near the maximum
permitted by the method, adhere closely
to the indicated weight.
37.3 Stopper the bottle and swirl until the
sample is completely dissolved. Enclose each bottle
in a fabric bag and place all bottles as close
together as possible in the steam bath at 98 f
2°C for 2 h. Maintain sufficient water in the bath
to cover the level of liquid in the bottles.
37.4 Remove the bottles from the bath and
allow them to cool to room temperature. Untie
the bags, uncap the bottles to release any pressure,
then remove the bags.
37.5 Carefully rinse any liquid on the stopper
into the bottle and rinse the walls of the flask,
using 20 to 30 mL of water. To each of the bottles
add clean crushed ice until about one half full.
37.6 Add 1 mL of the phenolphthalein indicator
solution and titrate (Note 8) immediately
with the 0.5 N NaOH solution to the first faint
pink end point permanent for 15 s. The solution
should be swirled during the titration, with vigorous
swirling as the end point is reached. Record
the volume of titrant to 0.02 mL (Note 9). Record
the temperature of the NaOH solution.
NOTE 9-If the volume of 0.5 N NaOH solution
required for the sample is less than 80 96 ofthat required
for the blank, the sample was too large and the analysis
should be repeated with a smaller weight of sample.
37.7 Acidity or Alkalinity Correction-If the
sample contains significant acidity or alkalinity,
correct the result as follows.
37.7.1 Weigh into a 400-mL Erlenmeyer flask
an amount of sample equal to that taken previously
for the hydroxyl determination. Add to the
flask 75 mL of redistilled pyridine, 75 mL of
distilled water, and 0.5 mL of phenolphthalein
indicator solution.
37.8 Acidity Correction-If the solution is
colorless, titrate with standard 0.1 N NaOH to a
pink end point that persists for at least 15 s.
Make a blank titration on the reagent mixture
described in 37.7.1, omitting the sample. The
acidity correction in milligrams of KOH per
gram is calculated as follows:
Acidity correction = [(A- B)N X 56.l]/W
where:
A = millilitres of the NaOH solution required
for titration of the sample,
B = millilitres of the NaOH solution required
for titration of the blank,
N = normality of the NaOH solution, and
W = grams of sample used.
37.9 Alkalinity Correction-If the solution in
37.7.1 is pink, titrate to the disappearance of the
pink color with 0.1 N HC1, then add 1 .O mL in
excess. Back titrate with standard 0.1 N NaOH
solution to a pink end point that persists for at
least 15 s. Titrate with standard 0.1 N NaOH
solution a blank containing exactly the same
amount of added 0.1 N HCl and the reagent
mixture described in 37.7.1, omitting the sample.
The alkalinity correction in milligrams of KOH
per gram is calculated as follows:
Alkalinity correction = [(B- A)N X 56.1]/W
where the terms are defined as in 37.8.
38. Calculation
38.1 Calculate the hydroxyl number in milligrams
of KOH per gram of sample as follows:
Hydroxyl number = [(B- A)N x 56.1]/W
where:
A = millilitres of NaOH required for titration
of the sample,
B = millilitres of NaOH required for titration
of the blank,
N = normality of the NaOH, and
300

W = grams of sample used.
38.2 If the sample contains free acidity or
alkalinity as measured in Section 37, the result
in 38.1 must be corrected as follows:
Hydroxyl number (corrected)
= hydroxyl number + acidity, or
Hydroxyl number (corrected)
= hydroxyl number - alkalinity
39. Report
39.1 Report the corrected hydroxyl number
to the nearest 0.1.
40. Precision
40.1 The following data should be used for
judging acceptability of results (95 % confidence
limit). I '
40.1.1 Repeatability-Duplicate results by
the same analyst should not be considered suspect
unless they differ by more than the following
amount:
Hydroxyl Number
Repeatability
Less than 120
I .O hydroxyl number
120 and over I %
40.1.2 Reproducibility-The average result
reported by one laboratory should not be considered
suspect unless it differs from that of another
laboratory by more than the following amount.
Hydroxyl Number
Reproducibility
Less than 120
I .5 hydroxyl number
120 and over 1.5 %
METHOD B-HYDROXYL NUMBER BY
PRESSURE BOTTLE PHTHALA TION
41. Apparatus
4 1.1 Bottles, pressure or storage, borosilicate
glass: I
4 1.2 Pressure Bottle Bags.I4
4 1.3 Buret, Normax, bulb, 100-mL capacity.
42. Reagents
42.1 Pyridine-Distill from phthalic anhydride,
discarding the heads fraction boiling below
114-1 15°C. Store in brown glass bottles.
42.2 Phthalic Anhydride-Pyridine Reagent-Weigh
1 1 1 to 1 16 g of phthalic anhydride
into a 1-qt brown bottle. Add 700 mL of pyridine
which has been distilled from phthalic anhydride
(see 42.1) and shake vigorously until complete
solution is effected. The reagent must stand overnight
before use. Reagent which develops a color
should be discarded. In the blank titration as
described in the following procedure, exactly 25
mL of this reagent must consume between 95
and 100 mL of 0.500 N sodium hydroxide.
42.3 Phenolphthalein Indicator Solution ( 10
g/L)-Prepare a solution of 1 g of phenolphthalein
in 100 mL of pyridine.
42.4 Potassium Acid Phthalate, National Bureau
of Standards standard sample.
42.5 Sodium Hydroxide, Standard Solution
(0.5 N)-Prepare a 0.5 N solution of sodium
hydroxide (NaOH) and standardize as follows:
42.5.1 Crush (do not grind) about 10 g of
potassium acid phthalate (KHCsH404) to a fineness
of approximately 100 mesh and dry for 1 to
2 h at 100°C. Place in a glass-stoppered container
and cool in a desiccator. Accurately weigh 4 to
4.5 gm of the dried potassium acid phthalate and
transfer it to a 500-mL flask that has been swept
free of carbon dioxide. Add 200 mL of water that
is free of carbon dioxide, stopper the flask, and
shake gently until the sample is dissolved. Add
phenolphthalein indicator and titrate to a pink
end point with the 0.5 N NaOH solution using a
50-mL buret.
42.5.2 Calculate the normality of the NaOH
as follows:
Normality = W/( V X 0.2042)
where:
W = grams of KHCsH404, and
V = millilitres of NaOH required for titration
of the KHCsH404.
43. Procedure
43.1 Prepare a sufficient number of clean, dry
pressure bottles to make all blank and sample
determinations in duplicate. Replace the rubber
gaskets, if necessary, and make certain the caps
can be fastened securely.
43.2 Accurately pipet 25 mL of the phthalic
anhydride-pyridine reagent into each of the bottles.
Use the same pipet for both sample and
blank determinations. Do not allow the reagent
to contact the rubber gasket.
43.3 Reserve two of the bottles for the blank
determination.
43.4 Into each of the other bottles introduce
the amount of sample calculated as follows, as
l3 Available from Scientific Glass Apparatus Co. Order No.
B-5317.
" Available from Flaherty-Kennedy Fabrics. 50-H Old Mill
Rd., Wall, NJ 07719.
30 1

D 2849
weighed to the nearest 0.1 mg:
Sample size, g = 56llestimated hydroxyl number
Since the calculated weight will be near the maximum
permitted by the method, adhere closely
to the indicated weight. Use a hypodermic syringe
or similar apparatus to weigh the sample.
Swirl to effect complete solution.
43.5 Cap the bottles and enclose each securely
in the pressure bottle bags. Place the samples and
blanks as close together as possible in a water
bath, maintained at 98 -+ 2"C, for 2 h. Maintain
sufficient water in the bath to just cover the liquid
in the bottles.
43.6 Remove the bottles from the bath and
allow them to cool to room temperature.
43.7 When the bottles have cooled, open the
bags, uncap carefully to release any pressure, and
then remove the bags.
43.8 To each bottle add 50 mL of redistilled
pyridine and 0.5 mL of the phenolphthalein indicator
solution and titrate with standard 0.5 N
NaOH solution to a pink end point permanent
for at least 15 s. It is essential that the net titration
(blank minus sample) be between 18 and 22 mL.
If it is not, repeat the determination, adjusting
the sample size accordingly.
43.9 Acidity or Alkalinity Correction-If the
sample contains significant acidity or alkalinity,
the result must be corrected as follows.
43.9.1 Weigh into a 400-mL Erlenmeyer flask
an amount of sample equal to that taken previously
for the hydroxyl determination. Add to the
flask 75 mL of redistilled pyridine, 75 mL of
distilled water, and 0.5 mL of phenolphthalein
indicator solution.
43.10 Acidity Correction-If the solution is
colorless, titrate with standard 0.1 N NaOH solution
to a pink end point that persists for at least
15 s. Make a blank titration on the reagent
mixture described in 43.9.1, omitting the sample.
The acidity correction in milligrams of KOH per
gram is calculated as follows:
Acidity correction = [(A - B)N x 56.111 W
where:
A = millilitres of the NaOH solution required
for titration of the sample,
B = millilitres of the NaOH solution required
for titration of the blank,
N = normality of the NaOH solution, and
W = grams of sample used.
43.1 1 Alkalinity Correction-If the solution
in 43.9.1 is pink, titrate to the disappearance of
the pink color with 0.1 N HC1, then add 1.0 mL
in excess. Back titrate with standard 0.1 NNaOH
solution to a pink end point that persists for at
least 15 s. Titrate with standard 0.1 N NaOH
solution a blank containing exactly the same
amount of added 0.1 N HCI and the reagent
mixture described in 43.9.1, omitting the sample.
The alkalinity correction in milligrams of KOH
per gram is calculated as follows:
Alkalinity correction = [(B - A)N X 56.1]/W
where the terms are defined as in 43.10.
44. Calculation
44.1 See Section 38.
45. Report
45.1 See Section 39.
46. Precision
46.1 See Section 40.
METHOD C-HYDROXYL NUMBER BY
REFLUX PHTHALA TION
47. Apparatus
47.1 Soil Digestion Flasks, 250-mL capacity
with standard-taper 24/40 joints and 24-in. air
condensers.
47.2 Oil Bath, maintained at 115 k 2°C.
47.3 Buret, Normax, bulb, 100-mL capacity.
48. Reagents
48.1 Pyridine-See 42.1.
48.2 Phthalic Anhydride-Pyridine Reagent-See
42.2.
48.3 Phenolphthalein (10 g/L)-See 42.3.
48.4 Potassium Acid Phthalate-See 42.4.
48.5 Sodium Hydroxide, Standard Solution
(0.5 N)-See 42.5.
49. Procedure
49.1 Weigh into the flasks, by means of a
hypodermic syringe or other suitable equipment,
the amount of sample calculated as follows, and
weighed to the nearest 0.1 mg. No material must
be allowed to touch the neck of the flask:
Sample size, g = 56l/estimated hydroxyl number
Since the calculated weight will be near the maximum
permitted by the method, adhere closely
to the indicated weight.
302

D2849
49.2 Accurately pipet 25 mL of the phthalic
anhydride-pyridine reagent into each flask. Swirl
the flask to effect solution of the sample. Put the
air condensers in place, and place the flasks in
an oil bath, maintained at 115 f 2"C, for I h.
Keep sufficient oil in the bath to cover approximately
one half of the flask.
49.3 After the heating period, remove the assembly
from the bath and cool to room temperature.
Wash down the condenser with 50 mL of
redistilled pyridine, and remove the condenser.
Add 0.5 mL of phenolphthalein indicator solution
and titrate with 0.5 N NaOH solution to a
pink end point that persists for at least 15 s.
49.4 Run a blank in the same manner, omitting
the sample. It is essential that the net titration
(blank minus sample) be between 18 and 22
mL. If it is not, repeat the determination, adjusting
the sample size accordingly.
49.5 Acidity or Alkalinity Correction-See
43.9 through 43.1 1.
50. Calculation
50.1 See Section 38.
51. Report
5 I . 1 See Section 39.
52. Precision
52.1 See Section 40.
UNSATURATION
53. Scope
53.1 This method covers the determination of
unsaturated compounds in polyether-type urethane
raw materials.
54. Summary of Method
54. I Carbon-to-carbon unsaturated compounds
in the sample are reacted with mercuric
acetate and methanol in a methanolic solution
to produce acetoxymercuricmethoxy compounds
and acetic acid. The amount of acetic
acid released in this equimolar reaction, which is
determined by titration with standard alcoholic
potassium hydroxide, is a measure of the unsaturation
originally present. Because the acid cannot
be titrated in the presence of excess mercuric
acetate, due to the formation of insoluble mercuric
oxide, sodium bromide is added to convert
the mercuric acetate to the bromide which does
not interfere. Inasmuch as the method is based
on an acidimetric titration, a suitable correction
must be applied if the sample is not neutral to
phenolphthalein indicator. Care must be taken
to exclude carbon dioxide which titrates as an
acid and gives erroneous results.
55. Interferences
55.1 The method does not apply to compounds
in which the unsaturation is conjugated
with carbonyl, carboxyl, or nitrile groups. Because
water presumably hydrolyzes the reaction
product to form basic mercuric salts, quantitative
results are obtained only when the system is
essentially anhydrous. Acetone in low concentrations
does not interfere significantly, although its
presence may be detrimental to the end point.
Inorganic salts, especially halides, must be absent
from the sample because even small amounts of
salts may nullify the reaction of the mercuric
acetate with the unsaturated compound.
56. Apparatus
56. I Pipet, 50-mL capacity.
56.2 Erlenmeyer Flask, 250-mL, glass-stoppered.
56.3 Balance, 1000-g capacity, 0.1-g sensitivity.
56.4 Buret, 50-mL capacity.
57. Reagents
57.1 Mercuric Acetate, Methanol Solution (40
g/L)-Dissolve 40 g of mercuric acetate
(Hg(C2H302)2) in sufficient methanol to make 1
L of solution and add sufficient glacial acetic acid
to require a blank titration of 1 to 10 mL of 0.1
N alcoholic KOH solution/50 mL of reagent.
Usually 3 or 4 drops of acid are sufficient. Prepare
the reagent fresh weekly and filter before
using.
57.2 Methanol.
57.3 Phenolphthalein Indicator Solution-
Dissolve 1 g of phenolphthalein in 100 mL of
methanol.
57.4 Potassium Hydroxide, Alcoholic Solution
(0.1 N)-Dissolve 6.9 g, of potassium hydroxide
(KOH) pellets in methanol and dilute to
I L. Filter through coarse filter paper if necessary.
Standardize the solution by a suitable method.
57.5 Sodium Bromide (NaBr).
303

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58. Procedure
58.1 Add 50 mL of methanol to a sufficient
number of 250-mL Erlenmeyer flasks to determine
the acidity of each sample in duplicate.
Neutralize to a faint pink end point, using a few
drops of phenolphthalein indicator solution and
0.1 N alcoholic KOH solution. Add 30 g of the
sample weighed to the nearest 0.1 g to each flask
and swirl to effect complete solution. Titrate with
0.1 N alcoholic KOH solution to a pink end
point that persists for at least I5 s and record the
volume of titrant as A.
58.2 Pipet 50 mL of the Hg(C2H302)2 solution
into each of a sufficient number of 250-mL Erlenmeyer
flasks to make all blank and sample
determinations in duplicate. Reserve two of the
flasks for the blank determination. Into each of
the other flasks introduce 30 g of the sample
weighed to the nearest 0.1 g and swirl to effect
complete solution. Allow the samples to stand
together with the blanks at room temperature for
30 min. Swirl the flasks occasionally. Add 8 to
10 g of NaBr crystals to each flask and swirl to
mix thoroughly. Add approximately 1 mL of
phenolphthalein indicator solution and titrate
immediately with 0.1 N alcoholic KOH solution
to a pink end point that persists for at least 15 s.
Record the volume of titrant used for the samples
as D and that used for the blank as E. The sample
titration should not exceed 50 mL of 0.1 N
alcoholic KOH solution.
59. Calculation
59.1 Calculate the concentration of unsaturated
compounds, in terms of milliequivalents
per gram, as follows:
C= (A x N)/W
where:
A = millilitres of 0.1 N alcoholic KOH solutien
required tG neutralize the sample
(58.1),
N = normality of the alcoholic KOH solution,
and
W = grams of sample used.
Therefore,
Total unsaturation = [(D - E)N/ W] - C
where:
D = millilitres of alcoholic KOH solution required
for titration of the sample (58.2),
E = average millilitres of alcoholic KOH solu-
tion required for titration of the blank
(58.2), and
C = milliequivalents of acidity per gram of
sample, average of results from first equation
above.
60. Precision
60.1 The following data should be used for
judging the acceptability of results (95 ?6 confidence
limits)."
60.1.1 Repeatability-Duplicate results by
the same analyst should not be considered suspect
unless they differ by more than 0.002.
60.1.2 Reproducibility-The average result
obtained by one laboratory should not be considered
suspect unless it differs from that of another
laboratory by more than 0.004.
WATER
61. Scope
6 1.1 This Karl Fischer titration is applicable
for water determination in polyesters, polyethers,
and many other organic compounds. The
method is not applicable in the presence of mercaptans,
peroxides, or appreciable quantities of
aldehydes or amines unless suitable modifications
are made.
62. Definition
62.1 electrometric endpoint-that point in the
titration when two small platinum electrodes
upon which a potential of 20 to 50 mV has been
impressed are depolarized by the addition of 0.05
mL of Karl Fischer reagent (equivalent to 2.5 to
3.0 mg H20/mL) causing a change of current
flow of 10 to 20 pA that persists for at least 30 s.
63. Summary of Method
63.1 This method is based essentially upon
the reduction of iodine by sulfur dioxide in the
presence of water. This reaction can be used
quantitatively only when pyridine and an alcohol
are present to react with the sulfur trioxide and
hydriodic acid produced according to the following
reactions:
H20 + 12 + SO2 + 3CsHsN ---*
2CsHsN. HI + C5H5N. SO3
C5H5N. SO3 + ROH + CsHsN. HS04R
63.2 To determine water, Karl Fischer reagent
(a solution of iodine, pyridine, and sulfur dioxide
in ethylene glycol monomethyl ether) is added to
304

a solution of the sample in methanol until all the
water present has been consumed. This is evidenced
by a current measuring device which
indicates the depolarization of a pair of platinum
electrodes. The reagent is standardized by titration
of water.
64. Apparatus
64.1 Titration Vessel-A vessel of approximately
300-mL capacity, such as a tall-form lipless
beaker, provided with a tight-fitting closure
to protect the reaction mixture from atmospheric
moisture. The vessel also shall be fitted with a
nitrogen inlet tube, a IO-mL buret, a stirrer (preferably
magnetic), and a port that may be opened
momentarily for sample and solvent addition or
removal and electrodes. It is convenient to provide
a vacuum line leading to a 1-L trap bottle
for drawing off the titrated solution. The nitrogen
shall be passed through a drying tube containing
anhydrous calcium sulfate (Indicating Drierite)
before entering the titration vessel.
64.2 Instrument Electrodes, platinum with a
surface equivalent of two No. 26 wires, 3/~6 in.
long. The wires should be 3 to 8 mm apart and
so inserted in the vessel that 75 mL of solution
will cover them.
64.3 Instrument Depolarization Indi~ator,’~
having an internal resistance of less than 5000 Q
and consisting of a means of impressing and
showing a voltage of 20 to 50 mV across the
electrodes and capable of indicating a current
flow of 10 to 20 pA by means of a galvanometer
or radio tuning eye circuit.
64.4 Buret Assembly, for Fischer reagent, consisting
of a IO-mL buret with a 0.05-mL subdivisions
connected by means of glass or polyethylene
(not rubber) connectors to a source of
reagent. Several types of automatic dispensing
burets may be used. Since the reagent loses
strength when exposed te mist air a! vents must
be protected against atmospheric moisture by
adequate drying tubes containing anhydrous calcium
sulfate (Indicating Drierite). All stopcock
and joints should be lubricated with a lubricant
not particularly reactive with the reagent. I6
64.5 Weighing Pipet, of the Lung type or
equivalent .
65. Reagents
65.1 Karl Fischer Reagent (equivalent to 2.5
to 3.0 mg water/mL). Dilute commercially avail-
D 2849
able stabilized Karl Fischer reagent” (6 mg H20/
mL) (Note 10) with an equal volume of anhydrous
ethylene glycol monomethyl ether (containing
less than 0.1 % water) (Note 1 1).
NOTE IO-If desired, a suitable concentrated reagent
(6 mg water/mL) may be prepared as follows:
For each L of solution dissolve 133 k 1 g of iodine in
425 +. 2 mL of anhydrous (less than 0.1 % water)
pyridine in a dry, glass-stoppered bottle. Add 425 k 2
mL of anhydrous (less than 0.1 % water) ethylene glycol
monomethyl ether. Cool to below 4°C in an ice bath
and add 70 mL of freshly drawn liquid sulfur dioxide
(SO*) in small increments.
NOTE 1 I-Ethylene glycol monomethyl ether containing
less than 0.1 % water is commercially available
but if drying is desired it may be accomplished by
distillation through a multiple plate column. Discard
the first 5 % of material distilling overhead and use the
95 % remaining.
65.2 Titration Solvent, Anhydrous Methanol-Unless
the methanol is extremely dry it will
require a large amount of dilute Karl Fischer
solution to react with its residual water. For this
reason the solvent should be further dried by
adding undiluted Karl Fischer reagent (6 mg
water/mL) to a bottle of methanol until a light
red-brown color persists. Add methanol until this
color is just removed and the solution is a pale
yellow. A 100 mL portion of the treated solvent
should require a titration of 1 to 10 mL of dilute
Karl Fischer reagent.
66. Standardization of Reagent
66.1 Standardize the Karl Fischer reagent
daily using the same procedure as used for titrating
the sample.
66.1.1 Add 100 mL of titration solvent to the
flask and titrate the residual moisture as described
in Section 68. Add to this titrated solvent
immediately 1 drop of water from a weighing
pipet. Weigh the pipet to kO.1 mg. Complete the
titration with Karl Fischer reagent as described
in sectinn 58. It m2y be necesS2l-y tn refi!! the
buret during the titration.
I’ A type of instrument, similar to the Fisher Scientific Co.
“Junior Titrimeter” or the Precision Scientific Co. “Aquatrator,”
may be used. An instrument providing automatic titration such
as the Beckman “Aquameter,” is convenient if many samples
are involved.
l6 Suitable lubricants are Apiezon N (James L. Biddle and
Co., Philadelphia, PA); High Vacuum Silicone Grease (Dow
Coming Co., Midland, MI); Sisco 300 (Swedish Iron and Steel
Co., New York, NY).
”Suitable Karl Fischer solution may be purchased from
Fisher Scientific Co., 71 I Forbes Ave., Pittsburgh, PA, or Catalog
NO. SO-K-3.
305

D 2849
66. I .2 Calculate the equivalency factor, F, in
terms of milligrams of water per millilitre of the
reagent as follows:
Equivalency factor, F = A/B
where:
A = milligrams of water added, and
B = millilitres of Fischer reagent required.
67. Sampling
67.1 It is essential to avoid changes in the
water content of the material during sampling
operations. Many polyols are quite hygroscopic
and errors from this source are particularly significant
in the determination of the small
amounts of water usually present. Use almostfilled,
tightly capped containers and limit as
much as possible contact of the sample with air
when transfemng the sample to the titration
vessel. Avoid intermediate sample containers, if
possible. If several different analyses are to be
performed on the same sample, determine the
water first and do not open the sample prior to
the actual analysis.
68. Procedure (Note 12)
68.1 Adjust the nitrogen valve to pass dry
nitrogen into the titration vessel at a slow rate
(20 to 50 mL/min). Introduce approximately 100
mL of titration solvent into the titration vessel,
making sure that the electrodes are covered with
solvent. Adjust the stirrer to give adequate mixing
without splashing. Titrate the mixture with
Karl Fischer reagent to the end point (see Section
63).
68.2 To the titration mixture thus prepared,
add an amount of sample as indicated in Table
1. Exercise care when the sample is transferred
so that water is not absorbed from the air particularly
under conditions of high humidity. Allow
the solution to stir a minute or two until dissolution
is complete. Again titrate the mixture with
Fischer reagent to the same end point previously
employed. Record the amount of reagent used to
titrate the water in the sample.
NOTE 12-A slight modification of this procedure
can be used with no effect on the final results as follows:
a known excess of Karl Fischer reagent shall be added
to the titration solvent described in 65.2. The sample
shall then be added and back-titrated with a standardized
water-methanol solution.
69. Calculation
69. I Calculate the water content of the sample
as follows:
Water, % = VF/IOW
where:
V = millilitres of Karl Fischer reagent required
by the sample,
F = equivalency factor for Karl Fischer reagent,
in milligrams of water per millilitre
of reagent, and
W = grams of sample used.
70. Precision
70.1 The following data should be used for
judging the acceptability of results (95 % confidence
limits).’ ’
70.1.1 Repeatability-Duplicate results by
the same analyst should not be considered suspect
unless they differ by more than the following
amount:
Water Content.
% Repeatability
Below 0.5
Over 0.5
0.01 % absolute
2 % relative
70. I .2 Reproducibility-The average result
reported by one laboratory should not be considered
suspect unless it differs from that of another
laboratory by more than the following amount:
Water Content,
% Reproducibility
Below 0.5
Over 0.5
0.02 % absolute
4 % relative
SUSPENDED MATTER
71. Scope
7 I. 1 This method covers a procedure for visual
inspection to determine the presence of insoluble
foreign material.
72. Procedure
72.1 Invert a glass bottle of the sample and
ejtiisiiiii~ “uj; iiaiismiiied light hi the presence or’
suspended matter.
73. Report
73. I Report presence or absence of suspended
matter.
SPECIFIC GRAVITY
74. Scope
74.1 These methods are intended for use in
determining the specific gravity of polyesters by
the pycnometer method.
306

D 2849
75. Definition
75.1 specific gravity-the ratio of the weight
in air of a given volume of the material at a stated
temperature to the weight in air of an equal
volume of water at a stated temperature. It shall
be expressed as specific gravity, 25/25"C, indicating
that the sample and reference water were
both measured at 25°C.
76. Apparatus and Materials
76.1 Pycnometer, of 25 or 50-mL capacity,
conical shape with a capillary side arm overflow
tube complete with a standard-taper 5/ 12
ground-glass joint to receive a ground-glass
vented cap. A thermometer with a scale graduated
from 12 to 38°C in 0.2-" divisions joins the
neck of the flask with a standard-taper 10/18
ground-glass joint. The thermometer contained
in the pycnometer shall be calibrated using the
ASTM thermometer specified in 76.3.
76.2 Water Bath-A water bath capable of
maintaining a temperature of 25.0 A 0.05"C during
the test.
76.3 Thermometer-An ASTM Low Softening
Point Thermometer having a range from -2
to +80"C and conforming to the requirements
for Thermometer 15C as prescribed in Specification
E 1.
76.4 Analytical Balance-A balance having a
sensitivity of between 2 and 3 scale divisions
displacement effected by an excess weight of 1
mg when carrying a load of between 15 and 20 g
in each pan.
76.5 Analytical Weights-Class S weights, as
certified by the National Bureau of Standards, or
equivalent weights.
76.6 Chromic Acid Cleaning Solution-Prepare
a saturated solution of chromic acid (CrO3),
in concentrated sulfuric acid (H2S04, sp gr 1.84).
77- Procedure
77,l Clean the pycnometer by filling it with a
chromic acid cleaning solution allowing it to
stand for a few hours, emptying, and rinsing well
with water.
77.2 Fill the pycnometer with freshly boiled
water that has been cooled to 22 to 24"C, and
put the pycnometer thermometer in place carefully,
avoiding trapping of air. Place the pycnometer
in the water bath maintained at 25.0 +.
0.05"C for at least 30 min. Wipe the overflow
from the side arm capillary and cover with the
vented cap, remove from the bath, wipe dry, and
weigh.
77.3 Empty the pycnometer, rinse successively
with alcohol and ether, remove the ether
vapor, and dry under vacuum for 15 min. Weigh
the pycnometer and subtract the weight of the
empty pycnometer from the weight when filled
with water in order to get the weight, W, of the
contained water at 25°C in air.
77.4 The sample for test must be completely
liquid. If the sample contains solid polyol, warm
the entire sample in the original container until
it becomes liquid. Then cool it to 22 to 24°C and
quickly fill the pycnometer with it, allowing a
minimum of time for exposure of the sample to
the atmosphere.
77.5 Insert the thermometer carefully, avoiding
trapping of air. Cover the side arm with the
vented cap and immerse the pycnometer in the
water bath for at least 30 min. Wipe overflow
from the side arm capillary and cover with the
vented cap, remove from the bath, wipe dry, and
weigh. Subtract the weight of the empty pycnometer
from the weight when filled with sample in
order to obtain the weight, S, of the contained
sample at 25.0"C.
78. Calculation
78.1 Calculate the specific gravity at 25/25"C
as follows:
Specific gravity, 25125°C = SI W
where:
S = grams of sample used (77.5), and
W = grams of water in the pycnometer (77.3).
79. Precision
79.1 The following data may be used for judging
the acceptability of results (95 '% confidence
limit)."
79.1.1 Repeatability-Duplicate results by
the same operator shouid not be considered suspect
unless they differ by more than 0.0002.
79.1.2 Reproducibility-The average result
reported by one laboratory should not be considered
suspect unless it differs from that of another
laboratory by more than 0.0003.
VISCOSITY
80. Scope
80.1 This method is intended for the direct
determination of viscosity of polyesters and pol-
307

D 2849
yethers whose viscosity falls in the range from 10
to 100 000 CP at 25°C or at 50°C. The method
is also applicable to more viscous samples that
are soluble in n-butyl acetate. Other temperatures
and solvents may be used as agreed upon by
purchaser and seller.
81. Definitions
81.1 viscosity-resistance of a fluid to uniformly
continuous flow without turbulence, inertia,
or other forces.
81.2 non-Newtonian flow-rate of flow of a
material that is not proportional to the degree of
force applied.
82. Summary of Method
82.1 The viscosity of resins is measured by
determining the torque on a spindle rotating at
constant speed in the liquid sample which is
adjusted to 25 f 0.1"C or 50 +_ 0.1"C. Samples
with viscosities exceeding 100 000 CP at 50°C
are dissolved in n-butyl acetate (or other solvent)
and the viscosity is determined at 25 k 0.1 "C.
83. Apparatus
83.1 Constant- Temperature Bath, capable of
maintaining temperatures of 25 & 0.1 "C and 50
& 0.1 "C shall be used. Water, water and glycerin,
or oil may be used as the heating medium and
the bath should be provided with heating, stirring,
and thermostating devices.
83.2 Bath and Sample Thermometers, graduated
in 0.1"C subdivisions and standardized for
the range of use to the nearest 0.01"C. ASTM
Saybolt Viscosity Thermometers having ranges
from 19 to 27°C and 49 to 57"C, as specified, and
conforming to the requirements for Thermometers
17C and 19C, respectively, as prescribed in
Specification E 1 are recommended.
83.3 Brookfield Synchro-lectric Viscometer's-Model
LVF with speeds of 60,30, ! 2, and
6 rpm is to be used when available. It is applicable
to the range of 10 to 100 000 cP. If this model
is not available, Model RVF or HAF may be
substituted. However, samples should be heated
or dissolved in the standard way as necessary to
keep the measured viscosity below 100 000 CP
so that the test may be repeated in other laboratories
under similar conditions with Model LVF.
The calibration of the instrument should be
checked periodically by measuring the viscosity
of Brookfield Engineering Laboratories Viscosity
Standard fluids." Standard fluids L-2, L-3, R-I,
R-2, H-1 are suitable for the usual range. The
calibration corrections shall be applied to sample
measurements.
84. Solvent
84.1 n-Butyl Acetate."
85. Preparation of Sample
85.1 The preparation of a homogeneous sample
is of primary importance in viscosity measurements.
A nonuniform temperature distribution
as well as the presence of air bubbles and
traces of extraneous material should be avoided.
Resins are not easily made homogeneous with
respect to temperature and the sample should be
thoroughly mixed and the temperature measured
at several locations in the sample vessel before
determining the viscosity.
86. Preparation of Apparatus
86.1 Attach the viscometer with an adjustable
clamp to a ring stand. Adjust the legs at the base
of the ring stand until the bubble is in the center
of the spirit level on the viscometer. Attach the
spindle that applies to the range expected for the
sample (see Section 88).
87. Choice of Temperature
87.1 Samples that are liquid and have a viscosity
of less than 100 000 CP at 25°C should be
measured at that temperature. Materials that fulfill
this requirement only when heated from 25
to 50°C should be measured at 50°C. If the sample
viscosity exceeds 100 000 CP at 50°C, the
sample may be dissolved in butyl acetate (70 or
35 % solids) and the viscosity of the solution
measured at 25°C. Other temperatures and solvents
may be used by agreement.
88. Choice of Spindle and Rotational Speed
88.1 The recommended Brookfield Synchrolectric
Viscometer models" offer a variety of
spindle sizes and rotational speeds. In the case of
non-Newtonian liquids, varying these factors will
cause variation in the results obtained. In general,
l8 Obtainable from the Brookfield Engineering Laboratories,
Stoughton, MA.
l9 n-Butyl acetate, Catalog No. B-396, obtainable from Fisher
Scientific Co., 7 I I Forbes Ave., Pittsburgh, PA, or Baker reagent
obtainable from A. H. Thomas Co., Philadelphia, PA, or material
of equivalent punty may be used.
308

D 2849
the following recommendations should guide in
the choice of spindle size and speed to be used
for a specific sample.
88.1.1 The combination chosen should give
an instrument reading near the center of the scale
(that is, 175 to 325 on the 500 scale).
88.1.2 The lowest possible speed consistent
with fulfilling the requirement given in 88.1.1
should be used in order to deemphasize certain
types of nowNewtonian behavior.
88.1.3 If these two recommendations conflict,
the requirements given in 88.1.1 have preference.
89. Procedure
89.1 Place sufficient sample in a 600-mL lowform
beaker to cover the immersion mark on the
viscometer spindle. Cover the beaker with a
watch glass and immerse to the sample level in
the constant temperature bath. Stir occasionally
without trapping air bubbles. Check the temperature
at several different locations in the beaker
to make sure uniformity has been achieved. After
the desired temperature has been observed
throughout the sample for 10 min, immerse the
viscometer spindle and guard into the sample to
the immersion line marked on the spindle. Caution
should be exercised to avoid air bubbles
gathering under the spindle during immersion. If
bubbles are observed, detach the spindle, keeping
it in the sample, and stir until the bubbles are
released. Reinsert the spindle.
89.2 Press down the viscometer clutch lever
and start the motor by snapping the toggle switch.
Release the clutch lever and allow rotation to
continue until the spindle has made eight or ten
revolutions. Depress the clutch lever, stop the
motor, and read the scale. If, when operating at
higher speeds the pointer is not in view when the
dial has come to rest, throw the motor switch on
and off rapidly until the pointer reaches the
window.
89.3 Repeat the procedure until 3 readings on
the 500 scale agree within 5 units.
90. Calculations
90.1 Multiply readings on the 500 scale by the
factors given in Table 2 to obtain viscoity in
centipoises.
90.2 At 60 r/min, air resistance on the pointer
has a certain effect. Values obtained should be
reduced as follows: No. 1 spindle, deduct 0.4 cP;
No. 2 spindle, deduct 2.0 cP; No. 3 spindle,
deduct 8.0 cP; No. 4 spindle, deduct 40.0 cP.
90.3 Apply all calibration corrections mentioned
in 83.3.
91. Report
9 I. 1 The report shall include the following:
9 1.1.1 Temperature of test,
91.1.2 Solids content and solvent, if sample
was diluted,
91.1.3 Model of viscometer,
91.1.4 Speed of rotation,
91.1.5 Spindle number, and
91.1.6 Viscosity in centipoises.
COLOR
COLOR OF POLYESTERS AND POL YETHERS
BY THE GARDNER METHOD
92. Scope
92.1 This method covers the visual measurement
of the color of essentially clear liquids. It is
applicable only to materials in which the colorproducing
bodies present have light absorption
characteristics similar to those of the standards
used.”
93. Apparatus
93. I Gardner-Holdt Tubes, of clear glass, with
closed, flat, even bottoms, and having the following
approxhate dimensions and markings:
93.1.1 A uniform internal length of 1 I2 mm,
93.1.2 A uniform internal diameter throughout
the length of the tube of 10.75 mm, and
93.1.3 An etched line around the outside of
the tube 5 mm from the open end and a second
etched line around the outside of the tube 13
mm from the open end.
94. Reagents
94.1 Cobalt Chloride Solution-Prepare a solution
containing l part by weight of cobalt chloride
(CoCI2. 6H20) to 3 parts of HCI ( 1 -t 17).
94.2 Ferric Chloride Solution-Prepare a solution
containing approximately 5 parts by
weight of femc chloride (FeCI3 6H20) and 1.2
parts of HCl ( 1 + 17). Adjust to exact color equivalence
to a freshly prepared solution containing
3 g of K2Cr207 in 100 mL of H2S04 (sp gr I .84).
See Test Method D I209 and Standard Methods for the
Examination of Water, Sewage, and Industrial Wastes, Am.
Public Health Assn., 10th Ed., 1955. New York, NY, pp. 87-
89.
309

D 2849
94.3 Hvdrochloric Acid (1+17)-Mix 1 volume
of concentrated hydrochloric acid (HCl, sp
gr 1.19) with 17 volumes of water.
94.4 Hydrochloric Acid (0.1 N)-Prepare 0.1
N HCl.
94.5 Potassium Chloroplatinate (K2PtC16).
94.6 Potassium Dichromate ( K2Cr207).
94.7 Sulfuric Acid (sp gr 1.84)-Concentrated
sulfuric acid (H2S04).
95. Gardner Color Reference Standards
95.1 The primary standards for color shall
consist of solutions defined by their spectral
transmittance in a 1-cm cell with parallel sides.
The chromaticity coordinates of these solutions
shall conform to those given in Table 3 when
determined on a 1-cm layer of the solution in
accordance with Method E 308.
95.2 For purposes of comparison, the use of
permanent solutions, the color of which has been
determined, is more satisfactory. The approximate
composition of solutions giving each of the
18 Gardner colors is also given in Table 3. The
solutions shall be made from K2PtC16 in 0.1 N
HC1, or, in the darker colors, from stock solutions
of Feel3, CoC12, and HCl (93.1, 93.2, and 93.3).
95.3 Solutions of K2Cr207 in H2S04 (sp gr
1.84) may be used as reference standards. The
approximate composition of these standards is
also given in Table 3. Each solution must be
freshly made for the color comparison, using
gentle heat, if necessary, to effect solution.
NOTE 13-Secondary reference standards may be
obtained in the form of 18 colored glass disks, which
are set into a pair of larger, plastic disks and the latter
mounted to rotate in a housing for holding the sample
tube and glass disk in close and fixed proximity.”
96. Procedure
96.1 Fill the tube with sample, free of solid
partic!es OF air bibbles SO that the appaicfit tipper
edge of the liquid meniscus is even with the lower
etched line on the tube.
96.2 Determine the color by comparison with
the reference standard solutions prescribed in
Table 3, by comparing the sample and the standard
in Gardner-Holdt viscosity tubes as described.
Make the comparison at 25 f 5°C by
placing tubes close together and looking through
them against a background that is substantially
equal in color to the northern sky.
97. Report
97.1 Report the color of the sample in terms
of the Gardner standard number that is nearest
to it in color.
APHA COLOR
98. Scope
98.1 This method covers the visual measurement
of the color of essentially clear liquids. It is
applicable only to materials in which the colorproducing
bodies present have light absorption
characteristics similar to those of the standards
used.I6
99. Apparatus
99.1 Nessler Tubes, matched 100-mL, tallform.
100. Reagents
100.1 Hydrochloric Acid (sp gr l.l9)-Concentrated
hydrochloric acid (HCl).
110.2 Potassium Chloroplatinate (K2PtC16).
101. Preparation of Color Standards
101.1 Measure 500 mL of water into a 1000-
mL volumetric flask. Add 100 mL of the HCl
and mix well. Weigh 1.245 g of K2PtC16 to the
nearest I mg and transfer to the flask (Note 14).
Dilute the solution in the flask to the mark with
water and mix thoroughly. The color of this
standard solution is equivalent to 500 units (500
mg metallic platinum/L), that it, each millilitre
of the standard contains 0.5 mg of metallic platinum.
NOTE 14-If potassium chloroplatinate is not available,
dissolve 0.500 g of pure metallic platinum in aqua
regia with the aid of heat; then remove HN03 by
repeated evaporation with fresh portions of HCI. Dissolve
this product as directed in 10 I. 1.
101.2 Prepare the required color standards by
diluting the No. 500 standard solution as shown
in Table 4. If more exact color comparison is
desired, prepare additional standards to supplement
those given below. One color unit is equivalent
to 1 mg metallic platinum/L. Protect these
*’ The pair of disks and a comparator housing may be obtained
as Set 605 from Hellige, Inc., 877 Steward Ave., Garden
City, NJ. Although these disks are marked “Hellige” they should
not be confused with the Hellige ( 1930) series of color standards
which were designated I L, I, 2L, 2, etc.
3 10

D2849
standards against evaporation and contamination
when not in use.
102. Procedure
102.1 Transfer 100 mL of the sample to one
of two matched 100-mL tall-form Nessler tubes.
Fill the second tube to the mark with the standard
that seems to match the color of the sample as
indicated by a preliminary estimation. Compare
the colors of the sample and the standard by
viewing vertically down through the tubes against
a white background. Replace the liquid in the
second tube with lighter or darker standards until
an exact match is obtained.
103. Report
103.1 Report the color of the sample in terms
of the color standard number that is nearest to it
in color.
Water Content,
%
TABLE 2 Correction Factors Corresponding to Various
TABLE 1 Recommended Sample Sizes Combinations of Spindles and Rotational Speeds
Sample Size," g
Below 0.5 weight containing approximately 25 mg
of water. This weight should not exceed
30 g.
Over 0.5 5
"Samples of smaller size may be used if the sample is not
suficiently soluble. Viscous samples exceeding I g may be
poured from a small bottle (20 to 50-mL capacity) and weighed
by subtraction to f5 mg. Smaller samples should be weighed to
f0. I mg in a Lunge pipet. Nonviscous samples may be weighed
in a Lunge pipet or in a weighing bottle fitted with a medicine
dropper. Solid samples that melt under 50°C may be liquefied
by heating for a minimum length of time in an oven at 50°C.
The sample bottle closure should be loosened slightly and the
sample should be removed from the oven as soon as it is melted.
Spindle
No.
Correction Factors
Rotational 6 12 30 60
speed, rpm
LVF I 2 1 0.4 0.2
2 IO 5 2 1
3 40 20 8 4
4 200 100 40 20
Rotational 2 4 10 20
speed, rpm
RVF I IO 5 2 I
2 40 20 8 4
3 100 50 20 IO
4 200 100 40 20
5 400 200 80 40
6 1000 500 200 100
7 4000 2000 800 400
Rotational 1 2 5 IO
sueed, rpm
HAF I 40 20 8 4
2 160 80 32 16
3 400 200 80 40
4 800 400 160 80
5 1600 800 320 160
6 4000 2000 800 400
7 16000 8000 3200 1600
31 1

~
TABLE 3 Gardner Reference Standard Color Solutions
Chromaticity
Coordinates
Iron-Cobalt Solutions
Gardner
Potassium
Potassium
Color
Standard
Chloroplatinate,
g/’Oo0 mL Of
Fenic
Chloride
Cobalt
Chloride
Hydrochloric
Dichromate,
g/100 mL
Number .Y I’ 0. I N HCI Solution. Solution. Acid. SUIfUriC Acid”
mL mL mL
I
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
0.3190
0.3241
0.33 I5
0.3433
0.3578
0.3750
0.4022
0.4 179
0.4338
0.4490
0.4836
0.5084
0.5395
0.5654
0.5870
0.6060
0.6275
0.6475
0.327 1
0.3344
0.3456
0.3632
0.3820
0.4047
0.4360
0.4535
0.4648
0.4775
0.4805
0.4639
0.445 I
0.4295
0.41 12
0.3933
0.3725
0.3525
0.550 0.0039
0.865 0.0048
1.330 0.007 I
2.080 0.01 I2
3.035 0.0205
4.225 0.0322
6.400 0.0384
7.900 0.0515
3.8 3.0 93.2 0.0780
5.1 3.6 91.3 0.164
7.5 5.3 87.2 0.250
10.8 7.6 81.6 0.380
16.6 10.0 73.4 0.572
22.2 13.3 64.5 0.763
29.4 17.6 53.0 1.044
37.8 22.8 39.4 1.280
51.3 25.6 23.1 2.220
100.0 0.0 0.0 3.00
” The dichromate color standards have been found to be less reliable than chloroplatinate or iron-cobalt color standards. They
are included in Table 3 for reference only.
TABLE 4 APHA Color Standards
Color No. 500 Water,
Standard No. Standard, mL mL
I
3
5
IO
15
18
20
25
30
40
50
60
70
80
90
100
I20
I40
160
I80
200
300
400
500
0.2
0.6
1 .O
2.0
3.0
3.6
4.0
5.0
6.0
8.0
10.0
12.0
14.0
16.0
18.0
20.0
24.0
28.0
32.0
36.0
40.0
60.0
80.0
100.0
99.8
99.4
99.0
98.0
97.0
96.4
96.0
95.0
94.0
92.0
90.0
88.0
86.0
84.0
82.0
80.0
76.0
72.0
68.0
64.0
60.0
40.0
20.0
0.0
The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject IO revision at any time by the responsible technical committee and must be reviewed every five years and
ij not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you &el that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.
3 12

eB
Designation: D 2979 - 71 (Reapproved 1982)"
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 49103
Reprinted from the Annual Book of ASMA Standards, Copyright ASTM
If not listed iwthe current combined index, will apped in the next edition.
Standard Test Method for
PRESSURE-SENSITIVE TACK OF ADHESIVES USING AN
INVERTED PROBE MACHINE'
This standard is issued under the fixed designation D 2979; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
'' NoTE--Section 2 was added editorially and subsequent Seaions renumbered in April 1985.
1. scope
1.1 This test method covers measurement of
the pressure-sensitive tack of adhesives. This test
method is applicable to those adhesives which
form a bond of measurable strength rapidly upon
contact with another surface and which can be
removed from that surface cleanly, that is, without
leaving a residue visible to the eye. For such
adhesives, tack may be measured as the force
required to separate an adhesive and the adherend
at the interface shortly after they have been
brought into contact under a defined load of
known duration at a specified temperature.
2. Applicable Document
2.1 ASTMStandard:
E 17 1 Specification for Standard Atmospheres
for Conditioning and Testing Materials'
3. Summary of Method
3.1 This test method involves bringing the tip
of a cleaned probe of defined surface roughness
into contact with the adhesive at a controlled
rate, under a fixed pressure, for a short time, at
a given temperature; and subsequently breaking
the bond formed between the probe and adhesive,
also at a controlled rate. Tack is measured
as the maximum force required in breaking the
adhesive bond.
4. Significance and Use
4.1 This test method provides a quantitative
measure of the pressure-sensitive tack of the adhesive.
4.2 The method is designed for the adhesive
mass itself and is suitable for measuring the tack
of pressure-sensitive adhesives for use on both
rigid and flexible backings.
4.3 This test method is suitable for quality
control and research purposes.
5. Apparatus
5.1 Probe-A Type 304 stainless steel rod, 5.0
mm (0.197 in.) in diameter, machined at one
end of 90' to the longitudinal axis. The tip shall
be finished to a surface roughness of not more
than 500 or less than 250 nm (20 to 10 pin.) rms
as measured by a surface-measuring device.'
NOTE 1-When the adhesive is supported on flexible
backings, or is greater than 0.25 mm (0.010 in.)
thick, a probe with a spherical crown of 0.05 mm (0.002
in.) high, and with a 62.5-mm (2.5-in.) radius may be
Used.
5.2 Pressure-Loading Weight-An annular
ring whose inside diameter is slightly larger than
the probe diameter. The ring weight shall be such
that the pressure applied to the sample is 9.79 f
0.10 kPa ( 1.42 psi).
NOTE 2-Contact pressures of 0.98, 1.96, or 4.90
kPa may be obtained by employing annuli of different
weight. These lower pressures as well as ones of 98 kPa
or higher can be used to show the effect of pressure
directly when tack is pressuredependent.
' This test method is under the jurisdiction of ASTM Committee
D14 on Adhesives and is the direct responsibility of
Subcommittee D14.10 on Working Properties.
Current edition approved Sept. 24, 1971. Published November
1971.
Annual Book of ASTM Standards, Vol 15.09.
'An example of a suitable surface-measuring device is a
Surfindicator manufactured by Could, Inc., Gage and Control
Div., 4601 Arden Dr., El Monte, CA.
313

D 2979
5.3 Forge Gage-A spring device with a dial
indicator that retains the maximum force reading
until reset manually. The spring characteristics
shall be such that between 8.9 and 22.2 N (2'and
5 lb) are required to extend it the permissible 2.5
mm (0.10 in.). The probe shall be mounted directly
on the force gage.
NOTE 3-0ther force-measuring devices such as
strain gage load cells, or devices with different forcedeflection
characteristics may be used in certain instances.
Tack values obtained with these devices will
differ in magnitude but will be related to standard
values obtained with the specified gage.
5.4 Testing Machin&-A mechanical system
for bringing the adhesive into contact with the
probe, automatically controlling the dwell time
during which the adhesive and probe are in contact
under pressure, and subsequently pulling the
adhesive away from the probe. The machine shall
be capable of maintaining a constant crosshead
speed of 10 f 0.1 mm/s (24 in./min), sensing
contact of probe with adhesive, stopping for 1 f
0.01 s, and then reversing at the same 10 f 0.1-
mm/s speed. The machine must support the
probe such that its top surface is parallel to the
plane of the adhesive at the time of contact to
less than a 0" 10 min angle between them.
NOTE 4-For some special purposes it may be desirable
to measure the tack at dwell times as short as
0.1 s or as long as 100 s, depending on how quickly the
adhesive bond is to be established in the end use.
6. Test Specimens
6.1 Adhesive shall be cast from solution, dispersion,
or as hot melt, etc. on 38-pm (1.5-mil)
polyester film to give a dried adhesive thickness,
preferably between 0.04 and 0.25 mm (0.0015
and 0.01 in.), but always greater than 0.025 mm
(0.001 in.) and less than 0.5 mm (0.02 in.). A
minimum of two adhesive films shall be made,
one from each of two separately prepared but
identical solutions. The adhesive film shall be
dried in a dust-free atmosphere to constant
weight before testing.
NOTE 5-Other films may also be used provided
they do not react with the adhesive or elongate excessively
during the test. Microscope slides or cover glasses
may be used to give rigid support to the adhesive.
6.2 Adhesives already on some supporting
material shall be examined as they exist.
7. conditioning
7.1 Testing Room-Test in a standard labo-
ratory atmosphere, in accordance with Specification
E 171.
8. procedure
8.1 Clean the probe with an absorbent material
such as surgical gauze or tissue wet with a
completely volatile solvent that is a good solvent
for the adhesive under test. To be suitable, the
material must be lint-free during use, absorbent,
and contain no additives that are soluble in the
cleaning solvents used. Wipe with another piece
of solvent-wet absorbent material, and finally
wipe the probe with a clean dry piece of absorbent
material to remove excess solvent. Wait 20 s or
a sufficiently longer time if necessary, to allow
for complete evaporation of the solvent and temperature
equilibration.
8.2 Place an appropriately sized sample of
supported adhesive, sticky side down, on the
annular ring weight. The sample need only be
large enough to cover the hole in the weight
without slippage during the test and should be
small enough so that it does not adhere to the
carrier supporting the weight. Place the weight in
the carrier.
NOTE 6-The proper relation of the supported adhesive
on the ring weight to the probe is sketched in
Fig. 1. One possible arrangement of the canier and
force gage is also illustrated.
8.3 At a speed of 10 f 0.1 mm/s, bring the
probe into contact with the adhesive. After a
dwell time of 1.0 f 0.01 s separate the probe
from the adhesive at 10 f 0.1 mm/s.
8.4 Record the tack as the maximum force in
newtons required to separate the probe from the
adhesive.
8.5 Make at least five determinations taken at
random points on the supported adhesive. With
grossly rough or nonuniform adhesive surfaces
more than five determinations may be necessary
to obtain the desired statistical reliability of the
average tack value.
8.6 Clean the probe surface with solvent after
each test. In instances where tack values neither
tend to increase or decrease systematically, cleaning
may be limited to each series of test on a
given adhesive.
Nom 7-If there is evidence of contamination by
lint, large dust particles, thumb prints, etc., the test shall
'An example of a suitable machine is the Polyken Robe
Tack Tester availabk from Testing Machines, Inc., Mineoh,
Long Island. NY.
3 14

D 2979
be discounted. If the probe surface shows to the unaided
eye presence of deposited adhesive, the test shall also
be discounted.
9. Report
9.1 The report shall include the following:
9.1.1 Identification of the adhesive,
9.1.2 Solvent used for dissolving the adhesive,
9.1.3 Percent solids contained in solution,
9.1.4 Temperature and time of drying used,
9.1.5 Conditioning time for the adhesive sur-
face,
9.1.6 Adhesive thickness,
9.1.7 Solvent used to clean probe,
9.1.8 Supporting backing material for the adhesive,
9.1.9 Separation rate of the probe,
9.1.10 Dwell time,
9.1.1 1 Contact pressure,
9.1.12 Temperature and relative humidity if
different from standard laboratory astmosphere,
and
9.1.13 Values of each of the tack readings,
and the arithmetic average. Tack values shall be
reported in newtons.
NOTE 7-Items 9.1.2, 9.1.3, and 9.1.4 need be reported
only if the adhesive is put in solution by the
person making the tack test.
315

f
A-Adhesive
&Backing
C--carrier
W-Weight
P--probe
G--Gage
The American Society for Testing and Materials takes no position respecling the validity of any patent rights asserted in connection
with any item mentioned in this stahid. Users of this standard are expressly advised that determination ofthe validity of any such
patent rights, and the risk of infingement ofsuch rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed evev/ive years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive carejid consideration at a meeting of the
responsible technical committee, which you may attend. ljyou feel thnt you comments have nol received a fair hearing you should
make your views known to the ASTM Committee on Standards. I916 Race St.. Philadelphia, PA 19103.
316

#iTb
Designation: D 31 11 - 76 R82
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa., 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined Index. will appear in the next edition
Standard Recommended Practice for
FLEXIBILITY DETERMINATION OF HOT MELT
ADHESIVES BY MANDREL BEND TEST
METHOD’
This Standard is issued under the fixed designation D 3 11 I; the number immediately following the designation indicates
the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the
year of last reapproval.
1. Scope
1.1 This recommended practice covers the
determination of the flexibility of a hot melt
adhesive in sheet form under specific test conditions.
This is a working test. Its results are
useful for comparing adhesives, not for absolute
characterization of adhesives.
2. Applicable Documents
2.1 ASTM Standards:
D 1737 Test for Elongation of Attached
Organic Coatings with Cylindrical Mandrel
Apparatus2
E 171 Specification for Standard Atmospheres
for Conditioning and Testing
Materials
2.2 Other Methods:
Federal Test Specification U. S. 141A,
Method 6221, Flexibility .
NOTE I-Although no tests related specifically to
flexibility of unsupported hot melt adhesives in
sheet form, the above tests concerned with film flexibility
of coatings (supported films) are similar.
3. Summary of Practice
3.1 Test strips of a hot melt adhesive properly
sized and conditioned, are bent 180 deg
over a mandrel (rod). Using a fresh specimen
for each test, the test is repeated with smaller
diameter mandrels until the adhesive tails on
bending. The flexibility of the adhesive is the
smallest diameter mandrel over which 4 out
of 5 test specimens do not break.
4. Significance
4.1 The “Mandrel Bend” test is simple
and fast. It requires little investment in equip-
ment and little operator training. The prime
purpose is to determine whether a hot melt
adhesive meets flexibility requirements. This
test is also useful for comparing flexibility of
several adhesives. It can be used to design
adhesives by comparing the flexibility of various
formulations to meet specific end use
parameters. The adhesive flexibility ean be
determined at temperatures other than ambient
by conditioning the test apparatus and
test specimens at the desired temperature and
performing the test under these temperature
conditions.
5. Apparatus
5.1 The test apparatus consists of a series
of different diameter cylindrical rods or
mandrels supported at each end. There should
be enough space to permit placement of the
flat side of a test specimen tangentially at
right angles to the longitudinal axis of the test
mandrel. Individual requirements determine
the diameter and lengths of the rods needed.
For most tests, 3.2 mm (- k in.), 6.4 mm (- ‘11
in.), and 12.8 mm (-h in.) diameter by 75
to !50 mm (-3 in. tn in.) !ong rods made of
brass or stainless steel are satisfactory. Figure
1 describes two simple test frames, one
with fixed mandrels and the other designed to
take any diameter mandrel.
I This recommended practice is under the jurisdiction of
Committee D-14 on Adhesives.
Current edition approved July 30, 1976. Published September
1976. Originally published as D 31 11 - 72 T. Last
previous edition D 31 11 - 72 T.
Annual Book oJASTM Slandards, Part 27.
Annual Book of ASTM Standards. Parts 35 and 41.
317

D 3111
6. Test Specimen
6.1 The test specimen dimensions can be
varied depending on the end use requirements
of the hot melt adhesive. Figure 2 describes
a recommended specimen size. It is IO
mm (approx 0.4 in.) wide, 75 mm (approx 3
in.) long and 1.25 f 0.01 mm (approx 0.05
in.) thick. The thickness dimension is critical
and must be accurately measured. The test
specimens shall be cut from molded or extruded
sheets or film. Plying of several
thinner samples shall not be permitted. No
flaws visible anywhere in the sample to the
naked eye shall be permitted.
7. Conditioning
7.1 Store the test specimens and test apparatus
at the test conditions for 24 h. Perform
the test under these same conditions. For
rapid screening, particularly at low temperatures,
a minimum of 4 h conditioning can be
used. Note this change when recording data.
If other conditions are not specified, the
storage and test conditions will be 23 f 2 C
and 50 f 5 percent relative humidity. Method
E 171, details these and other tests conditions.
8. Failure
8.t Failure is a visible fracture, crazing, or
cracking of the hot melt adhesive. This can
occur at any time during the bending of the
adhesive test specimen over the mandrel.
Color changes or blushing not affecting the
tensile properties of the material is not a failure,
but should be reported.
9. Procedure
9.1 Run the tests in the same-environment
used to condition the test specimens and test
apparatus.
9.2 Put the largest diameter mandrel in the
horizontal operating position in the test
frame.
9.3 Grasp the test specimen between the
thumb and forefinger of one hand with the
longest dimension between the fingers. For
low temperature testing, use ordinary cotton
work gloves to insulate the test specimens
from the warm fingers.
9.4 Lay the flat-side of the test specimen
tangentially at right angles to the longitudinal
axis of the test mandrel.
9.5 Within 1 s, fold the test specimen 180
deg to form an inverted ‘‘U” shaped angle
over the mandrel maintaining intimate contact
with the mandrel.
9.6 If no failure occurs, fold a fresh specimen
over the next smaller diameter mandrel.
Repeat the test using a fresh sample each
time until failure occurs.
9.7 Now repeat the test 5 times using 5
fresh test specimens on the smallest diameter
mandrel at which failure had not occurred. To
be significant, at least 4 out of 5 test specimens
must pass. Follow this procedure with
smaller or larger diameter mandrels until 4
out of 5 test specimens pass.
9.8 Record the flexibility of the hot melt
adhesive as
over which 4
the smallest diameter mandrel
out of 5 test specimens passed.
10. Report
10.1 The report should include the following:
IO. 1.1 Method of specimen preparation,
molded, extruded, or other method.
IO. 1.2 Specimen dimensions, especially
thickness to within 0.01 mm (K in.).
IO. 1.3 Conditioning and test conditions,
temperature and, if important, relative humidity.
IO. I .4 Smallest diameter mandrel over
which 4 out of 5 test specimens did not fail.
10.1.5 Color changes or blushing of nonfailing
test specimens after bending.
318

FIXED TEST MANDREL
TEST MANDREL
FRAME
VARIABLE TEST MANDRAL
(Note 1 Recess to fit test frame) Figures in parentheses are approximate.
FIG. 1 Test Mandrel (Various Diameters) for Test Frame.
319

FIG. 2
Test Specimen.
1.25 2 0.01MM (0.05")
4
0 5
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted
in connection with any item mentioned in ihis standard. Users ofthis standard are expressly advised thai deiermination of the
validity of any such patent rights, and the risk of infringement of such rights, is entirely their own responsibility.
320

ab
AMERICAN
Designation: D 3166 - 73 p.79
SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa., 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
Standard Method of Test for
FATIGUE PROPERTIES OF ADHESIVES IN SHEAR
BY TENSION LOADING (METAL/METAL)'
This Standard is issued under the fixed designation D 3166; the number immediately following the designation indicates the
year of original adoption or. in the case of revision. the year of last revision. A number in parentheses indicates the year of
last approval.
1. Scope
INTRODUCTION
The purpose of this test procedure is to provide for the determination of the fatigue
properties of adhesives. The accuracy of the results of strength tests of adhesive bonds
will depend on the conditions under which the bonding process is carried out. Unless
otherwise agreed upon by the manufacturer and the purchaser, the bonding conditions
shall be prescribed by the manufacturer of the adhesive. In order to ensure that
complete information is available to the individual conducting the tests, the manufacturer
of the adhesive shall furnish numerical values and other specific information for
each of the following variables:.
(I) Procedure for preparation of the surfaces prior to application of the adhesive, the
cleaning and drying of metal surfaces, and special surface treatments such as sanding,
which are not specifically limited by the pertinent test method.
(2) Complete mixing directions for the adhesive.
(3) Conditions for application of the adhesive, including the rate of spread or
thickness of film, number of coats to be applied whether to be applied to one or both
surfaces, and the conditions of drying where more than one coat is required.
(4) Assembly conditions before application of pressure. including the room temperature,
length of time, and whether open or closed assembly is to be used.
(5) Curing conditions, including the amount of pressure to be applied, the length of
time under pressure, and the temperature of the assembly when under pressure. It
should be stated whether this temperature is that of the glue line, or of the atmosphere at
which the assembly is to be maintained.
(6) Conditioning procedure before testing, unless a standard procedure is specified,
including the length of time, temperature, and relative humidity.
A range may be prescribed fer any i~ariab!e by the m:rnufzc!urer of the adhe~ive, if it
can be assumed by the test operator that any arbitrarily chosen value within such a
range or any combination of such values for several variables will be acceptable to both
the manufacturer and the purchaser of the adhesive.
I. 1 This method covers the measurement of ' This method is under the jurisdiction of ASTM Comfatigue
strength in shear by tension loading of
adhesives on a standard specimen and under
m i ~ ~ r ~ ~ Mar, ~ I, 4,973, e Published ~ ~ April i ~ ~ ~ ~ ~
1973.
321

D 3166
specified conditions of preparation, loading,
and testing.
NOTE I-While this method is intended for use in
metal-to-metal applications it may be used for
measuring the fatigue properties of adhesives using
plastic adherends. provided consideration is given to
the thickness of the plastic adherends. Doublers may
be required for plastic adherends to prevent bearing
failure in the adherends.
NOTE 2-A variation in the thickness of the
adherends can influence the test results. For this
reason, the thickness of the sheets used to make the
test specimens shall be specified in the material
specification. When no thickness is specified. metal
adherends 1.63 mm (0.064 in.) thick are recommended.
2. Applicable Documents
2. I ASTM Standat-&
D 1002 Test for C,rrengrh Properties of
Adhesives ir. Shear by Ten\lon Loading
{Metal to
3. Apparatus
3.1 Testing Machine-The testing machine
shall be capable of applying a sinusoidal cyclic
axial load. The cyclic rate and type of equipment
(constant load or constant displacement)
can influence test results. For this reason, the
cyclic rate and equipment used shall be specified
in the material specification. When no
cyclic rate is specified 1800 cycles per minute is
recommended. The machine shall be provided
with suitable grips and jaws so that the specimen
can be gripped tightly and held in alignment
as the load is applied. Loads shall be
accurate within 3=2 9%.
4. Test Specimens
4.1 Test specimens shall conform to the
shape and dimensions shown in Fig. I. Grip
ends shall be-suitable for use in the particular
testing machine. These specimens are similar
to the tension lap-shear specimens described in
Method D 1002.
4.2 At least 25 specimens shall be tested,
representing at least 4 different panels.
4.3 Prepare, cut, finish, and condition the
specimens in the same manner as for Method
D 1002. The length of the overlap shall be 9.5
mm (0.38 in.) for 1.63 mm (0.064 in.) aluminum
alloys. Dimensions of other materials
shall be such that failures occur in the bond.
(An overlap of 12.7 mm (0.50 in.) for 6.4 mm
(0.25 in.) thick nonmetals should be used if
possible).
5. Procedure
5'. 1 Unless otherwise specified test the specimens
in an atmosphere maintained at 50 + 4 9%
relative humidity and 23 f 1.1 C (73.5 f 2 F).
Precondition the specimens for at least 16 h.
5.2 Place the specimen in the jaws of the
testing machine and grip tightly so that the
specimen and the jaws are perfectly aligned in
such a position that an imaginary vertical line
would pass through the center of the bonded
area and through the points of suspension (Fig.
I). The edge of the lap shall be 25.4 mm (1 in.)
from the edge of the grip. Apply the cyclic load
and check periodically. This load shall range
from a muimum io approximately IO R of the
maximum. The maximum load selected will
depend upon the strength of the adhesive in
shear tension loading and the desired life.
5.3 Test five specimens each at five or more
maximum loads which shall be selected such
that failures occur with regular spacing over a
range varying from at least IO 000 000 cycles
to not less than 2000 cycles. (As a guide, the
initial maximum !oad may be 50 70 of the
strength of the adhesive in shear by tension
loading.)
5.4 Record the number of cycles to failure
and the corresponding loads, calculated in
pounds-force per square inch (or megapascals).
Measure the specimen bond dimensions
accurately enough to calculate the area to the
nearest 0.6 mm (0.01 in.2). The location of
failure (adhesive or joint material), and nature
of failure if in the adhesive. (amounts of
cohesion, adhesion, or contact failures) should
be recorded for each specimen.
6. Report
6.1 The report shall include the following:
6.1.1 Complete identification of the materials,
procedures, and equipment (constant load
or constant displacement) used.
6.1.2 Dimensions of the bond area including
width and length +2.5 mm (0.01 in.) and
bonding thickness 10.0127 mm (0.0005 in.).
The method of obtaining the thickness of the
Annual Book of ASTM Siandards. Part 16.
322

D 3166
adhesive layer shall be described including
procedure, location of measurements and
range of measurements.
6. I .3 Temperature and relative humidity in
the test room.
6.1.4 Cycling rate in cycles per minute.
6.1.5 Number of cycles to failure and corresponding
loads calculated in pounds-force per
square inch or megapascals recorded on stresslog
cycle coordinates. The point at which the
curve intercepts the 10 million cycle coordinatt
shall be designated as the “fatigue strength a.
IO million cycles.”
6.1.6 Conditioning procedure used fo;
specimens prior to testing.
6.1.7 Number of specimens tested
6.1.8 Location and nature of failure (rela.
tive percentage of adhesive or adherend, ad.
hesion, or contact) for each specimen if ii
occurs before the fatigue test is completed.
NoTb-Minimum
specimen length in the grip 25.4 mm ( I in.).
FIG. 1.
323

Designation: D 3247 - 73
R84
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa., 19103
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Method of Test for
COEFFICIENT OF STATIC FRICTION OF
CORRUGATED AND SOLID FIBERBOARD
(HORIZONTAL PLANE METH0D)l
This Standard is issued under the fixed designation D 3247; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval.
1. Scope
1.1 This method covers the determination of
the coefficient of static friction of corrugated
and solid fiberboard or of the materials used to
make such board.
1.2 The horizontal instrument requires some
means of movement of the specimen in relation
to the surface upon which it rests. The coefficient
of friction is measured directly from the
resistance to that force and the applied weight.
1.3 An inclined plane method is described in
Method D3248. Either method gives essentially
equivalent results. The choice of approach
depends on the equipment available and the
means of measurement.
2. Applicable Documents
2.1 ASTM Standards:
D 585 Sampling and Accepting a Single Lot
of Paper, Paperboard, Fiberboard, or Related
Product2
D 685 Conditioning Paper and Paper Products
for Testing2
D 2534 Test for Coefficient of Kinetic
Friction for Wax Coatings3
D 3248 Test for Coefficient of Static Friction
of Corrugated and Solid Fiberboard (Inclined
Plane Method)2
2.2 Special Technical Publication:
STP 335 Manual for Conducting an Interlaboratory
Study of a Test Method4
3. Significance
3.1 The coefficient of friction of corrugated
and solid fiberboard indicates how containers
made from that board will perform in many
critical applications. A high coefficient of fric-
tion of one surface of board to itself means that
containers having that surface will tend to resist
sliding in unit loads. A low coefficient may
indicate potential problems with the containers
slipping from the load.
3.2 The coefficient of friction test is empirical.
It describes the condition of that surface at
the moment of test. This may or may not relate
to the condition of the surface in use. Nevertheless,
the test results are useful in determining
the properties of the surface tested. Its condition
will depend upon the historical treatment
of the surface. Because the previous history is
unknown, measurement is not made until the
third slide. Experience has shown that variability
is greatly reduced after the second slide.
4. Definitions
4.1 coefficient of friction-the ratio of the
frictional force resisting movement of the surface
being tested to the force applied normal to
that surface (the weight of the material above
that surface).
4.2 kinetic coefficient-the ratio of the force
resisting motion of the surface once the motion
is in progress.
NOTE 1-Kinetic coefficient is not determined in
this method (Appendix Xl).
4.3 static coefficient-the ratio of the force
resisting initial motion of the surface.
This method is under the jurisdiction of ASTM Committee
D-6 on Paper and Paper Products.
Current edition approved Sept. 27, 1973. Published October
1973.
'Annual Book of ASTM Standards, Part 15.
Annual Book of ASTM Standards, Part 18.
' Available from ASTM Headquarters, 1916 Race St.,
Philadelphia, Pa. 19103.
324

D 3247
5. Apparatus (Fig. 1)
5.1 Instrument Table-A horizontal. plane
surface of a smooth incompressible material
(metal, hard wood, plate glass, or plastic),
having a width at least 1 in. (25 mm) wider
than the test sled (5.2) with means of leveling it
in two directions. The base serves as a support
for the rest of the mechanism. When placed on
a solid support, the instrument must be free of
vibration.
5.2 Sled, or specimen block, having a bottom
area of at least 3 in.2 (20 cm2) smoothly
finished to exert a pressure of 0.50 f 0.25 psi
(3.44 1.72 kPa) on the horizontal surface.
A sled 2.5 by 2.5 in (62.5 by 62.5 mm) weighing
3 lb (1.36 kg) has been found to be satisfactory.
Means are provided for clamping the
specimen to the block, also for fastening the
sled to the force measuring device.
5.3 Mechanical Power Unit-Means for
moving the specimen block horizontally along
the instrument table or the horizontal table
under the specimen block at a speed of 6.0 f
1.0 in./min. (2.54 f 0.42 mm/s). This unit
must not transmit vibration to the instrument
table. The unit is connected to the sled or table
with some kind of inelastic linkage.
5.4 Measuring Device-Means for measuring
the force required to move or restrain the
specimen block to the nearest 0.01 lb (5 g).
6. Test Specimens
6.1 From each test unit of a sample obtained
in accordance with Method D 585, cut five
specimens (see 6.3 for size). Carefully mark
each specimen with its machine direction, on a
place that will not be the actual test area. For
corrugated board this will be perpendicular to
the direction of the flutes.
6.2 Cut and orient the specimens as follows:
6.2.! If the specimens are from a container.
carefully cut them from a flap area of the
container. It is usually desirable to test a flap
area since this is the area that normally comes
in contact with the next container in pallet
loads.
6.2.2 Paper is anisotropic and the coefficient
of friction is particularly so. Care must be
taken in making the test to orient the surfaces
to each other just as they will be oriented in
actual use. Therefore, if the layers of containers
are to be alternated in palletization, the coefficient
should be measured with one surface MD
(machine direction) and the other CD (crossmachine
direction).
6.2.3 If it is of interest to know how the
container will perform on packaging machinery
or be retained by conveyors, floors, shelves,
etc., measure the coefficient between a sample
of the paperboard and the material from which
the conveyor or floor or shelf is made.
6.2.4 If there is no known relationship to use
conditions, cut the test specimens so that the
measurements will be made with both parts
oriented in the CD direction.
6.3 Each specimen consists of two sheets.
Cut the smaller sheet, to fit the size of the sled
allowing for excess material if it is to be
clamped. It is suggested that the specimen be
scored with a suitable instrument and folded to
conform to the sled base. Cut the larger sheet at
least 1 in. (25 mm) larger in width than the test
surface of the sled, and sufficient in length to fit
the horizontal table, also allowing for material
to be clamped. For some instruments it may be
necessary to separate the outer facing of the
board from the medium and inner facing or
from the filler in order to clamp onto the sled or
block.
NOTE 2-Take care not ta touch the test area since
skin oils, pencil marks, etc. can affect the test results.
7. Conditioning
7.1 Precondition, condition and test the
specimens in an atmosphere in accordance with
Method D685.
7.2 With a clean cloth or tissue lightly wipe
the test surface to remove any loose fibers or
debris which may be present.
8. Procedure
8.1 Place the instrument upon a solid and
vibration-free base or table and level it.
8.2 If necessary, adjust the force gage to
zero.
8.3 Place the longer specimen on the table
top and clamp the end of the sheet farthest from
the measuring device in the sheet clamp.
8.4 Clamp the smaller sheet in place on the
sled. It is best to clamp one end of the specimen
and then draw the specimen uniformly
tight before clamping the remaining end.
325

D 3247
8.5 Place the sled with the specimen in position
on the other specimen and fasten the
cable on the block to the power unit, or to the
force gage.
8.6 Start the power unit, taking care to
maintain the cable(s) taut as the drive takes up
the load.
8.7 Continue the motion of the two specimens
in relation to each other until the entire
test area has been traversed.
8.8 Repeat 8.4 to 8.6 and record the force to
just begin the motion on the third slide.
8.9 Repeat the test on the other four specimens.
9. Calculations
9.1 Divide the force required to just hegin
motion of the block by the weight of the block.
This is the coefficient of static friction.
10. Report
10.1 The report shall include the following:
10.1.1 Average coefficient of s;atic friction
of the five specimens with the maximum and
minimum values for each combination of MD
and CD directions tested, and
10.1.2 If any side other than the top side of
the board was tested (see 8.3 and 8.4).
11. Precision
1 1.1 Repeatability-The repeatability is f
6.4% over the range exhibited by corrugated
linerboard.
1 1.2 Reproducibility-The reproducibility is
not known.
11.3 Comparabilit.v-The comparability is
not known; in accordance with the definitions
of these terms in STP 335.
Sled with specimen
Force Gage
/
A Specimens
Base
cantilever
(External Loading Optional)
Spring I // Specimens
Base
FIG. 1. Schematics for Two Horizontal Plane Instruments.
326

APPENDIX
X
RELATIOF TO KINETIC COEFFICIENT
XI ,I The kinetic coefficient is not measured in Not all surfaces, particularly those with some surface
this method. The static coefficient is usually of treatment such as wax, retain this relationship and
greater importance. For most corrugated and solid therefore if it is desirable to know the kinetic
fiberboard and their components the static and coefficient, it should be measured. Method D 2534
kinetic coefficients are usually related to each other describes how to measure the kinetic coefficient for
(that is, a surface with high static Coefficient will waxed coatings.
usually have a high (relatively) kinetic coefficient).
By publication of this standard no position is taken with respect to the validity of any patent rights in connection therewith,
and the American Society for Testing and Materials does not undertake to insure anyone utilizing the standard against liability
for infringement of any Letters Patent nor assume any such liability.
327

Designation: D 3248 - 73 ~ 8 4
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa., 19103
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Method of Test for
COEFFICIENT OF STATIC FRICTION OF
CORRUGATED AND SOLID FIBERBOARD
(INCLINED PLANE METHOD)'
This Standard is issued under the fixed designation D 3248, the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision A number In parentheses indicates the year of last
reapproval.
1. Scope
1.1 This method covers the determination of
the coefficient of static friction of corrugated
and solid fiberboard or of the materials used to
make such board.
1.2 The inclined plane is raised until sliding
begins. The coefficient of friction is equal to the
tangent of the angle at which sliding begins.
1.3 A horizontal plane method is described
in Method D 3247. Either method gives essentially
equivalent results. The choice of approach
depends on the equipment available and the
means of measurement.
2. Applicable Documents:
2.1 ASTM Standards:
D 585 Sampling and Accepting a Single Lot
of Paper, Paperboard, Fiberboard, or Related
Product2
D685 Conditioning Paper and Paper Products
for Testing*
D 2534 Test for Coefficient of Kinetic Friction
for Wax Coatings3
D 3247 Test for Coefficient of Static Friction
of Corrugated and Solid Fiberboard (Horizontal
Plane Method)2
2.2 Special Technical Publication:
STP 335 man^! fer CQX!CC~IQ 2:: !fiteilaboratory
Study of B Test Method'
3. Significance
3.1 The coefficient of friction of corrugated
and solid fiberboard indicates how containers
made from that board will perform in many
critical applications. A high coefficient of friction
of one surface of board to itself means that
containers having that surface will tend to resist
sliding in unit loads. A low coefficient may
indicate potential problems with the containers
slipping from the load.
3.2 The coefficient of friction test is empirical.
It describes the condition of that surface at
the moment of test. This may or may not relate
to the condition of the surface in use. Nevertheless,
the test results are useful in determining
the properties of the surface tested. Its condition
will depend upon the historical treatment
of the surface. Because the previous history is
unknown, measurement is not made until the
third slide. Experience has shown that variability
is greatly reduced after the second slide.
4. Definitions
4.1 coefficient of friction-the ratio of the
frictional force resisting movement of the surface
being tested to the force applied normal to
that surface (the weight of the material above
that surface).
4.2 kinetic coefficient-the ratio of the force
resisting motion of the surface once the motion
is in progress.
NOTE I-Kinetic coefficient is not determined in
this method (Appendix Xl).
4.3 static coefficient-the ratio of the force
resisting initial motion of the surface.
5. Apparatus (Fig. 1)
5.1 Sleds-A metal block, rectangular, with a
plane lower surface. A,means for clamping the
This method is under the jurisdiction of ASTM Committee
D-6 on Paper and Paper Products.
Current edition approved Sept. 27, 1973. Published October
1973.
*Annual Book of ASTM Standards, Part 15.
Annual Book of ASTM Standards, Part 18.
' Available from ASTM Headquarters, 1916 Race St.,
Philadelphia, Pa. 19103.
328

D 3248
specimen to the sled is desirable, but is not
necessary if the lower surface is faced with soft
rubber '43 in. (3 mm) thick. The size and weight
of the metal block are not critical, but a 2 by 4
in. (50 by 100 mm) block weighing 1.65 lb (750
g) giving 0.2 i 0.1 psi (1.38 f 0.69 kPa) when
horizontal has been found satisfactory.
5.2 inclined Plane-A plane surface, hinged
so that it can be tilted, with a smooth, incompressible
top surface which may be made of
metal, hard wood, plate glass or plastic having
a width at least 1 in. (25 mm) wider than the
sled and a length sufficient to permit the sled to
move at least 5/i3 in. (15 mm). The plane is
provided with a clamp ai the upper end to fix
the test specimen to the plane.
NOTE 2-When the plane is horiLonta1, means are
provided to level the instrument in two directions.
5.3 Means to indicate the angular displacement
of the plane to within 0.5 deg.
5.4 Means to smoothly increase the inclination
of the plane from the horizontal through an
arc of at least 45 deg at a rate of 1.5 f 0.5
deg/s.
6. Test Specimens
6.1 From each test unit of a sample obtained
in accordance with Method D 585, cut five
specimens (see 6.3 for size). Carefully mark
each specimen with its machine direction, on a
place that will not be the actual test area. For
corrugated board this will be perpendicular to
the direction of the flutes.
6.2 Cut and orient the specimens as follows:
6.2.1 If the specimens are from a container,
carefully cut them from a flap area of the
container. It is desirable to test a flap area since
this is the area that normally comes in contact
with the next container in pallet loads.
6.2.2 Paper is anisotropic and the coefficient
of friction is pariicuiariy so. Take care in
making the test to orient the surfaces to each
other just as they will be oriented in actual use.
Therefore, if the layers of containers are to be
alternated in palletization, measure the coefficient
with one surface MD (machine direction)
and the other CD (cross-machine direction).
6.2.3 If it is of interest to know how the
container will perform on packaging machinery
or be retained by conveyors, floors, shelves,
etc., measure the coefficient between a sample
of the paperboard and the material from which
the conveyor or floor or shelf is made.
6.2.4 If there is no known relationship to use
conditions, cut lhe test specimens so that the
measurements will be made with both parts
oriented in the CD direction.
6.3 Each specimen consists of two sheets.
Cut the smaller sheet to fit the size of the sled
allowing for excess material if it is to be
clamped. It is suggested that the specimen be
scored with a suitable instrument and folded to
conform to the sled base. Cut the larger shepVt at
least 1 in. (25 mm) larger in width than the test
surface of the sled, and sufficient in length for
the sled to move 0.6 in. (15 mm), also allowing
for material to be clamped. For some instruments
it may be necessary to separate the outer
facing of the board from the medium and inner
facing or from the filler in order to clamp onto
the sled.
NOTE 3-Take care not to touch the test area since
skin oils, pencil marks, etc. can affect the test
results.
7. Conditioning
7.1 Precondition, condition, and test the
specimens in an atmosphere in accordance with
Method D685.
7.2 With a clean cloth or tissue lightly wipe
the test surface to remove any loose fibers or
debris that may be present.
8. Procedure
8.1 Level the plane so that it is horizontal
when the inclinometer indicates zero.
8.2 Mount the larger sheet on the plane with
the surface to be tested upward. Clip the other
specimen to the sled and position it on top of
the lower specimen with the surface to be tested
facing downward. Unless an unusual orientation
is used in making the container, this will be
the top side of the board as made on the paper
.-- I -L:--
IIIdLlIIIIC.
8.3 Incline the plane at the specified rate.
When the sled starts to move, stop the inclinator
immediately and allow the sled to slide to
the stop. Carefully lift the sled and attached
specimen and place the assembly in its original
starting position with the plane in its horizontal
position. Repeat this for a total of three slides
and read the angular displacement at the moment
the sled starts to move on its third side.
NC~F +-It has been shown that after two slides
on a giwn surface, friction measurements are then
329

D 3248
essentially constant for repeated slides. Since the
previous history of the specimen is not known, two
preliminary slides wili bring the surface to that more
uniform level.
8.4 Repeat 8.1 to 8.3 on the other four
specimens.
9. Calculations
9.1 Calculate the tangent of the angle at
which sliding begins on the third slide. This is
the coefficient of static friction.
10. Report
10.1 The report shall include the following:
10.1.1 Average coefficient of static friction
of the five specimens with the maximum and
minimum values for each combinaiion of PAD
and CD directions tested, and
10.1.2 If any side other than t3e top side of
the board was tested (see 8.2).
11. Precision
11.1 Repeatability-The repeatability is
~0.026 (tangent of 1.5 deg). This is 5.6 to 8.1 %
of the average in the range of values usually
obtained for corrugated board.
11.2 Reproducibility-The reproducibility is
not known.
11.3 Comparability-The comparability is
not known, in accordance with the definitions
of these terms in STP 335.
Sled with specimen
FIG. 1 Schematic of Inclint Inclined Plane Apparatus.
APPENDIX
XI. RELATION TO KINETIC COEFFICIENT
X1.1 The kinetic coefficient is not measured in
this method. In the inclined plane method, the kinetic
coefficient is not as easily determined to the same
precision as the static coefficient. The static coefficient
is usually of greater importance. For most
corrugated and solid fiberboard and their components,
the static and kinetic coefficients are usually
related to each other (that is, a surface with high
static coefficient will usually have a high (relatively)
kinetic coefficient). Not all surfaces, particularly
those with some surface treatment such as wax, retain
this relationship and therefore if it is desirable
to know the kinetic coefficient, it should be measured.
Method D 2534 describes how to measure
the kinetic coefficient for waxed coatings.
X 1.2 Testing Corrugated and Solid Fiber
Containers-With most instruments it is not possible
to test actual containers unless they are unusually
small; however, some inclined plane instruments are
large enough to test whole containers. With such
equipment, perform the test as follows:
XI .2.1 The instrument characteristics should conform
to those stated above for the inclined plane
instrument.
330

X1.2.2 Clamp one board specimen (top of one
box) to the inclined plane; or if friction is to be
measured against another surface, such as metal or a
conveyor belt, clamp that material to the inclined
plane.
X 1.2.3 Place a container on top of the test surface.
Orientation should correspond to the orientation of
the two surfaces in actual use.
X1.2.4 Raise the inclined plane until sliding just
begins. Repeat for three slides.
X1.2.5 On the third slide, record the angle for
which sliding just begins on the third slide.
X 1.2.6 Report the coefficient of static friction,
which is the tangent of that angle.
By publication of ihis standard no position is iaken with respect to the validiiy of any patent rights in connection therewith,
and the American Society for Testing and Materials does not undertake to insure anyone utilizing the standard against liability
for infringement of any Letters Patent nor assume any such liability.

lsTr,
Designation: D3334 - 80
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Methods of Testing
FABRICS WOVEN FROM POLYOLEFIN
MONOFILAMENTSl
This standard is issued under the fixed designation D 3334. the number immediately following the designation indicates the
year of original adoption. or in the case of revision. the year of last revision A number in parentheses indicates the year of last
reapproval
I. Scope
1.1 These methods cover the characterization
of fabrics woven from polyolefin monofilaments.
1.2 The methods appear as follows:
Title
Applicable Documents
Coefficient of Static Friction
Conditioning
De fin i t ions
Fabric Count
Fabric Weight
Gloss
Heat Shrinkage
Resistance to Ultraviolet Radiation
Sampling and Number of Test Specimens
Stability to Thermal Oxidation
Summary of Methods
Tensile Properties
Uses and Significance
Section
2
15
7
3
8
9
14
I I
13
6
I2
4
10
5
NOTE I-For methods of testing and specifications
for polyolefin monofilaments, refer to Specification
D 3218, for Polyolefin Monofilaments.*
2. Applicable Documents
2.1 ASTM Standards:
D 76 Specification for Tensile Testing Machines
for Textiles3
D 123 Definitions of Terms Relating to
Textiles3
D 1248 Specification for Polyethylene Plastics
Molding and Extrusion Materials4
D 1682 Tests for Breaking Load and Elongation
of Textile Fabrics'
D 1776 Practice for Conditioning Textiles
and Textile Product for Testing"
D 1910 Test for Construction Characteristics
of Woven Fabrics2
D 2146 Specification for Polypropylene Plas-
tic Molding and Extrusion Materials4
D 2565 Recommended Practice for Operating
Xenon-Arc Type ( Water-Cooled)
Light- and Water-Exposure Apparatus for
Exposure of Plastics5
G 23 Recommended Practice for Operating
Light- and Water-Exposure Apparatus
(Carbon-Arc Type) for Exposure of Nonmetallic
Materials6
2.2 Other Documents:
Federal Test Method Standard No. 141a,
Sept. I, 1965, Section 6000, Method 6101,
60 Degree Specular Gloss7
TAPPI Test Method T 503, Coefficient of
Static Friction of Shipping Sack Papers
(Inclined-Plane Method)"
3. Definitions
3.1 breaking load, n.-the maximum force
applied to a specimen in a tensile test carried to
rupture.
3.1.1 Force is commonly expressed in
grams-force (gf), kilograms-force (kgf),
pounds-force (lbf), newtons (N), or millinewtons
(mN).
.__
'These methods are under the jurisdiction of ASTM
Committee D-! 3 on Tex!i!es. a d are !he d:rec: :espen:ibi!i:y
of Subcommittee D13.59 on Fabric Test Methods. General.
Current edition approved March 3. 1980. Published May
1980. Originally published as D 3334 - 74 T. Last previous
edition D 3334 - 74 T.
Annual Book of ASTM Standards, Part 32.
3Annual Book ofASTM Standards, Parts 32 and 33.
4Annual Book of ASTM Standards, Part 36.
Annual Book ofASTM Standards. Part 35.
Annual Book ofASTM Standards. Part 4 I .
' Available from the Superintendent of Documents, U. S.
Government Printing Office, Washington. D.C. 20402.
' Available from the Technical Association of Pulp and
Paper Industry, One Dunwoody Park, Atlanta, Cia. 30341.
332

D 3334
3.2 elongation at the breaking load, n.-the
elongation corresponding to the maximum
load.
3.2.1 Elongation is expressed as a percentage
of the length of the original specimen.
3.3 gloss (specular gloss), n.-the luminous
fractional reflectance of a fabric specimen in
the specular direction.
3.4 heat shrinkage, n.-the change in dimension
of a fabric specimen exposed to heat.
3.4.1 Negative shrinkage is designated as
growth.
3.5 polyolefin fabric, n.-a fabric woven
from polyolefin monofilaments. Polyethylene
(PE) fabrics have a composition conforming to
Specification D 1248. Polypropylene (PP) fabrics
have a composition conforming with Specification
D 2 146.
3.5.1 A common type of polyolefin fabric is
woven from 2 by 100-mil monofilaments.
3.6 resistance to ultraviolet radiation polyolefin
fabric), n.-the average retained
strength of a fabric, exposed to ultraviolet
radiation for a specified length of time, under
specified conditions.
3.7 stability to thermal oxidation (polyolefin
fabric), n.-that property of a fabric which
resists breaking under a specified tensile strain,
when exposed to a current of air at an elevated
temperature.
3.7.1 The stability of polyolefin fabric to
thermal oxidation is measured in time-to-failure,
in days, at 125°C.
3.8 For definitions of other textile terms
used in these methods, refer to Definitions
D 123.
4. Summary of Methods
4.1 Summaries of the various testing procedures
are included in the referenced test
methods, or in pertinent sections herein.
5. Uses and Significance
5.1 Only on the condition that interlaboratory
precision data are available for the specific
procedure, is any method described or referenced
in this standard recommended for acceptance
testing of commercial shipments.
5.2 No justifiable statement on the accuracy
of the methods included in this standard, can be
made since the true value of the properties
cannot be determined by accepted reference
met hods.
6. Sampling and Number of Specimens
6.1 Take samples as directed in an applicable
specification or as agreed upon between the
purchaser and the seller.
6.2 The desired number of specimens is
covered in the referenced methods, or in pertinent
sections herein.
7. Conditioning
7.1 Expose the specimens in the standard
atmosphere for testing textiles, as directed in
Recommended Practice D 1776, for a minimum
of 1 h.
8. Fabric Count
8. I Procedure:
8.1.1 Take the specimens no closer to a
selvage than one tenth of the width of the
fabric.
8.1.2 Count the yarns in both the warp and
the filling directions, over a 3-in. (75")
length or width, as directed in Sections 30 and
32 of Methods D 1910.
8.1.3 Repeat the count on five different areas
of each specimen. Average the five counts for
each direction.
8.2 Report:
8.2.1 State that the specimens were tested as
directed in Section 8 of ASTM Methods
D 3334, and Sections 30 to 32 of Methods
D 1910. Describe the material or product sampled,
and the method of sampling used.
8.2.2 Report the average warp count, and
the average filling count, to the nearest yarn
unit.
8.3 Precision and Accuracy:
8.3.1 Precision-No changes in procedure
have been made which affect the precision of
the method for fabric count, as specified in
Secticns 30 to 32 nf Method D 1910.
8.3.2 Accuracy-This method for testing
fabric count has no known bias, and is generally
used as a referee method.
9. Fabric Weight
9.1 Procedure-Determine the weight (Note
2) of the fabric, as directed in Section 38 of
Methods D 1910.
NOTE 2-The term "weight" is used in this standard
because of established trade usage. in place of
the technically correct term "mass."
333

9.2 Report:
9.2. I State that the specimens were tested as
directed in Section 9 of ASTM Methods
D 3334 and Section 38 of Methods D 1910.
Describe the material or product sampled, and
the method of sampling used.
9.2.2 Report the weight per square yard
(or square metre) to three significant figures.
State that the weight as reported does not
include the selvage.
9.3 Precision and Accuracy:
9.3. I Precision-No changes in procedure
have been made that affect the precision of the
method for fabric weight, as specified in Section
38 of Methods D 1910.
9.3.2 Accuracy-This method for testing
fabric weight has no likely bias, and is generally
used as a referee method.
10. Tensile Properties ( Breaking Load and
Elongation at the Breaking Load)
10. I Apparatus-Tensile Testing Machine.
of a type conforming to Specification D 76.
I 0.2 Procedure- Determine the breaking
load and elongation as directed in Section 15
(Grab Test) of Methods D 1682.
NOTL 3-The I by 2-in. (25 by 50-mm) jaw faces
are preferable. because the larger gripping area tends
to reduce slippage.
10.2.1 Test five specimens, each 4 by 8 in.
(100 by 200 mm), with the long dimension
parallel to the direction, for which the breaking
load is to be determined.
10.3 Report:
10.3.1 State that the specimens were tested,
as directed in Section IO of ASTM Methods
D 3334. Describe the material or product sampled,
and the method of sampling used.
10.3.2 Report the following information:
10.3.2.1 Average breaking load in each direction,
for all specimens giving acceptable
breaks,
10.3.2.2 Average percent apparent elongation
in each direction, for all specimens giving
acceptable breaks,
10.3.2.3 Type of testing machine used, and
10.3.2.4 Average time required to break all
specimens giving accept able breaks.
10.4 Precision and Accuracy:
10.4.1 Precision-No changes in procedure
have been made that affect the precision of the
D 3334
methods for tensile properties, as specified in
Section 15 of Methods D 1682.
10.4.2 Accurac.v-This method for testing
tensile properties of fabrics has no known bias,
and is generally used as a referee method.
11. Heat Shrinkage
11. I Scope-This method covers the determination
of the dimensional change of woven
polyolefin fabrics, after exposure to air at an
elevated temperature.
I I .2 Apparatus:
I I .2. I Oven,!' mechanical-convection type,
for controlled circulation of air; with adjustable
air intake and exhaust facilities. and designed
for air velocities up to I m/s. The oven shall be
equipped with a temperature-control system
designed to maintain the oven temperatures at
the levels specified in 11.4, with a precision of
+I"C. A device to prevent temperature
overrides"' shall be included in the temperature-control
system.
I 1.2.2 Thermometer, with the temperature
range from 0 to 150°C, and graduated at
intervals of 1 deg.
11.2.3 Marking Pen, such as a felt-tip
marker, or any other device that will produce a
suitable mark.
11.2.4 Rule, or other measuring device,
graduated in 0.025411. (I-mm) units.
I 1.3 Test Specimens:
11.3.1 Take three specimens each at least
12-in. (300-mm) square. Lay out a specimen
fully extended, but not stretched, on a flat,
horizontal surface. Place a mark about I in. (25
mm) from the edge. Measure IO in. (250 mm)
along one principal direction of the specimen,
and place a second mark. Place similar pairs of
marks on the specimen in the other principal
direction. Prepare the other two specimens in
the ~aiiie Xai;nei.
1 I .3.2 Measure the distance between each
pair of marks on each specimen to the nearest
0.025 in. (I mm). Record the three measure-
" Freas Model 835. Precision Scientific Co., 3737 W.
Cortland St.. Chicago. 111. 60647; or Blue M. Model
POM-136 C. Blue M Electric Co., 138th and Chatham Sts,
Blue Island, 111 60406; or any other equivalent oven, have
been found satisfactory for this method.
'I' A bimetallic-strip temperature switch. Fenwal Inc.. 261
Main St., Ashland, Me. 01721; or any other equivalent
device has been found satisfactory for this method.
-
334

D 3334
ments along each principal direction. Calculate
the two averages.
11.3.3 When a more accurate method is
needed, make cuts in the fabric specimen,
instead of using marks. This will provide a
more precise bench mark for the alignment of
the measuring device. Marks usually tend to be
wavy on woven Fabrics, thus introducing
sources of imprecision into the measurements.
I 1.4 Procedure:
11.4.1 Maintain the temperature at 125 =t
IOC, for testing fabrics made from polypropylene
materials and at 100 & I"C, for
testing fabrics made from polyethylene materials.
Monitor the temperature by placing the
thermometer bulb 75 to 80 mm from the top
liner of the oven, in the vicinity of the exhaust
port.
11.4.2 Maintain nominal air velocity at 0.5
f 0.1 m/s during the test. Adjust the air intake
and exhaust ports to allow at least one volume
change per hour.
11.4.3 When the oven has been at the specified
test conditions for at least 30 min, place the
fabric specimens on the perforated shelf, and
leave them in the oven for 20 + 2 min.
1 I .4.4 Remove the specimens from the oven,
and condition them for 1 h in the standard
atmosphere for testing textiles (see 7.1). Remeasure
each sei of specimens. Record the
results, and calculate the average for each
principal direction.
I I .4.5 Calculate the percentage change in
dimension for each direction of the specimen to
the nearest 0. I ?k using Eq 1:
Dimensional change, % = [(A - B) IOO]/A (1)
where:
A = average length, before heat agings, and
B = average length, after heat aging.
I 1.5 Report:
11.5.1 State that the specimens were tested
as directed in Section I I of ASTM Methods
D 3334. Describe the material or product sampled,
and the method of sampling used.
1 I .5.2 Report the average percent change in
length, for each principal direction, to the
nearest 0.1 %, and indicate whether it was
shrinkage or growth.
1 1.6 Precision and Accuracy:
1 1.6.1 Precision-The precision of this
method for heat shrinkage of fabrics has not
been established.
I I .6.2 Accurac-v-See 5.2.
12. Stability to Thermal Oxidation
12.1 Summary of Method-Specimens of
polyolefin fabrics are exposed to a current of
air, in a mechanical-convection oven at an
elevated temperature until mechanical failure
occurs.
12.2 Uses and Significance-Under the severe
conditions of this accelerated-aging test,
the specimens undergo degradation at a rate
that is dependent upon the thermal endurance
of the polyolefin materials. The time-to-failure
by this test is a common criterion for assessing
the stability to thermal oxidation of polyolefin
fabrics.
12.3 Apparatus:
12.3. I Oven, as described in I I .2. I .
12.3.2 Thermometer, as described in 1 I .2.2.
12.3.3 Air Meter,'' designed for the measurement
of linear velocities in the range from 0
to 1 m/s.
12.3.4 Glass Rod, approximately 250 mm
long, with a diameter of about 12 mm.
12.3.5 Weights, 5-g, in the form of leaded
No. 2 small paper clips.
12.3.6 Polytetrajluoroethylene Film.
12.4 Test Specimens:
12.4.1 Cut five strips of polyolefin fabric, I
by IO in. (25 by 250 mm), with the longer
dimension in the warp or filling direction,
whichever is to be tested.
12.4.2 Attach a weight to each end of a
specimen, and form a loop from the specimen.
Avoid direct contact of metal with the specimen
by using polytetrafluoroethylene film as parting
element. Attach weights to the other four
specimens in a similar manner. Insert the glass
rod through the loop of each specimen. The
specimen assemblage is now ready for mounting.
12.5 Procedure:
12.5.1 Maintain the temperature in the oven
at 125 =t I'C, during the thermal aging test.
Monitor this temperature, by locating the ther-
I' hnemotherm Model 60, Anemostat Product Div., Dynamic
Corporation of America. P.O. Box 1083. Scranton.
Pa. 18500. or its equivalent. has been found satisfactory for
this method.
335

D 3334
mometer bulb 2 in. (50 mm) from the top liner
of the oven. in the vicinity of the exhaust port.
12.5.2 Maintain the air velocity at 0.5 f 0. I
m/s, inside the oven. Adjust the air intake and
exhaust ports to allow at least one air-volume
change per hour.
12.5.3 Suspend the specimen assemblage
from the upper shelf of the oven.
12.5.4 Inspect the specimens daily for failure,
as evidenced by the material breakdown
which causes the two parts of the specimen, and
their attached weights, to fall onto the bottom
shelf of the oven.
12.5.5 Record the time-to-failure of eiich
specimen, and calculate the average time-tofailure,
in days, for the five specimens.
12.6 Report:
12.6.1 State that the specimens were tested
as directed in Section 12 of ASTM Methods
D 3334. Describe the material or product Sampled,
and the method of sampling used.
12.6.2 Report the average time-to-failure, in
days, as stability to thermal oxidation, and
indicate the direction in which the fabric was
tested (warp or filling).
12.7 Precision and Accuracy:
12.7. I Precision-The precision of this
method for stability to thermal oxidation has
not been established.
1 2.7.2 Accurac v-See 5.2.
13. Resistance to Ultraviolet Radiation
13. I Summary of' Method-Specimens are
exposed to an artificial light source simulating
natural sunshine. The test conditions of temperature
and humidity approximate those encountered
in outdoor exposure in subtropical regions.
The breaking load is determined on
fabric specimens, as directed in Section 10, and
after the specified exposure time agreed upon
between the purchaser and the seller.
13.2 Uses and Signifi:cance-Data obtained
by this method are expected to correlate reasonably
well with data from outdoor exposure.
The previous statement is particularly applicable
to Procedure B of Recommended Practice
D 2565. For many applications of polyolefin
fabrics, a total exposure of 100 h is adequate,
but longer exposure periods may be required.
13.3 Apparatus-The apparatus shall be as
specified in Recommended Practices D 2565
and G 23.
13.4 Test Specinlens-Mount a 4- by &in.
(100 by 200-mm) specimen in the frame-type
specimen holder, an accessory supplied with
each exposure apparatus. Place the long dimension
of the specimen holder parallel to the
principal direction of the specimen to be tested
(warp or filling). Prepare three mounted specimens.
I 3.5 Procedure:
13.5. I Expose three mounted specimens, for
each test direction, to xenon-arc weathering, in
accordance with Procedure A of Recommended
Practice D2565. In case of dispute use Procedure
B.
13.5.2 Alternatively, if agreed to between the
purchaser and the seller or if there is some other
bilateral agreement, expose the mounted specimen
to sunshine-carbon-arc weathering, as directed
in Recommended Practice G 23.
13.5.3 At the end of the exposure period,
remove the mounted specimen from the apparatus
and determine the breaking load, as
directed in Section 10. Record the results and
calculate the average breaking load for each
principal direction of the specimens tested.
I 3.6 Cafcufations- Determ ine the percentage
retention of the original breaking load
using Eq 2:
Retained strength, '70 = (E x iOO)/U (2)
where:
E = average breaking load of exposed specimen,
Ibf (N), and
U = breaking load of unexposed specimen, Ibf
(N).
13.7 Report:
13.7.1 State that the specimens were tested
as directed in Section 13 of ASTM Methods
D 3334. Describe the material or product sampled,
and the method of sampling used.
13.7.2 Report the following information:
13.7.2. I Average retained strength, in percent,
for both the warp and filling directions,
and
13.7.2.2 Exposure period, and type of exposure.
13.8 Precision and Accuracv:
13.8.1 Precision-The precision of thl
method for resistance to ultraviolet radiatio
336

D 3334
has not been established.
13.8.2 Accuracy-See 5.2.
14. Gloss
14. I Summary of Merhod-Gloss is determined
on fabric specimens with a glossmeter,
which measures the fractional reflectance of the
specimen with the axis of the incident beam 60
deg from a plane perpendicular to the test
surface. Basically, the method is derived from
Federal Test Method Standard No. 141a,
Method 6101.
14.2 Uses and Signficance-Gloss is undesirable
in many applications of polyolefin
fabrics. This method is used to provide a
measure of this characteristic.
14.3 Apparatus:
14.3.1 Glossmeter," graduated in 0. I-gloss
units.
14.3.2 Polished Glass, Standard of Reflectance,
supplied with the glossmeter.
14.4 Test Specimens-Cut three specimens,
approximately IO by IO in. (250 by 250 mm),
across the width of the fabric. Take the specimens
no closer to the selvage than one tenth of
the width of the fabric.
14.5 Standardi=ation-Using polished gloss
standards, standardize the glossmeter in accordance
with the instructions supplied with the
unit.
14.6 Procedure:
14.6.1 Stack the three specimens on top of
each other and place them on a dull surface.
14.6.2 Place the rectangular head of the
glossmeter parallel with the warp direction of
the fabric, and take three measurements, moving
the unit to another area of the specimen
before taking each successive measurement.
Place the glossmeter parallel with the filling
direction, and take three readings in a similar
manner. E-ecord each reading to two significant
figures.
14.6.3 Place the top specimen at the bottom
of the stack and test the second specimen as
directed in 14.6.2. ?lace the top specimen at the
bottom of the stack and test the third specimen
as directed in 14.6.2.
14.6.4 Calculate the average of the 18 gloss
readings.
14.7 Report:
14.7.1 State that the specimens were tested
as directed in Section 14 of ASTM Methods
D 3334. Describe the material or product sampled,
and the method of sampling used.
14.7.2 Report the average gloss reading to
two significant figures.
14.8 Precision and Accuracy:
14.8. I Precision-The precision of this
method for gloss has not been established.
14.8.2 Accuracy-See 5.2.
15. Coefficient of Static Friction
15.1 Surnmarjs of Method-The coefficient
of static friction is determined on woven polyolefin
fabric. using an inclined-plane method.
One specimen is attached to a plane, which can
be raised at one end, and another specimen is
attached to *a test sled. The fabric-covered sled
is placed crosswise on the fabric-covered plane,
and the plane inclined until sliding occurs. The
tangent of the angle is reported as an index of
the static friction. This method is derived from
TAPPI Method T 503.
15.2 Uses and Significance-An excessively
high or low coefficient of friction may be
detrimental to many products in which polyolefin
fabrics are used. This method provides a
measure of the coefficient of static friction of
one fabric on another.
15.3 Apparatus:
15.3.1 Timer, or stop watch graduated in
seconds .
15.3.2 Inclined Plane, having a smooth, incompressible
top surface, with a width at least 1
in. (25 mm) wider than the test sled, and a
sufficient length to permit the sled to move by
gravity at least 0.5 in. (12 mm). It must be
provided with clamps for the test specimen, and
an inclinometer to indicate the angular displacement
of the plane, within 0.5 deg. The
device must be designed so that the inclination
of the plane from the horizontal can be increased
smoothly through an arc of at least 45
deg at a rate of 1.5 * 0.5 deg/s.
15.3.3 Test Sled, a metal block, preferably
rectangular. with a flat lower surface 3.5 by 4
in. (90 by 100 mm), with a weight to provide a
pressure of 0.2 psi (I .4 kPa), when horizontal.
15.4 Specimen Preparation-Cut three specimens,
5 by IO in. (125 bj 250 mm). across the
fabric, with no specimen cut closer to the
'' Gardner automatic photometer unit. Model AUX-3. or
its equivalent. has been found satisfactory for this method.
337

~
~
selvage than one tenth of the width of the
fabric. Cut each of the three specimens into two
5-in. ( 125”) squares.
I 5.5 Procedure:
15.5. I Level the plane, so that it is horizontal
when the inclinometer reads zero.
15.5.2 Clamp one half of one specimen to
the plane, with the warp direction parallel to the
direction of slide, and the surface to be tested
facing upward. The fabric should be flat with no
creases or wrinkles.
15.5.3 Clamp or tape the other half of the
specimen to the bottom of the test sled, with the
filling parallel to the long dimension and the
surface to be tested facing downward. The
fabric should be flat with no creases or wrinkles.
15.5.4 Place the test sled on the plane with
the long dimension parallel to the direction of
slide. The two surfaces of the specimen should
now be in contact, with their warp direction at
right angles. Allow a dwell time of 30 f 3 s,
then incline the plane at a rate of 1.5 =t 0.5
deg/s. Stop the plane when the test sled starts
to move. Repeat this procedure twice and read
the inclinometer to the nearest 0.5 deg. Record
the angle at which the test sled begins to slide
on the third trial.
15.5.5 Repeat 15.5.4 with each of the specimens.
Calculate the average angle required to
produce movement of the test sled. Determine
the trigonometric tangent of the average angle.
15.6 Report:
15.6. I State that the specimens were tested
as directed in Section 15 of ASTM Methods
D 3334. Describe the material or product sampled,
and the method of sampling used.
15.6.2 Report the trigonometric tangent of
the average angle as the coefficient of static
friction.
15.7 Precision and Accuracy:
15.7.1 Precision-The precision of the
method for static friction has not been established.
15.7.2 Accuracy-See 5.2.
The American Society for Testing and Materials takes no position respecting the validit!, of any patent rights asseried in
connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the
validity of any such patent rights, and the risk of infringement of such rights, is entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every jive
years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or
for additional standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration
at a meeting of the responsible technical committee, which you may attend. If you feel that your comments have not received
a fair hearing you should make your views known to the ASTM Committee on Standards, I916 Race St.. Philadelphia, Pa.
19103, which will schedule a further hearing regarding your comments. Failing satisfaction there. you may appeal to the
ASTM Board of Directors.
338

eb
Designation: D 3359 - 87
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Methods for
MEASURING ADHESION BY TAPE TEST'
This standard is issued under the fixed designation D 3359: the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
Thew methods haw been approvedfor use b.v agencies qfthe Department of Definse and. for listing in the DoD 1ndiB.v qf Specifications
and Standard.9.
1. scope
1.1 These test methods cover procedures for
assessing the adhesion of coating films to metallic
substrates by applying and removing pressuresensitive
tape over cuts made in the film.
1.2 Method A is primarily intended for use at
job sites while Method B is more suitable for use
in the laboratory. Also, Method B is not considered
suitable for films thicker than 5 mils (125
CLm).
NOTE I-Subject to agreement between the purchaser
and the seller. Method €3 can be used for thicker
films if wider spaced cuts are employed.
1.3 These test methods are used to establish
whether the adhesion of a coating to a substrate
is at a generally adequate level. They do not
distinguish between higher levels of adhesion for
which more sophisticated methods of measurement
are required.
NOTE 2-It should be recognized that differences in
adherability of the coating surface can affect the results
obtained with coatings having the same inherent adhesion.
1.4 In multicoat systems adhesion failure may
occur between coats so that the adhesion of the
coating system to the substrate is not determined.
1.5 This standard may involve hazardous materials;
operations: and equipment. This standard
does not purport to address all of the safeiyproblems
associated with its use. It is the responsibility
of the user ofthis standard to establish appropriate
safety and health practices and determine
the applicability oj'regulatory limitations prior to
use.
2. Referenced Documents
2.1 ASTM Stavrdards:
D609 Methods for Preparation of Steel Panels
for Testing Paint, Varnish, Lacquer, and
Related Products'
D823 Methods of Producing Films of Uniform
Thickness of Paint, Varnish, and Related
Products on Test Panels'
D 1730 Practices for Preparation of Aluminum
and Aluminum-Alloy Surfaces for Painting'
D2092 Practices for Preparation of Zinc-
Coated Galvanized Steel Surfaces for Paint'
D 3330 Test Method for Peel Adhesion of Pressure-Sensitive
Tape of 180" Angle3
3. Summary of Test Methods
3.1 Test Method A-An X-cut is made in the
film to the substrate, pressure-sensitive tape is
applied over the cut and then removed, and
adhesion is assessed qualitatively on the 0 to 5
scale.
3.2 T~SI Method B-A lattice pattern with
either six or eleven cuts in each direction is made
in the film to the substrate, pressure-sensitive
tape is applied over the lattice and then removed,
and adhesion is evaluated by comparison with
descriptions and illustrations.
TEST METHOD A-X-CUT
4. Apparatus and Materials
TAPE TEST
4. I Cutting Tool-Sharp razor blade, scalpel,
knife or other cutting devices. It is of particular
importance that the cutting edges be in good
condition.
4.2 Cutting Guide-Steel or other hard metal
straightedge to ensure straight cuts.
' These test methods are under the jurisdiction of ASTM
Committee DI on Paint and Related Coatings and Materials
and are the direct responsibility of Subcommittee DO1.23 on
Physical Properties of Applied Paint Films.
Current edition approved May 29, 1987. Published September
1987. Originally published as D 3359 - 74. Last previous
edition D 3359 - 83.
Annual Book ofASTM Standardr. Vol06.01.
'Annual Book of ASTM Standardr, Vol 15.09.
339

0 3359
4.3 Tape-One-inch (25") wide semitransparent
pressure-sensitive tape with an adhesion
strength of 38 f 5 oz/in. (43 f 5.6 g/mm or N/
100 mm) width when tested in accordance with
Test Method D 3330. The adhesion shall not
change by more than f: 6.5 % of its mean value
within 12 months. The backing of the tape may
consist of fiber-reinforced cellulose acetate? unplasticized
poly(viny1 chloride), or polyester film.
Tape with different properties may be used subject
to agreement between the purchaser and the
seller. When results obtained in different laboratories
do not agree, it is recommended that the
test be repeated using tape from the same batch.
4.4 Rubber Eraser, on the end of a pencil.
4.5 Illumination-A light source is helpful in
determining whether the cuts have been made
through the film to the substrate.
5. Test Specimens
5. I When this test method is used in the field,
the specimen is the coated structure or article on
which the adhesion is to be evaluated.
5.2 For laboratory use apply the materials to
be tested to panels of the composition and surface
conditions on which it is desired to determine
the adhesion.
NOTE 3-Applicable test panel description and surface
preparation methods are given in Methods D 609
and Practices D I730 and D 2092.
NOTE 4-Coatings should be applied in accordance
with Methods D823. or as agreed upon between the
purchaser and the seller.
NOTE 5-If desired or specified, the coated test
panels may be subjected to a preliminary exposure such
as water immersion, salt spray, or high humidity before
conducting the tape test. The conditions and time of
exposure will be governed by ultimate coating use or
shall be agreed upon between the purchaser and seller.
6. Procedure
6.1 Select an area free of blemishes and minor
surface imperfections. For tests in the field, ensure
that the surface is clean and dry. Extremes
in temperature or relative humidity may affect
the adhesion of the tape or the coating.
6.2 Make two cuts in the film each about 1.5
in. (40 mm) long that intersect near their middle
with a smaller angle of between 30 and 45'. When
making the incisions, use the straightedge and
cut through the coating to the substrate in one
steady motion.
6.3 Inspect the incisions for reflection of light
from the metal substrate to establish that the
coating film has been penetrated. If the substrate
has not been reached make another X in a different
location. Do not attempt to deepen a
previous cut as this may affect adhesion along
the incision.
6.4 Remove two complete laps of the pressure-sensitive
tape from the roll and discard.
Remove an additional length at a steady (that is,
not jerked) rate and cut a piece about 3 in. (75
mm) long.
6.5 Place the center of the tape at the intersection
of the cuts with the tape running in the same
direction as the smaller angles. Smooth the tape
into place by finger in the area of the incisions
and then rub firmly with the eraser on the end
of a pencil. The color under the transparent tape
is a useful indication of when good contact has
been made.
6.6 Within 90 f: 30 s of application, remove
the tape by seizing the free end and pulling it off
rapidly (not jerked) back upon itself at as close
to an angle of 180' as possible.
6.7 Inspect the X-cut area for removal ofcoating
from the substrate or previous coating and
rate the adhesion in accordance with the following
scale:
5A No peeling or removal
4A Trace peeling or removal along incisions
3A Jagged removal along incisions up to '/I6 in. ( I .6 mm) on
either side
2A Jagged removal along most of incisions up to '/E in. (3.2
mm) on either side
IA Removal from most of the area of the X under the tape
OA Removal beyond the area of the X
6.8 Repeat the test in two other locations on
each test panel. For large structures make sufficient
tests to ensure that the adhesion evaluation
is representative of the whole surface.
6.9 After making several cuts examine the
cutting edge and, if necessary, remove any flat
spots or wire-edge by abrading lightly on a fine
oil stone before using again. Discard cutting tools
that develop nicks or other defects that tear the
film.
7. Report
7.1 Report the number of tests, their mean
and range, and for coating systems, where the
failure occurred that is, between first coat and
substrate, between first and second coat, etc.
7.2 For field tests report the structure or article
tested, the location and the environmental conditions
at the time of testing.
' Permacel 99 manufactured by Permacel. New Bnmswick.
NJ 08903, and available from various Permacel tape distributors
is reponed to be suitable for this purpose. The manufacturer of
the tape used in the interlaboratory study' has advised that as
of September I98 I the properties of this tape are being changed.
Users of its should, therefore, check whether current material
gives comparable results to previous supplies.
340

D 3359
7.3 For test panels report the substrate employed,
the type of coating, the method of cure,
and the environmental conditions at the time of
testing.
8. Precision Test'
8.1 In an interlaboratory study of this test
method in which operators in six laboratories
made one adhesion measurement on three panels
each of three coatings covering a wide range of
adhesion, the within-laboratories standard deviation
was found to be 0.33 and the betweenlaboratories
0.44. Based on these standard deviations,
the following criteria should be used for
judging the acceptability of results at the 95 %
confidence level:
8.1. I Repeafabilify-Provided adhesion is
uniform over a large surface, results obtained by
the same operator should be considered suspect
if they differ by more than I rating unit for two
measurements.
8. I .2 Reproducibilify-Two results, each the
mean of triplicates, obtained by different operators
should be considered suspect if they differ
by more than 1.5 rating units.
TEST METHOD B-CROSS-CUT TAPE TEST
9. Apparatus and Materials
9. I Cutting Tool-Sharp razor blade, scalpel,
knife or other cutting device having' a cutting
edge angle between 15 and 30' that will make
either a single cut or several cuts at once. It is of
particular importance that the cutting edge be in
good condition.
9.2 Culling Guide-If cuts are made manually
(as opposed to a mechanical apparatus) a
steel or other hard metal straightedge or template
to ensure straight cuts.
9.3 Rule-Tempered steel rule graduated in
0.5 mm for measuring individual cuts.
9.4 Tope, as described in 4.3.
9.5 Rubber Eraser, on the end of a pencil.
9.6 Illumination, as described in 4.5.
9.7 Magnifving Glass-An illuminated magnifier
to be used while making individual cuts
and examining the test area.
10. Test Specimens
10.1 Test specimens shall be as described in
Section 5.
11. Procedure
11.1 Where required or when agreed upon,
subject the specimens to a preliminary test before
conducting the tape test (see Note 3). After drying
or testing, select an area free of blemishes and
minor surface imperfections.
I I .2 Place the panel on a firm base and under
the illuminated magnifier make parallel cuts as
follows:
11.2.1 For coatings having a dry film thickness
up to and including 2.0 mils (50 pm) space
the cuts 1 mm apart and make eleven cuts unless
otherwise agreed upon.
11.2.2 For coatings having a dry film thickness
between 2.0 mils (50 pm) and 5 mils (125
pm), space the cuts 2 mm apart and make six
cuts. For films thicker than 5 mils use Method
A.
11.2.3 Make all cuts about '1.1 in. (20 mm)
long. Cut through the film to the substrate in one
steady motion using just sufficient pressure on
the cutting tool to have the cutting edge reach
the substrate. When making successive single
cuts with the aid of a guide, place the guide on
the uncut area.
1 1.3 After making the required cuts brush the
film lightly with a soft brush or tissue to remove
any detached flakes or ribbons of coatings.
11.4 Examine the cutting edge and, if necessary,
remove any flat spots or wire-edge by abrading
lightly on a fine oil stone. Make the additional
number of cuts at 90" to and centered on the
original cuts.
11.5 Brush the area as before and inspect the
incisions for reflection of light from the substrate.
If the metal has not been reached make another
grid in a different location.
11.6 Remove two complete laps of tape and
discard. Remove an additional length at a steady
(that is, not jerked) rate and cut a piece about 3
in. (75 mm) long.
1 I .7 Place the center of the tape over the grid
and in the area of the grid smooth into place by
a finger. To ensure good contact with the film
rub the tape firmly with the eraser on the end of
a pencil. The color under the tape is a useful
indiction of when good contact has been made.
I I .8 Within 90 k 30 s of application, remove
the tape by seizing the free end and rapidly (not
jerked) pulling it off at as close to an angle of
180' as possible.
1 I .9 Inspect the grid area for removal of coating
from the substrate or from a previous coating
' Supporling data are available from ASTM Headquarters.
Request R R WI-1008.
34 1

D 3359
using the illuminated magnifier. Rate the adhesion
in accordance with the following scale illustrated
in Fig. I:
59
49
39
29
IB
OB
The edges of the cuts are completely smooth none of the
squares of the lattice is detached.
Small flakes of the coating are detached at intersections;
less than 5 % of the area is affmd.
Small flakes of the coating are detached along edges and at
intersections of cuts. The area affected is 5 to I5 % of the
lattice.
The coating has flaked along the edges and on parts of the
squares. The area affected is I5 to 35 % of the lattice.
The coating has flaked along the edges of cuts in large
ribbons and whole squares have detached. The area affected
is 35 to 65 % of the lattice.
Flaking and detachment worse than Grade 1.
1 1.10 Repeat the test in two other locations
on each test panel.
12. Report
12.1 Report the number of tests, their mean
and range, and for coating systems, where the
failure occurred, that is, between first coat and
substrate, between first and second coat, etc.
12.2 Report the substrate employed, the type
of coating and the method of cure.
13. Precision5
13.1 On the basis of two interlaboratory tests
of this test method in one of which operators in
six laboratories made one adhesion measurement
on three panels each of three coatings covering a
wide range of adhesion and in the other operators
in six laboratories made three measurements on
two panels each of four different coatings applied
over two other coatings, the pooled standard
deviations for within- and between-laboratories
were found to be 0.37 and 0.7. Based on these
standard deviations, the following criteria should
be used for judging the acceptability of results at
the 95 ?6 confidence level:
13. I. Repeatability-Provided adhesion is
uniform over a large surface, results obtained by
the same operator should be considered suspect
if they differ by more than one rating unit for
two measurements.
13.1.2 Reproducibility-Two results, each the
mean of duplicates or triplicates, obtained by
different operators should be considered suspect
if they differ by more than two rating units.
342

D3359
Classification of Adhesion Test Results
Classification
Surface of cross-cut area from
which flaking has occurred.
(Example for six paralled cutsi
-
58
None
c
(le
38
c
28
16
__ ~
00
Greater than 65%
FIG. 1 CL.ssiCiat&a of Adhesion Test Results
The American Society for Testing and Materials takes no position respecting the validity ofany patent rights asserted in connection
with an.v item mentioned in this standard. Users ofthis standard are expressly advised that determination oJthe validity of any such
patent rights. and the risk of infiingement of such rights, are entirely their own responsibiity.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
ij not revised- either reapproved or withdrawn. Your comments are invited either /or revision of this standard or /or additional
standards and should be addressed to ASTM Headquarters. Your comments will receive care/irl consideration at a meeting ofthe
responsible technical committee. which you may attend. Uyou fwl that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards. 1916 Race St., Philadelphia, PA 19103.
343

ClSTb
Designation: D 3363 - 74 (Reapproved 1980)"
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
FILM HARDNESS BY PENCIL TEST'
This standard is issued under the fixed designation D 3363; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (E) indicates an editorial change since the last revision or reapproval.
NOTE-section 2 was editorially added and subsequent sections renumbered in June 1980.
1. Scope
1.1 This method covers a procedure for
rapid, inexpensive determination of the film
hardness of an organic coating on a substrate
in terms of drawing leads or pencil leads of
known hardness.
2. Significance
2.1 This method is especially useful in development
work and in production control testing
in a single laboratory. It should be recognized
that the results obtained may vary between
different operators and laboratories. Every
effort should be made to standardize the
hardness of the lead used and the technique
followed. If used as a basis for purchase agreement,
this method will achieve maximum accuracy
if a given set of referee pencils be agreed
upon between the purchaser and the seller.
3. Summary of Method
3.1 A coated panel is placed on a firm horizontal
surface. The pencil is held firmly against
the film at a 45" angle (point away from the
operator) and pushed away from the operator
in a ?&in. (6.5") stroke. The process is
started with the hardest pencil and continued
down the scale of hardness to either of two end
points: one, the pencil that will not cut into or
gouge the film (pencil hardness), or two, the
pencil that will not scratch the film (scratch
hardness).
4. Apparatus
4.1 A set of calibrated drawing leads (preferred)
or equivalent calibrated wood pencils
meeting the following scale of hardness:'
The difference between two adjacent leads shall
be considered one unit of hardness.
4.2 Mechanical Lead Holder, for drawing
leads if used.3
4.3 Mechanical Sharpener, draftsman-type,
is helpful for trimming wood pencils if
4.4 Abrasive Paper, grit No. 400.
5. Test Specimens and Conditions
5.1 Apply the surface coating by appropriate
means to a smooth rigid substrate and cure
properly, or use representative panels cut from
coated stock. The panels used, the curing conditions,
and the age of the coating prior to the
test shall be within the limits agreed upon
between the purchaser and the seller.
5.2 The film thickness of the coating shall
be as specified or as agreed upon between the
purchaser and the seller.
5.3 Conduct the test at 77 & 3.5"F (25 &
2°C) and 50 f 5 % relative humidity.
6. Procedure
6.1 For wood pencils, remove approximately
' This method is under the jurisdiction of ASTM Committee
D-l on Paint and Related Coatings and Materials and
is the direct responsibility of Subcommittee D01.53 on Fac-
D--,...- A c.-:-
wry-, ~scuai~u auip Meid.
Current edition approved Oct. 25. 1974. Published November
1974.
' Pencils from many manufacturers have been and may
be used in pencil hardness testing but it was apparent to the
test group (D01.53.02) that the leads supplied by two manufacturers
were more uniform. and reproducible results could
be obtained from batch to batch of leads. These are: (a)
Eberhard Faber--Microtomic and (b) Eagle Turquoise--
T 2315.
.'I Turquoise No. IO is the preferred holder, however. any
holder adequately constructed to eliminate lead slippage may
be used.
6B-5B-4B-3B-2B-B-HB-F-H-2H-3H-4H-5H-6H
Apsco Products. Inc.. Dexter Super IO Draftsman type
AlOD Cutter Assembly. or equivalent, has been found suit-
Softer
Harder
able.
6 ^_..
344

D 3363
%fi to ?4 in. (5 to 6 mm) wood from the point of
each pencil using a draftsman-type mechanical
sharpener, being careful to leave an undisturbed,
unmarked, smooth cylinder of lead.
Holding the pencil or lead holder (when using
drawing leads) at an angle of 90" to the abrasive
paper, rub the lead against the paper maintaining
an exact angle of 90" to the abrasive paper
until a flat, smooth and circular cross section is
obtained, free of chips or nicks in the edge of
the cross section. The desired edge may be
attained by cementing the abrasive paper to a
flat motor driven disk. By supporting the pencil
at 90" to the rotating disk a uniform flat lead
end may be obtained more reproducibly.5
6.2 Place the coated panel on a level, firm,
horizontal surface. Starting with the hardest
lead, hold the pencil or lead holder firmly with
the lead against the film at a 45" angle (point
away from the operator) and push away from
the operator. Exert sufficient uniform pressure
downward and forward either to cut or scratch
the film or to crumble the edge of the lead. It
is suggested that the length of the stroke be VI
in. (6.5 mm).
6.3 Repeat the process down the hardness
scale until a pencil is found that will not cut
through the film to the substrate l(either metal
or a previous coat) for a distance of at least %
in. (3 mm) (see 7.1.1).
NOTE I-The operator must watch closely for
cutting into or scratching the film. Some finishes
contain compounds that may tend to lubricate the
film. Checks should be made by close visual inspection
and by fingernail feel.
NOTE 2-111 conducting the test, if the sharp edge
of the lead is slightly chipped or crumbled, the lead
must be resharpened.
6.4 Continue the process until a pencil is
found that will neither cut through nor scratch
the surface of the film. Any defacement of the
film other than a cut (gouge) is considered a
scratch. Record each end point (if appiicable j
for gouge and scratch hardness (see 7.1).
NOTE 3-With some films, the two end points will
be identical.
6.5 Make a minimum of two determinations
for gouge hardness (6.3) and scratch hardness
(6.4) for each pencil or lead.
7. Report
7.1 Report two end points as follows:
7.1.1 Gouge Hardness-The hardest pencil
that will leave the film uncut for a stroke length
of at least $6 in. (3 mm).
7.1.2 Scratch Hardness-The hardest pencil
that will not rupture or scratch the film.
7.2 Report the make and grade of lead or
pencil used.
7.3 Report any deviation from standard conditions,
including roughness in the finish.
8. Precision
8.1 In an interlaboratory test of this method
with three different films on panels, ten laboratories
and operators and repeated by switching
leads and panels between laboratories, the
within-laboratories standard deviation was
found to be 0.52 and the between-laboratories
standard deviation was found to be 0.6 I. Based
on these standard deviations the following criteria
should be used for judging the acceptability
of results at a 95 96 confidence level:
8.1.1 Repeatability-Two results obtained
by two operators within a laboratory using the
same pencils and panels should be considered
suspect if they differ by more than one pencil
unit on the scale described in 4.1.
8.1.2 Operator Reproducibility-Two results,
each the mean of at least two determinations,
obtained by operators in different laboratories
using the same pencils and panels or different
pencils with the same panels should be considered
suspect if they differ by more than one
pencil unit on the scale described in 4. I.
"A suitable device for this purpose is available from
Gardner Laboratories, Inc., P. 0. Box 5728. Bethesda. Md.
The American Society for Testing and Materials takes no position respecting the validicv of an,. patent rights asserted in
connection with any item mentioned in this standard. Users ofthis standard are express!, advised that determination ofthe validity
of any such patent rights, and the risk of infringement of such rights. are entire!, their own responsibili!,.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyfive years
and if not revised, either reapproved or withdrciwn. Your comments cre invited either for revision of this Ttandard orfor additional
standards and should be addressed to ASTM Headquarters. Your comments will Ycceive careful conridcration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, Pa. 19103.
345

AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa., 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not hted in the current combined Index. will appear in the next edition
Standard Test Method for
STRENGTH PROPERTIES OF DOUBLE LAP SHEAR
ADHESIVE JOINTS BY TENSION LOADING'
This Standard is issued under the fixed designation D 3528; the number immediately following the designation indicates
the year of original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year
of last reapproval.
INTRODUCTION
The accuracy of the results of strength tests of adhesive bonds will depend on the
conditions under which the bonding process is carried out. Unless otherwise agreed
upon between the manufacturer and the purchaser, the bonding conditions should be
prescribed by the manufacturer of the adhesive. In order to ensure that complete
information is available'to the individual conducting the tests, the manufacturer of the
adhesive should furnish numerical values and other specific information for each of the
following variables:
(1) Surface preparation
(2) Mixing directions
(3) Adhesive application
(4) Assembly conditions
(5) Curing conditions
(6) Testing conditions
A range may be prescribed for any variable by the manufacturer of the adhesive if it
can be assumed by the test operator that any arbitrarily chosen value within such a
range, or any combination of such values for several variables will be acceptable to
both the manufacturer and the purchaser of the adhesive.
1. Scope
1.1 This method covers the determination
of the tensile shear strengths of adhesives for
bonding metals when tested in an essentially
peel-free standard specimen that develops adhesive
stress distribution representative of
those developed in a typical low peel production
type structural joint. The reproducibility
of the strengths achieved are directly related
to conformance with specified conditions of
preparation and testing.
2. Applicable Documents
2.1 ASTM Standards:
B 36 Specification for Brass Plate, Sheet,
Strip, and Rolled Bar2
B 152 Specification for Copper, Sheet,
Strip, Plate, and Rolled Bar2
B 209 Specification for Aluminum-Alloy
Sheet and Plate3
B 265 Specification for Titanium and Titanium
Alloy Strip,3 Sheet, and Plate4
E 4 Verification of Testing Machines'
E 122 Sample Size to Estimate the Average
Quality of a Lot or Process, Choice of6
E i7 i Standard Atmosphere for Condirioning
and Testing Materials'
This method is under the jurisdiction of ASTM Committee
D-14 on Adhesives, and is the direct responsibility
of Subcommittee D 14.80 on Metal Bonding Adhesives.
Current edition approved Aug. 27, 1976. Published
October 1976.
Annual Book of ASTM Standards, Part 6.
Annual Book of ASTM Standards, Part 7.
Annual Book of ASTM Standards, Parts 8 and 45.
Annual Book of ASTM Standards, Parts 10, 14, 32,
35, and 41.
Annual Book ofASTM Standards, Parts 15 and 41.
Annual Book of ASTM Standards, Parts 35 and 41.
346

D 618 Conditioning Plastics and Electrical
Insulating - Materials for Testing8
3. Significance
3.1 This method is designed to produce
shear property data for the process control
and specification of adhesives. The method
may also be useful for research and development
of adhesives.
3.2 Lap shear properties vary with specimen
configuration preparation, speed, and
environment of testing. Consequently, where
precise comparative results are desired, these
factors must be carefully controlled and reported.
4. Apparatus
4.1 Testing Machine, conforming to the requirements
of Methods E 4. The testing machine
should be so selected that the breaking
load of the specimens falls between 15 and
85 % of the full-scale capacity. The machine
should be capable of maintaining a rate of
loading Of 8'27 to 9'65 MPa (l2O0 to l4Oo
psi)/min, or if the rate is dependent on crosshead
motion, the machine should be set to
approach the rate of loading. It should be
provided with a suitable pair of self-aligning
grips to hold the specimen. The grips and
vestigated. The maximum permissible length may
be computed from the following relationship:
where:
L = length of overlap, in., (Figs. 1 and 3),
t, = thickness of doubler, in., (Figs. 1 and
3)9
t2 = thickness of aderend in., (Figs. 1-and
31,
Fty = yield point of adherend (or stress at
proportional limit), psi, and
T = 150 % of the estimated average shear
strength of the adhesive bond, psi.
NOTE 2-Variations in adherend thickness, and
of the length of the overlap, normally influence the
test values and make direct comparison of test data
questionable. Therefore, it is preferable for the
comparative or specification tests, to standardize on
the typical specimen configuration shown with ap
propriate adherend gages as computed per Note 1.
When specimens incorporating special lap lengths
are developed for specific studies, the adherend
gage and geometry, once established, should not be
altered.
5 -2 The following grades of metals are retommended
for the test specimens:
Brass
Copper
Aluminum
Specification B 36. CDA 268
Specification B 152, CDA 110
Specification B 209, Alloy 2024,
T3 Temper
attachments should be so constructed that Corrosion-resisting Specification A 167, Type 302,
they will move into alignment with the test
specimen as soon as the load is applied, so
that the long axis of the test specimen will
coincide with the direction of the applied pull
through the center line Of the grip
5. Test Specimen
5.1 The test specimens should conform to
one of the alternative types as dimensioned
and shown in Figs. 1 or 3. Cut the specimens
from the appropriate test panels that have
been prepared as prescribed in Section 6. For
aluminum-alloy specimens the recommended
thickness of the sheet is 3.24 ? 0.125 mm
(0.125 - 0.005 in.). The recommended test
overlap length (L) for most metals, with adherends
of the prescribed metal thickness and
arranged as shown in Figs. 1 and 3, is 12.7 ?
0.25 mm (0.5 ? 0.01 in.).
NOTE 1 -Since it is undesirable to exceed the
yield point of the metal in tension during test, the
permissible length of overlap in the specimen will
vary with the thickness and type of metal and on the
general level of strength of the adhesive being in-
Titanium
2B Finish
Specification B 265, Grade 3
5.3 The minimum sample size necessary to
develop typical or design values for a given
joint geometry should be specified on the test
request in accordance with the principles presented
in Recommended Practice E 122. Because
of inherent variations in adhesive properties,
due to process variables, specimens
should be selected from a minimum of four
different test panels.
6. Test Specimens
6.1 It is recommended that the test panels
be of a width sufficient to be cut into at least
five test specimens unaffected by panel joint
edge variables. Do the cutting operation in a
manner that will not overheat, damage by
exposure to unsatisfactory coolants, or mechanically
damage the bonded joints. Panels
Annual Book of ASTM Standards, Parts 22, 35, and
39.
347

of two alternative configurations ure shown in
Figs. 2 and 4 from which the test specimens
(Figs. 1 or 3) may be cut. Vary the adherend
sheet length to accommodate changes in bond
lap length. Cut sheets of the prescribed adherend
metals to suitable size. The edges of the
metal panels which will be within (or bound)
the lap joints should be free of burrs, deformation,
and bevels. The bond faying surfaces
should be smooth (rms 160 max) before the
panels are surface treated and bonded. Prepare
the bond faying surfaces carefully in accordance
with the procedure prescribed by the
adhesive manufacturer or the governing ap
proved process specification and assemble
with adequate spacer sheets to prevent bondline
deformation in the lap area. Prepare and
apply the adhesive in accordance with the
prescribed process specification. The prime
coat, if used, apply to a bond area faying
surface in sufficient width to extend beyond
the lap bond area by approximately 6 mm
(0.125 in .) . The adhesive, liquid or film, a p
ply or position in the bond area limiting its
extension beyond the adherends to 1.62 k
0.25 mm (0.064 2 0.001 in.) to prevent excessive
filleting. Cure the adhesive in conformance
with the prescribed process specification.
NOTE 3 -Bonding specimens in multiple-width
panels is believed to produce the most representative
individual test specimens. Die-punched panels
or individual specimens may be used for s ecial
studies; however, fabrication problems will E e increased
due to inadvertent slippage of the individual
adherends.
7. Procedure
7.1 Precondition the finished specimens as
specified in the test request. Conduct room
temperature tests under controlled temperature
and relative humidity conditions in accordance
with Specification E 171 (23 k 2°C
(73.4 ? 3.6"F) and 50 2 5 % relative humidity).
7.2 Conduct depressed or elevated temperature
tests in a controlled chamber. The
chamber should be of sufficient size to accommodate
the test grips for preconditioning and
thermal stability during the test. After the test
chamber and grips have been brought to equilibrium,
place an instrumented dummy specimen
in the grips and calibrate the bondline
temperature for each desired test condition.
D 3528
NOTE 4 -It is recommended that the dummy
specimen be calibrated by the following procedure.
Instrument the specimen with two thermocouples.
Position one in the geometric center of the bondline
and secure the second to the external surface, in the
geomctric center of the metal lap area. Position and
secure the dummy specimen in the test grips within
the thermally stabilized test chamber. Record the
time required for the bondline to reach the test
temperature. Monitor and simultaneously record
the temperature of the surface thermocouple.
7.3 Measure the width of the specimen and
the overlap lengths to the nearest 0.25 mm
(0.01 in.) to determine the shear areas.
7.4 Place the specimens in the grips of the
test machine so that the terminal 31.8-mm
(1.25411.) ends are engaged firmly and so that
the long axis of the test specimen coincides
with the direction of the pull.
7.4.1 There should be no slack in the test
linkage just prior to applying a load; a preload,
if used, shall not exceed 350 kPa (50
psi) during final stabilization and soak.
7.4.2 Control the temperature exposure,
where applicable, by the cycle determined
with the calibration. A periodic check of the
cycle maybe' made by attaching a thermocouple
to the external surface of a test specimen
in a manner similar to the calibration test.
7.5 The test temperature tolerance shall be
in accordance with Method D 618.
7.6 Unless otherwise specified, load the
test specimen to failure at a rate of 8.27 to
9.65 MPa (1 200 to 1400 psi)/min. This rate of
loading will be approximated by a free crosshead
speed of 1.27 mm (0.05 in.)/minute.
7.7 Record the load at failure, the test
temperature and soak time, the nature and
amount of failure (cohesion in the adhesive,
adhesion between adhesive and metal or
metal). Failing stresses shall be expressed in
kilograms per square centimeter (or poundsforce
per square inch) of total shear area
(Goth God iiries) caicuiaieci to the nearest
0.06 cm,2 (0.01 in.'), and to the third significant
figure.
8. Report
8.1 The report should include the following:
8.1.1 Complete identification of the adhesive
tested, including type, form, source,
manufacturer's code numbers, procurement
specification number (where applicable),
348

D 3528
weight per square foot at application and
cured glueline thickness.
8.1.2 Complete identification of the adherend
material, the individual adherend thicknesses
and the heat treat condition (where
applicable),
8.1.3 Adherend preparation for bonding,
8.1.4 Adhesive application and bonding
conditions used in preparation of the specimens
(specification number, where applicable),
8.1.5 Final width of specimen and length
of bond overlap measured to the nearest 0.25
mm (0.01 in.),
8.1.6 Conditioning procedures for specimens
prior to testing,
8.1.7 Test temperature and soak time,
8.1.8 Number of specimens tested, coded
for positions in test panels,
8.1.9 Type of specimen and number of test
panels represented,
8.1 .10 Maximum, minimum, average, and
coefficient of variation for the stress at failure,
and
8.1.11 Nature of failure, including the estimated
percentage of failure in cohesion and
adhesion or metal failure.
T, = 1.6 mm
Tz = 3.2 mm
A = Test Gluelines
B = Spacer = T2
C = Area in Test Grips
D = Shear Area
FIG. 1 Form and Dimensions of Specimen Type A.
349

T
I
0
4 190.6 m + L
4- 95.3 m + L -b
A = Predrilled Pinholes
(4 required; 2.4-mm diameter)
FIG. 2 Form and Dimensions of Standard Test Panel for Type A Specimens.
I, A C I-B
63.5 m 63.5 m
k- 129.4 + 2L m
193 + 2L m
TI = 1.6 mm
Tz = 3.2 mm
A = Test Gluelines
B = Area in Test Grips
C = Shear areas
FIG. 3 Form and Dimensions of Specimen Type B.
350

2.4 m-b
c- 95.3 + L mm +
193 + 2L mm
f-- 95.3 + L "
A = Predrilled Pinholes
(4 required; 2.4-mm diameter)
B = Suggest TFE-fluorocarbon Filler for
Adhesive Flash Control
FIG. 4 Form and Dimensions of Standard Test Panel for Type B Specimens.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted
in connection with any item mentioned in this standard. Users of this standard are expressly advised that determination
of the validity of any such patent rights, and the risk of infringement of such rights, is entirely rheir own responsibility.
35 1

Designation: D 3658 - 78 (Reapproved 1984)"
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Practice for
DETERMINING THE TORQUE STRENGTH OF
ULTRAVIOLET (UV) LIGHT-CURED GLASS/METAL
ADHESIVE JOINTS'
This standard is issued under the fixed designation D 3658; the number immediately following the designation indicates the
year of on inal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapprovaf A superscript epsilon (a) indicates an editorial change since the last revision or reapproval.
'' NOTE--Section 6.5.3 was corrected editorially in February 1984.
1. scope
1.1 This practice covers the simplistic comparison
of strengths of glass/metal joints when
the adhesive is cured by ultraviolet (UV)
radiation and standard specimens are used
and tested under specified conditions of prep
aration, radiation, and load.
1.2 This practice involves torque loading
UV-bonded hexagonal metal blocks to glass
plates.
1.3 This practice may be used to obtain comparative
torque strength-to-failure data for other
bonded joint systems, radiation cured or not.
1.4 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health practices
and determine the applicability of regulatory limitations
prior to use.
2. Applicable Documents
2.1 ASTM Standards:
A 109 Specification for Steel, Carbon, Cold-
Rolled Strip'
A 167 Specification for Stainless and Heat-
Resisting Chromiun-Nickel Plate, Sheet,
and Strip'
B 36 Specification for Brass Plate, Sheet, Strip,
and Rolled Ba?
€3 152 Specification for Copper Plate, Sheet,
Strip, and Rolled Ba?
B 265 Specification for Titanium and Titanium
Alloy Strip, Sheet, and Plate'
D 1002 Test Method for Strength Properties
of Adhesives in Shear by Tension Loading
( Metal-to-Metal)6
3. Apparatus
3.1 The apparatus is schematically shown
in Fig. 1.
3.2 The apparatus shall be capable of
transferring a uniform and continuous torque
to the bonded hexagonal block.
3.3 An accurate and reliable means of recording
load to failure, that is, x-y or strip
chart recorder, should also be a part of the
test system.
3.4 A safety shield or other safety device
shall be incorporated as part of the system to
prevent injury from possible shattering glass.
4. Test Specimens
4.1 Recommended specimens are as shown
in Fig. 2.
4.2 Selection of the test metal for hexagofial
blocks is ai the discretion of the user;
however, the following grades are recommended
(see Test Method D 1002):
I This practice is under the jurisdiction of ASTM-Committee
D-14 on Adhesives and is the'direct responsibility of Subcommittee
D14.20 on Durability.
Current edition approved Feb. 24,1978. Published May 1978.
*Annual Book of ASTM Standards, VOI 01.03.
Annual Book of ASTM Standards, Vol02.0 I.
' Annual Book of ASTM Standards, Vol02.02.
209 Specification for A1uminum-A1loy Annual Book ofASTM Standards, Vol02.04.
Sheet and Plate4
Annual Book of ASTM Standards, Vol 15.06.
352

Metal
Specification
Brass B 36, Alloy 8
Copper
B 152, Type A
Aluminum
B 209, Alloy 2024, T3
Temper
Steel A 109, Grade 2
Corrosion-resisting steel A 167, Type 302
Titanium B 265
4.3 Hexagonal blocks may be reused after
testing by bonding the opposite end of the
block or by cleaning the original bonded end
by sanding or grinding and taking care to
ensure that ends are smooth and parallel.
4.4 Selection of the glass plate is at the
discretion of the user. Standard lh-in. (13-
mm) thick pressed plate glass is recommended.
5. Preparation of Test Specimens
5.1 The assembly and cure of the specimen
is recommended as shown in Fig. 3.
5.2 Cut glass plates 3 by 3 in. (76 by 76
mm) square to fit the holding fixture without
lateral movement.
5.3 A recommended cleaning procedure is
to soak the glass plates in a dilute detergent
solution for 2 to 3 min, followed by light
scrubbing with an absorbent cleaning tissue .'
Then thoroughly rinse the glass plates with
distilled or deionized water and air dry.
5.4 Metal hexagonal blocks, '/z in. (13
mm) high, may be prepared by light sanding
with 400 grade wet or dry emery paper,
followed by solvent wiping, such as l,l,ltrichloroethane.
NOTE - Preparation of adherends are recommended
only. Users may employ methods conducive
to actual practice. Reported data should be
qualified as to the method of surface preparation.
5.5 Apply adhesive to the hexagonal button
in sufficient quantity to cause wetting of
the entire surface when clamping pressure is
applied by means of two 10-lb (0.9-kg) spring
clamps.
6. Procedure
6.1 The level of the radiation and time of
exposure should be within the tolerances
specified for the cure.
6.2 Measure the intensity of the radiation
with a suitable meter sensitive to the radiation
used. Place the meter in a position related to
the bond line.
6.3 If the material is subject to post curing,
it must remain at specified conditions of temperature,
humidity, etc, prior to testing.
6.4 Fully cured specimens may be subjected
to environmental exposure such as
weathering, humidity, temperature, or combinations
thereof, prior to testing.
6.5 Test the bonded specimen as follows:
6.5.1 Place the specimen in the holding
fixture, ensuring that no lateral movement is
evident.
6.5.2 Mechanically apply a torque on the
hex nut assembly or by means of a constant
drive loader at a rate of 0.5 rpm (suggested)
until failure occurs.
6.5.3 Record the load at failure and the
nature and amount of the failure (cohesive in
adhesive or glass or adhesive at metal/adhesive
or gladadhesive interface). Express all
failure loads in lbf. in. (or N. m).
7. Report
7.1 The report shall include the following:
7.1.1 Complete identification of the adhesive
tested, including type, source, manufacturers'
code numbers, form, etc.
7.1.2 Complete identification of the metal
used, its thickness, and the method of cleaning
and preparing its surfaces prior to bonding.
7.1.3 Complete identification of the glass
used, as in 7.1.2.
7.1.4 Application and bonding conditions
used in preparing specimens, including the
type intensity (watts per steradian), and exposure
time of the radiation used.
7.1.5' Conditioning procedure prior to testing.
7.1.6 Number of specimens tested.
7.1.7 Maximum, minimum, and average
values for load at failure.
7.1.8 Standard deviation and coefficient of
variation for the specimens tested.
7.1.9 k:erzge thickness of the adhesive
layer after cure of the joint. Subsequent measurements
should be obtained if the specimens
are exposed to environmental conditioning.
7.1.10 The nature of the failure, including
the average estimated percentages of failure;
that is, adhesives-cohesive, glass-cohesive, interface
failure (glass/adhesive or metal/adhesive)
.
' Kimwipes, available from Kimberly-Clark Corp., 128
N. Lake, Neenah. Wisc. 54956, or equivalent, have been
found satisfactory for this purpose.
353

D 3658
Details
1 -Base plate
2 -Upright
3 -Mounting bracket
4-Lebow socket wrench sensor Model 2133-103
5-Pillow block-Boston #PPBlO
6-Extension -Armstrong #4-105 A
7 - 1-in. (25.4") hexagonal socket-Armstrong #A4632
8 - UV specimen (see Fig. 2)
9-Adjustable side guides (Fig. 2)
10-Neoprene pad (bonded to Detail 9) (Fig. 2)
Dimensions
in.
mm
A 0.50 13
B 3.75 95
C 0.62 16
D 5.50 140
E 0.50 13
F 6.75 170
G 6.25 160
H 2.62 66
Flg. 1 UVTestlagAppntus.
354

I
"p:
t
I\
D"
A
B
c
D
E
L
"C"
t
,
Details
1 -Glass plate
2 -Hexagonal metal block
Dimensions
Dimensions
in. mm in .z
3 .OO
76
Bond
1 SO
38
Area F
0.866
0.47 12
1 .oo 25
0.50 13
FIG. 2 UV Specimen Configuration.
1
"E"
t
mmz
559
355

UV RADIATION
Details
1 - UV specimen
2 -Clamp
3 -Neoprene cushion
4 -Clamp support (glass or metal)
5 -Bond surface (Ref.)
FIG. 3 Adhesive Joint Preparation.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every jive years and
not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive cardul consideration at a meeting of the
responsible technical committee, which you may attend. uyou fie1 that your comments have not received a fair hearing you should
make your.views known to the ASTM Committee on Standards, 1916 Race St.. Philadelphia. Pa. 19103.
356

4Ib
Designation:
0 3807 - 79 (Reappmved 1984p'
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 49103
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
STRENGTH PROPERTIES OF ADHESIVES IN CLEAVAGE
PEEL BY TENSION LOADING (ENGINEERING PLASTICS-
TO-ENGINEERING PLASTICS)'
This standard is issued under the fixed designation D 3807; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
NoTE-!%dOn 9 was added editonally in July 1984.
INTRODUCTION
The accuracy of the results of strength tests of adhesive bonds will depend on the
conditions under which the bonding process is carried out. Unless otherwise agreed
upon by the manufacturer and the purchaser, the bonding conditions shall be prescribed
by the manufacturer of the adhesive. In order to ensure that complete information is
available to the individual conducting the tests, the manufacturer of the adhesive shall
furnish numerical values and other specific information for each of the following
variables:
(I) Procedure for preparation of surfaces prior to application of the adhesive, the
cleaning and drying of the plastic surfaces, and surface treatments.
(2) Complete mixing directions for the adhesive.
(3) Conditions for application of the adhesive, including the amount of adhesive to
apply or thickness of films, number of coats to be applied, whether the coats are to be
applied to one or both surfaces, and the conditions of drying where more than one coat
is required.
(4) Assembly conditions before application of pressure, including the room temperature,
relative humidity, length of time, and whether open or closed assembly is to be
used.
(5) Curing conditions, including the amount of pressure to be applied, the length of
time under pressure, method of applying pressure, heat-up rate, and the temperature of
the assembly when under pressure. It should be stated whether this temperature is that
of the bond line or of the atmosphere at which the assembly is to be maintained.
(6) Conditioning procedure before testing, unless a standard procedure is specified,
including the length of time, temperature, and relative humidity.
A range may be prescribed for any variable by the manufacturer of the adhesive if it
can be assumed by the test operatoi that any arbitrarily chosen value within such a
range, or any combination of such values for several variables, will be acceptable to
both the manufacturer and the purchaser of the adhesive.
NOTE 1-Results of round-robin tests is available adhesives for bonding engineering plastics when
from ASTM Headquarters, 1916 Race St., Philadel- tested on a standard specimen and under specific
phia, PA 19103 as RR: D14-1002.
' This test method is under the jurisdiction of ASTM Com-
1. scope
mittee D-14 on Adhesives and is the direct reswnsibility of
Subcommittee D14.40 on Adhesives for Plastics.
This test method the Current edition approved July 27, 1979. Published Septemof
the comparative cleavage/peel strengths of ber 1979.
357

D 3807
conditions of preparation and testing.
1.2 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health practices
and determine the applicability of regulatory limitations
prior to use.
2. Description of Terms
2.1 cleavage/peel strength-the average load
per unit width of bond line required to produce
progressive separation of two bonded, semirigid
adherends, under conditions designated in this
method.
2.2 semirigid-indicates that the adherends
shall have such dimensions and physical properties
as to permit bending them through any
angle of up to 30 deg without breaking or
cracking.
3. Apparatus
3.1 Tension Testing Machine, capable of applying
a tensile load having the following prescribed
conditions:
3.1.1 The machine and loading range shall
be so selected that the maximum load on the
specimen falls between 15 and 85% of the
upper limit of the loading range.
3.1.2 The rate of movement between heads
shall remain essentially constant under fluctuating
loads.
NOTE 2-It is difficult to meet this requirement
when loads are measured with a spring-type or pendulum-type
weighmg device. Gear-driven head separation,
such as Instron testing units employ, would
be recommended.
3.1.3 The machine shall be equipped with
suitable grips capable of clamping the specimens
f d y throughout the tests.
3. !.4 The maehhe shall be autographic, giving
a chart that can be read in terms of cencimetres
(or inches) of separation as one coordinate
and applied load as the other coordinate.
3.1.5 The applied tension as measured and
recorded shall be accurate within fl %.
3.2 Conditioning Room or Desiccators, capable
of maintaining a relative humidity of 50
f 5 96 at 23 f 2°C.
4. Test Specimen
4.1 Laminated test panels (see Fig. 1) shall
consist of two semirigid adherends properly
prepared and bonded together in accordance
with the adhesive manufacturer's recommendations.
Specially prepared test specimens shall
be 25.4 mm (1 in.) wide by 177.3 mm (7 in.)
long, but shall be bonded only over approximately
76 mm (3 in.) of their length. Test
specimens of these same dimensions may also
be cut from larger, fully laminated panels.
NOTE 3-Direct comparisons of different adhesives
can be made only when specimen construction
and test conditions are identical.
NOTE &General purpose ABS (acrylonitrile-butadiene-styrene)
molded plaques approximately 6.3
mm (0.25 in.) thick have been found satisfactory as
adherends for structural adhesives. Other engineering
plastics and metals have been found satisfactory for
specific adhesives.
NOTE 5-The adherend substrate selected must
exhibit sufficient toughness and stiffness to resist
substrate failure, thus forcing the adhesive layer to
absorb the stresses of the testing process. Should the
substrate fail cohesively, the ultimate cleavage/peel
strength of the adhesive under test has not been
determined.
4.2 The bonded panels shall be cut into 25-
mm (1-in.) wide test specimens by a means that
is not deleterious to the bond. A suggested
cutting process employs Rockwell-Delta band
saw with a 6.3" (0.25-in.) thick blade with
18 teeth per 25.4 mm (1 in.) and 12.5 mm (0.5
in.) wide. The feed rate and saw speed controlled
to minimize heat build up during the
sawing process.
4.3 The 101-mm (4 in.) long unbonded ends
shall be separated sufficiently to insert gripping
wires for attachment to testing machine jaws.
4.3.1 The gripping wire employed shall be
20-gage American Standard steel wire [0.8 mm
(0.03 in.) in diameter] attached to the specimen
in a manner shown in Fig. 1. The gripping
wires shall be twisted together yielding approximately
10 twists per 25 mm (1 in.) of twisted
length.
NOTE 6-Aitemaiive methods of gripping wire
attachment may be employed if necessary. Sufficient
flexibility in the attaching wires must be maintained
to allow self-alignment of the gripping wires during
the course of the pull testing of the specimens.
4.4 At least ten test specimens shall be tested
for each adhesive.
NOTE 7-Within the limitations imposed by Note
3 under other specimen widths may be used, provided
the test machine grips are of ample width to apply
the load uniformly across the width of the adherends.
5. Conditioning
5.1 Condition specimens for 3 days at a rel-
358

ative humidity of 50 k 5 96 at 23 f 2"C, except
where the adhesive manufacturer may specify
such an aging period to be unnecessary or a
shorter period to be adequate.
6. Procedure
6.1 Clamp the connecting wires from the
specimen (Fig. 1) in the test grips of the tensiontesting
machine. Apply the load at a constant
crosshead speed of 12.7 mm (0.5 in.)/min.
6.2 During the cleavage/peel test make an
autographic recording of load values versus
crosshead movement or load versus distance
peeled.
6.3 Determine the cleavage/peel resistance
over at least a 50.8" (2-in.) length of the
bond line after the initial peak.
7. Calculations
7.1 Determine the average load (in kilonewtons
per metre width of specimen required to
separate the adherends) from the autographic
curve for the first 50.8 mm (2 in.) of cleavage/
peel after the initial peak. It is preferred that
the average load be determined from the curve
with the use of a planimeter.
NOTE 8-In case a planimeter is not used, the
average load may be calculated as the average of
load readings taken at fmed increments of crosshead
motion. For example, the load may be recorded at
each 5-mm (0.2-in.) intervals of head motion following
the initial peak, until at least seven readings have
been obtained.
8. Report
8.1 The report shall include the following:
8.1.1 Complete identification of the adhesive
tested, including type, source, manufacturer
code number, batch or lot number, form, etc.
8.1.2 Complete identification of adherends
used, including material, thickness, surface
preparation, and orientation.
8.1.3 Description of bonding process, including
method of application of adhesive,
glue-line thickness, drying or precuring conditions
(where applicable), curing time, temperature,
and pressure.
8.1.4 Average thickness of adhesive layer
after formation of the joint, within 0.025 mm
(0.001 in.). The method of obtaining the thickness
of the adhesive layer shall be described
including procedure, location of measurement,
and range of measurements.
8.1.5 Complete description of test specimens,
including dimensions and construction
of test specimens, conditions used for cutting
individual test specimens, number of test panels
represented, and number of individual test
specimens.
8.1.6 Conditioning procedure prior to test-
ing.
8.1.7 Type of test machine and crosshead
separation rate used.
8.1.8 Method of recording load and determining
average load.
8.1.9 Average, maximum, and minimum
cleavage/peel load values for each individual
specimen.
8.1.10 Average cleavage/peel strength in kilonewtons
per metre width for each combination
of materials and constructions under test
and
8.1.1 1 Type of failure, that is, cohesive failure
with the adhesive or adherend, adhesion to
the adherend, or combinations thereof, for each
individual specimen.
9. Precision and Bias
9.1 Precision and bias have not been determined
for this test method.
359

FIG. 1 Cleavage Peel Test Specimen
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any ilem mentioned in this standard Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed evevjve years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee. which you may attend. Ifyoukel that your comments have not received ahir hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St.. Philadelphia, Pa. 19103.
360

AMERICAN
Designation: D 4060 - 84
SOCIETY FOR TESTING AND MATERIALS
1916 Ram St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will -r in the next edition.
Standard Test Method for
ABRASION RESISTANCE OF ORGANIC COATINGS BY THE
TABER ABRASER’
This standard is issued under the fixed designation D 4060, the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (6) indicates an editorial change since the last revision or reapproval.
1. scope
I. I This test method covers the determination
of the resistance of organic coatings to abrasion
produced by the Taber Abraser on coatings ap
plied to a plane, rigid surface, such as a metal
panel.
1.2 Because of the poor reproducibility of this
test method, it should be restricted to testing in
only one laboratory when numerical abrasion
resistance values are to be used. Interlaboratory
agreement is improved significantly when rankings
of coatings are used in place of numerical
values.
I .3 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safetyproblems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health practices
and determine the applicability of regulatory limitations
prior to use.
2. Applicable Documents
2.1 ASTM Standards:
D823 Methods of Producing Films of Uniform
Thickness of Paint, Varnish, Lacquer,
and Related Products on Test Panels’
D 1005 Methods for Measurement of Dry Film
Thickness of Organic Coatings2
D I 186 Methods for Nondestructive Measurement
of Dry Film Thickness of Nonmagnetic
Coatings Applied to a Ferrous Base’
D 1400 Method for Nondestructive Measurement
of Dry Film Thickness of Nonconductive
Coatings Applied to a Nonferrous Metal
Base’
D2240 Test Method for Rubber Property-
Durometer Hardness3
3. Descriptions of Terms Specific to This Standard
3.1 Abrasion resistance can be expressed as
one or more of the following terms:
3.1.1 wear index-I000 times the loss in
weight in milligrams per cycle.
3.1.2 weight loss-the loss in weight in milligrams,
determined at a specified number of cycles.
3. I .3 wear cycles per mil-the number of cycles
of abrasion required to wear a film through
to the substrate per mil of film thickness.
4. Summary of Method
4.1 The organic coating is applied at uniform
thickness to a plane, rigid panel and, after curing,
the surface is abraded by rotating the panel under
weighted abrasive wheels.
4.2 Abrasion resistance is calculated as loss in
weight at a specified number of abrasion cycles,
as loss in weight per cycle, or as number of cycles
required to remove a unit amount of coating
thickness.
5. Apparatus
5.1 Taher Abra~er.~
5.2 Abrasive Wheels-Resilient calibrase
’ This test method is under the jurisdiction of ASTM Committee
D- I on Paint and Related Coatings and Materials and is
the direct responsibility of Subcommittee DO I .23 on Physical
Properties of Applied Paint Films.
Current edition approved Aug. 3 I. 1984. Published January
1985. Originally published as D 4060 - 81. Last previous edition
D4060-81.
Annual Book of ASTM Standards. Vol06.0 I .
’ Annical Book ofASTM Standards, Vols 08.02 and 09.01.
‘ Available from Teledyne Taber. North Tonawanda. NY
14120.

~
wheels No. CS- 10 or CS- 17, as required, shall be
used. Because of the slow hardening of the rubber
bonding material in this type of wheel, the wheels
should not be used after the date marked on
them, or one year after their purchase if the
wheels are not dated.
NOTE 1 -The hardness of the wheels can be checked
by Test Method D2240. An acceptable hardness for
both types of wheels is 8 1 * 5 units on Shore Durometer
A-2 Scale.
NOTE 2-The CS- 17 wheels produce a harsher abrasion
than the CSIO wheels.
5.3 Resurfacing Medium, an Sll abrasive
disk, used for resurfacing the abrasion wheels.
5.4 Vacuum Pick-Up Assembly, consisting of
a vacuum unit, a variable transformer suction
regulator, a nozzle with bracket attachment, and
a connecting hose with adaptor.
6. Test Specimens
6.1 Apply a uniform coating of the material
to be tested to a plane, rigid panel. Specimens
shall be a disk 4 in. (100 mm) in diameter or a
plate 4 in. ( 100 mm) square with rounded corners
and with a ‘/&in.(6.3-mm) hole centrally located
on each panel. Prepare a minimum of two coated
panels for the material.
NOTE 3-The coatings should be applied in accordance
with Methods D823, or as agreed upon by the
purchaser and the seller.
NOTE 4-The thickness of the dry coatings should
be measured in accordance with Methods D 1005,
D 1186, or D 1400.
7. Standardization
7.1 Mount the selected abrasive wheels on
their respective flange holders, taking care not to
handle them by their abrasive surfaces. Adjust
the load on the wheels to 10oO g.
7.2 Mount the resurfacing medium (S11abrasive
disk) on the turntable. Lower the abrading
heads carefully until the wheels rest squarely on
the abrasive disk. Fiace the vacuum pickup nozzle
in position and adjust it to a distance of I1.2
in. (1 mm) above the abrasive disk.
7.3 Set the counter to “zero” and set the suction
regulator to approximately 50 points on the
dial. The setting may be increased to 90 if more
effective removal of the abradings appears nec-
-rY.
7.4 Start the vacuum pickup and then the
turntable of the abrader. Resurface the wheels by
running them 50 cycles against the resurfacing
medium.
NOTE 5-The wheels should be resurfaced in this
manner before testing each specimen and after every
500 cycles.
8. Conditioning -
8.1 Cure the coated panel under conditions of
humidity and temperature as agreed upon between
purchaser and seller.
8.2 Unless otherwise agreed upon between
purchaser and seller, condition the coated panel
for at least 24 h at 23 2 2°C and 50 k 5 % relative
humidity. Conduct the test in the same environment
or immediately on removal therefrom.
9. Procedure
9.1 Weigh the test specimen to the nearest 0.1
mg and record this weight, if either the wear
index or the weight loss is to be reported.
9.2 Measure the coating thickness of the test
specimen in several locations along the path to
be abraded.
9.3 Mount the test specimen on the turntable.
Place the abrading heads on the test film and the
vacuum pickup nozzle in position as outlined in
7.2. Set the counter and suction regulator as
outlined in 7.3.
9.4 Start the vacuum pickup and then the
turntable of the abrader. Subject the test specimen
to abrasion for the specified number of
cycles or until wear through of the coating is
observed. In determining the point of wear
through, stop the instrument at intervals for examination
of the test specimen.
9.5 Remove any loose abradings remaining
on the test specimen by light brushing. Reweigh
the test specimen.
9.6 Repeat 9.1 to 9.5 on at least one additional
test specimen of the material under test.
10. Calculation
10.1 Wear Index-Compute the wear index
of a test specimen as follows:
(A- B) lo00
wear index =
C
where:
A = weight of test specimen before abrasion,
m&
B = weight of test specimen after abrasion, mg,
and
C = number of cycles of abrasion recorded.
NOTE 6-111 calculating wear index it may be advisable
to discard the last 200 cycles because the results
may be afectedby abrasion of the exposed substrate.
362

10.2 Weight Loss-Compute weight loss of
the test specimen as follows:
weight loss = A - B
where:
A = weight of test specimen before abrasion,
mg, and
B = weight of test specimen after abrasion, mg.
10.3 Wear Cycles Per Mil-Compute the
wear cycles per mil of the test specimen as follows:
wear cycles per mil = DIT
where:
D = number of cycles of abrasion required to
wear coating through to substrate and
T = thickness of coating, mils (0.001 in.) (to
one decimal place).
NOTE 7-In calculating the wear cycles, it is advisable
to discard the first and last readings because the
first may be affected by an uneven surface and the last
by abrasion of parts of the substrate.
11. Report
1 1.1 Report the following for each test material:
1 1.1.1 Temperature and humidity during
conditioning and at the time of testing,
11.1.2 Thickness of coating when wear cycles
are specified,
1 I . 1.3 Kind of calibrase abrasive wheels used,
11.1.4 Load applied to the abrasive wheels,
11.1.5 Number of wear cycles recorded for
each test specimen,
11.1.6 Wear index, weight loss, or wear cycles
per mil for each test specimen, and
11.1.7 Mean and range of the abrasion resistance
values of the replicate coated panels.
I 2. hecision’
12.1 On the basis of an interlaboratory test of
this test method in which operators in five laboratories
tested four coatings having a broad range
of abrasion resistance, the within-laboratory coefficients
of variation and between-laboratories
coefficients of variation were found to be those
in Table 1. Based upon these coefficients, the
following criteria should be used for judging the
acceptability of results at the 95 % confidence
level:
12.1.1 Repeatability-Two results by the
same operator should be considered suspect if
they differ by more than the maximum allowable
difference values shown in Table 1.
12.1.2 Reproducibility-Two results obtained
by operators in different laboratories should be
considered suspect if they differ by more than
the maximum allowable difference values shown
in Table 1.
NOTE 8-When this test method is used to rank a
series of coatings by magnitude of abrasion resistance,
the precision is significantly better than shwn in Table
1. In the interlaboratory study for evaluating precision,
all laboratories ranked the coatings in the same order
of abrasion resistance.
’ Supporting data are available on loan from ASTM Headquarters.
Request RR: WI-1037.
Weight loss at 500 cycles
Weight loss at lo00 cycles
Wear index at 500 cycles
Wear index at IO00 cycles
Cycles mr mil
TABLE I
Precision of Taber Abrasion Values
Within Laboratory
Between Laboratories
Maximum Al-
Maximum Al-
Coeficient Of lowable Differ- Coefficient Of lowable Differ-
Variation, %
Variation, %
ence, %
ence, %
12 48
10 46
13 52
10 46
13 44
36 I05
30 90
36 106
30 92
31 92
The American Socii~~.v,/i~r Tmting and Materials takes no position respecting the validity ofany patent rights asserted in connection
with any item mentioned in this standard. Users ofthis standard are expressly advised that determination ofthe validity of any such
patent rights. and the risk of infringement qf such rights, are entirely their own responsibility.
This standard i.s subjivt to revision al any time by the responsible technical committee and must be reviewed everyjive years and
(1 not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should he addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
ri~.vponsihle lechnical committee, which you may attend. I$ you fie1 that your comments have not received a fair hearing you should
make your views known to tht ASTM Committee on Standard.7, 1916 Race SI., Philadelphia. Pa. 19103.
363

ab
Designation: D 4144 - 82
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Method for
ESTIMATING PACKAGE STABILITY OF COATINGS FOR
ULTRAVIOLET CURING'
This standard is issued under the fixed designation D 4144; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. scope 4. Apparatus
1.1 This method covers procedures for test- 4.1 Oven, maintained at 60 f 2°C.
ing the package stability of coatings intended 4.2 Glass Jars, wide-mouth, 4-oz (115-mL),
to be cured by ultraviolet radiation. One pro- with 38-mm closures.
cedure is given for clear coatings and another 4.3 Cans, lined, 4-oz (115-mL), friction top,
for opaque fillers.
with lids.
4.4 Spheres, glass or porcelain, 7 to IO-"
2. Summary of Method
diameter.
2.1 Specimens are placed in several containers,
some of which are subjected to an
elevated temperature while others are stored at
room temperature. At specified intervals a specimen
is checked for evidence of gelling. Clear
materials are held in glass containers so they
can be examined visually without opening to
prevent contact with air which might inhibit
polymerization. Opaque materials are checked
by opening one can, probing the contents with
a spatula to determine the extent of any polymerization,
and then discarding that specimen.
3. Significance and Use
3.1 Coatings intended to be cured by ultraviolet
radiation, especially those involving free
radical chemistry, tend to polymerize during
storage. It is of interest to determine how well
a formulation resists this effect. Many factors
influence the storage stability nf a cnapositien.
The procedures described here are intended to
improve the precision of determining this property.
Because the effects of resins, monomers,
photoinitiators, synergists, stabilizers, or pigments
can alter the relation between elevated
and room temperature stabilities, any correlation
of performance at two different temperatures
is possible only with a given formulation
and, therefore, is useful only for quality control.
5. Procedure
5.1 Clear Coatings:
5.1.1 Fill three 4-oz (115-mL) wide-mouth
jars to ?4 in. (6 mm) from the top. Add a small
glass or porcelain sphere to each container and
put the lids on tightly.
5.1,l. 1 The amount of head space in a jar or
can is critical because the volume of air in
contact with the sample has an effect on the
rate of polymerization. The stability is also
related to the ratio of the area of liquid-air
interface to the volume of liquid.
5.1.2 Put two jars in an oven at 60 & 2°C.
Retain the third at ambient temperature, 25 rfr
2"C, and in the dark.
5.1.3 Check an oven jar daily but do not
open or invert. Rather, tip slightly, no more
than 30", to determine the extent of polymerizatioii
tij: noting the mobiiiiy of the sphere.
When gelling is noticed, check the second jar
to confirm.
5.1.4 Record the duration of the test in days.
' This method is under the jurisdiction of ASTM Committee
D-1 on Paint and Related Coatings and Materials and
is the direct responsibility of Subcommittee D01.52 on Factory-Coated
Wood Products.
Current edition approved June 25, 1982. Published September
1982.
364

Indicate the last day the sphere is mobile followed
by the first day it is immobile, and if the
days are not consecutive, why the interval occurred.
5.1.5 Check the jar stored at room temperature
every week but do not open or invert. Tip
slightly, no more than 30°, to determine if the
sphere is immobile.
5.1.6 Record the number of weeks not gelled
followed by the first week the sphere is immobile.
5.2 Pigmented (Opaque) Coatings:
5.2.1 Fill twelve 4-02 (1 15-mL) lined cans to
?4 in. (6 mm) from the top and put the lids on
tightly.
5.2.1.1 See 5.1.1.1.
5.2.2 Put six of the cans in an oven at 60 f
2°C. Retain six cans at ambient temperature,
25 f 2°C.
5.2.3 After one day remove one can from the
oven, open, and probe to the bottom to determine
if gelling is beginning. Discard the can
after the test. Check one of the remaining cans
on the 2nd, 4th, 8th, 16th, and 32nd days and
discard after testing. By starting on a Monday
all the testing will fall on normal working days.
5.2.4 Record the condition of the specimen
each day tested, indicating the fractional
amount of any gelled material present.
5.2.5 After one week check one of the cans
held at ambient temperature by opening and
probing to the bottom to determine if gelling is
D 4144
beginning. Discard the can after the test. Check
one of the remaining cans after 2,4, 8, 16, and
32 weeks.
5.2.6 Record the condition of the specimen
after each test and indicate the fractional
amount of any gelled material present.
6. Report
6.1 Report whether the material was clear or
pigmented and the length of time it was stable
as indicated by the occurrence of gelation at
both ambient and elevated temperatures. Report
the age of the material when the test began,
if it is known.
7. Precision
7.1 Clear Coatings:
7.1.1 At the elevated temperature, four of
five cooperators reported a clear coating with-'
out inhibitor gelled on the 8th or 9th day. Four
of five cooperators reported a coating with
inhibitor gelled on the 32nd day; the fifth reported
gelation on the 18th day.
7.1.2 At room temperature four of four cooperators
reported no gelling at 32 weeks, with
or without inhibitor.
7.2 Pigmented Coatings:
7.2.1 At the elevated temperature six of six
cooperators reported a filler gelled at 8 days.
7.2.2 At room temperature four of four cooperators
reported various degrees of gelation
after 32 weeks.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in
connection with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity
of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyfive years
and ifnot revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsibletechnical committee, which you may attend. Ifyou feel that your comments have not received a fair hearingyou should
makeyour views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, Pa. 19103.
365

!Sib
Designation: D 421 2 - 82
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
VISCOSITY BY DIP-TYPE VISCOSITY CUPS'
This standard is issued under the fixed designation D 4212; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reapproval. A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method describes the determination
of viscosity of paints, varnishes, lacquers,
and related liquid materials by dip-type
viscosity cups. Due to poor reproducibility, this
method is recommended for viscosity control
work within one plant or laboratory and should
not be used to check compliance with specifications.
2. Applicable Document
2.1 ASTM Standard
E 1 Specification for ASTM Thermometer2
3 Summary of Method
3.1 The cup is completely immersed in the
material to be tested and then withdrawn so
that the time of flow of the material, through
a hole in the base of the cup, can be measured.
4. Significance and Use
4.1 This type of cup is used to measure
viscosity because it is easy to use, robust, and
may be used in tanks and reactors.
4.2 There are other types of apparatus for
measuring viscosity in the laboratory that provide
better precision and accuracy.
5. Apparatus
5.1 Zahn Viscosity Cup"-No. 1 through No.
5 Zahn viscosity cups made of corrosion- and
solvent-resistant materials. The capacity of the
cup is nominally 44 mL, but may vary from 43
to 48 mL, depending on the manufacturer. A
diagram of a Zahn cup is given in Fig. 1. The
dimensions, including orifices, are only approximate
because the cups are not made to one
given specification. Each manufacturer produces
a different cup and considerable variation
between batches from a given manufac-
turer has been noted in the past. This is a major
reason why Zahn cups should not be referred
to in specifications between producer and user.
5.1.1 Nominal Zahn cup orifice diameters
are listed in Table X1.l. Cup No. 1 with the
smallest orifice is used for determining the
viscosity of thin bodied materials. Cup No. 2,
for use with clears, lacquers, and enamels; Cups
3 and 4 for heavier bodied materials.
5.2 Shell Viscosity Cup4-S- 1 through S-6
Shell viscosity cups made of stainless steel with
a capacity of 23 mL and a 1-in. (25-mm) long
capillary in the bottom and conforming to the
dimensions shown in Fig. 2.
5.2.1 Nominal Shell cup orifice diameters
are listed in Table X 1.1. Cups 1 through 2% are
recommended for use with reduced rotogravure
inks; Nos. 3 through 4 for industrial enamels,
lacquers, flexographic, and gravure inks; and
Nos. 5 and 6 for heavy materials.
5.3 Calibration Thermometer-ASTM Saybolt
Viscosity Thermometer 17F having a range
of 66 to 80°F and subdivisions of 0.2"F or
17°C having a range of 19 to 27°C and subdivisions
of O.l"C, both conforming to the requirements
of Specification E 1.
'This test method is under the jurisdiction of ASTM
Committee D- 1 on Paint and Related Coatings and Materials
and is the direct responsibility of Subcommittee D01.24 on
Physical Properties of Liquid Paints and Paint Materials.
Current edition approved Nov. 26, 1982. Published Janua
1982.
'1982 Annual Book o$ASTM Srondards, Parts 25 and 44.
:' Zahn cups may be obtained from Paul N. Gardner Co.,
2 18-D Commercial Blvd/Suite 204, Lauderdale-by-the Sea,
Fla. 33308; General Electric Co.. Instrument Products Div.,
40 Federal St., Lynn. Mass. 01910 and Pacific ScientificCo.,
Gardner/Neotec Instrument Div.. 243 I Linden Lane, Silver
Sp$ng. Md. 20910.
Shell cups may be obtained from the Norcross Corporation.
255 Newtonville Ave., Newton, Mass. 02158.
366

D 4212
5.3.1 For general operations, any thermometer
with 1 "C subdivisions may be used.
5.4 Timer-Any timing device may be used
provided that the readings can be taken with a
discrimination of 0.2 s or better.
6. Test Materials
6.1 The material to be tested should be visibly
homogeneous and free from any foreign
material or air bubbles.
7. Temperature of Testing
7.1 Measurements should be made at 77°F
(25°C) unless otherwise specified. Temperature
drift during the test should be kept to a minimum.
7.2 A temperature correction curve may be
constructed for each liquid by plotting viscosity
(seconds) against temperature over the expected
temperature range. With this curve, a
viscosity determined at one measured temperature
may be converted quickly to a viscosity
at another temperature.
8. Calibration
8.1 Cups should be checked in accordance
with the procedure described in the Appendix.
The frequency of this check depends upon the
amount of use and care that the individual cup
receives.
9. Procedure
9.1 Choose the proper cup so that the time
of efflux will be between 20 and 80 s. See Table
1.
9.2 Immerse the cup in the container, which
may be a can or beaker, but is more likely to
be a thinning or mixing tank or even a resin
reactor. Stir or agitate the fluid well to give
uniform temperature and density. Allow the
cup to remain in the fluid for at least 5 min. To
standardize conditions, control the temperature
and construct a temperature correction curve
as described above.
9.3 Lift the cup vertically out of the material
in a quick steady motion. As the top edge of
the cup breaks the surface, start the timer.
During the time of flow hold the cup vertically
no more than six inches above the level of the
liquid. Stop the timer at the first definite break
in the stream at the base of the cup. The efflux
time in seconds constitutes the viscosity. It is
common to make only a single measurement,
but for greater precision and accuracy the nl
of two measurements should be taken.
10. Care of the Cup
10.1 Following each determination, clean
the cup with a suitable solvent and a soft brush.
Use no metal tools in contact with the instrument
as nicks or wear of the drilled orifice
affect the accuracy of the cup.
11. Report
11.1 Report the efflux time to the nearest 0.5
s for Zahn or Shell Cup No. - manufactured
by
and whether the result is from
a single measurement or the mean of two measurements.
12. Precision
12.1 Dip cups are not precision instruments
and should be used for viscosity control at a
given location only. However, if comparisons
are made, cups from the same manufacturer
must be used. The following criteria can be
used for judging the acceptability of results at
the 95 % confidence level:
12.1.1 Zahn Cups-Precision was determined
on the basis of an interlaboratory test in
which six laboratories used new Zahn cups (all
from the same manufacturer) to test eight
paints covering a broad range of viscosities.
12.1.1.1 Repeatability-Two results obtained
by the same operator should be considered
suspect if they differ by more than 1 1 % of
their mean value.
12.1.1.2 Reproducibility-Two results, each
the mean of two measurements, obtained by
operators in different laboratories should be
considered suspect if they differ by more than
33 % of their mean value.
12.1.2 Shell Cups-Precision was determined
on the basis of an interlaboratory test in
which four iaboraiories tested seveii paiiiis COYering
a broad range of viscosities.
12.1.2.1 Repeatability-Two results obtained
by the same operator should be considered
suspect if they differ by more than 9 % of
their mean value.
12.1.2.2 Reproducibility-Two results, each
the mean of two measurements, obtained by
operators in different laboratories should be
considered suspect if they differ by more than
18 % of their mean value.
367

TABLE 1 Approximate Kinematic Viscosities at 77°F
(2S"C), cst
CUP
Number
Zahn Cup
Shell Cup
2os~
80 s 20 s 80 s
...
1 60 1.6 15
2
2%
20
...
230
...
9
16
43
71
3 150 850 27 I20
3% ... ... 40 170
4 220 1100 65 270
5 460 I 840 I25 515
...
6 ... 320 1300
A Zahn Cup No. 1 does not permit a 20-s flow time.
, 1 1!.6
i.
(295)
13.6
(347)
c.4
3 (33)
2.4
(61)
4'x
ORIFICE
0.7(17) 1
SPHERICAL R
(35)
DIMENSIONS IN INCHES
C MILLIMETERS IN PARENTHESES)
NOTE-Dimensions are approximate only and may vary with the manufacturer and from batch to batch.
FIG. 1 ZahnCup
368

D4212
.13 (3.3) DIA x%2 (0.8) DEEP
I
FLAT BOTTOMED HOLE
I
DIMENSIONS IN INCHES
(MILLIMETERS IN PARENTHESES)
(61.9)
(34.9)
1.25 DIA
(31.8 )
1. 1.375
=/_ 1.000 j L 1 6 1 SEE TABLE XI.1
(34.9) (25.4) (1.6)
FIG. 2 Shellcup
369

D4212
APPENDIX
XI. CHECKING PROCEDURE
X1.1 The orifice of the cup is subject to wear with
use and cleaning. A small change in the diameter of
the orifice becomes significant in the results obtained
with this type of viscosity-measuring device.
X 1.2 Select the appropriate liquid viscosity standard
for the cup to be ~hecked.~ (Table X1.l).
X1.3 Bring the cup and the liquid viscosity standard
to a constant temperature as close as possible to
77.0°F (25.0"C). Determine the time of efflux to the
nearest 0.2 s using the procedure detailed in Section
9. Record the temperature. If it is not 77"F, correct
the viscosity of the standard oil to the actual temperature.
X1.4 Convert the time of flow in seconds to kinematic
viscosity as follows:
where:
V = k(t - C)
V = kinematic viscosity, cSt,
t = eMux time, s, and,
k, c = appropriate constants from Table X1.2.
X1.5 Calculate the correction factor b dividing
the true kinematic viscosity of the standar B oil by the
kinematic viscosity calculated from the efflux time.
This factor may then be used to correct viscosity
readings taken with the cup. The product of the
factor and an efflux time gives a corrected viscosity
in Zahn or Shell seconds.
Certified kinematic viscosity standards (I-pt samples
only) are available from the Cannon Instrument Co., P.O.
Box 16, State College, Pa. 16801. For particular oils applicable
for use with each cup refer to Table X1.l:Oils available
from other sources, having known kinematic viscosities, may
also be used.
TABLE X1.l
Viscosity Standards Recommended for Calibrating DipType Viscosity Cups
Cup Number
Nominal DiameterA
of Orifice, Range: cSt Standard Oil Number"
Approximate Oil Viscosity"
@ 77F (25C),
mm
cst
Zahn
I 2.0 20 to 90 S20, S60 35,120
2 2.7 50 to 250 S60 I20
3 3.8 90 to 800 S60, S200 120,480
4 4.3 150 to 1200 s200 480
5 5.3 280 to 1700 S200, S600 480, 1600
Shell
1 1.8 4 to 20 S6 9
2 2.4 6 to 60 S6, S20 9, 35
2% 2.7 16 to 90 s20 35
3 3.1 20 to 150 S20, S60 35, 120
3% 3.5 40 to 180 S60 120
4 3.8 50 to 360 S60 120
5 4.6 70 to 740 S60, S200
120,480
6 5.8 170 to 1600 s200 480
A Information based on literature of cup manufacturers
Range within which the viscosity formula is valid.
See Footnote 5.
Exact viscosity is supplied with each oil standard.
370

D4212
TABLE X1.2
Constants for Use With Viscosity
FormulaA
Cup Number k C
Zahn I
Zahn 2
Zahn 3
Zahn 4
Zahn 5
Shell 1
Shell 2
Shell 2%
Shell 3
Shell 3%
Shell 4
Shell 5
Shell 6
1.1
3.5
11.7
14.8
23
0.226
0.576
0.925
1.51
2.17
3.45
6.5
16.2
29
14
7.5
5
0
13
5
3
2
1.5
1
1
0.5
A Zahn and Shell cup constants from T. C. Patton, Paint
Flow and Pigment Dispersion, second edition, John Wiley and
Sons, New York, 1979, p. 82.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in
connection with any item meniioned in this standard. Users of this standard are express4 advised that determination of the validiiy
of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical commiitee and must be reviewed everypve years
and if not revised, eiiher reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
makeyour views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, Pa. 19103.
37 1

Designation: D 4361 - 84'*
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St, Philadelphia, Pa 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition
Standard Test Method for
APPARENT TACK OF PRINTING INKS BY THE
INKOMETER'
This standard is issued under the fixed designation D436 I; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (c) indicates an editorial change since the last revision or reapproval.
-___
__
" NOTE-Paragraphs 6.2 and 13.2 were editorially changed in November 1985.
" Nom-Paragraph 13.2 was editorially corrected in November 1986.
1. Scope
1.1 This test method describes the use of the
Inkometer for determining the apparent tack of
printing inks using mechanically or electronically
controlled models.
I .2 This test method is applicable to inks that
are essentially nonvolatile at 73.5"F (23°C).
1.3 Ttiis standard may involve. hazardoiis matcrials,
operations, and cxiiripmcnt. This standard
docs not pitrport to addrcm all ql'thc. safety proh-
1om.s associated with its i ~sc. It is the) re~sponsibility
of whocw~r iisc~s this standard to cvnsuli and
establish appropriate. safety and health practics
and dcvcv-minc. the applicability t$regztlatory limitations
prior to use. Specific precautionary statements
are given in Section 7.
2. Summary of Method
2.1 Two kinds of Inkometers may be used:
mechanical and electronic models. A measured
quantity ofthe sample is spread on the Inkometer
rollers and distributed at a given speed(s) for a
given period(s) of time, at controlled water bath
and ambient temperature conditions. At the end
of the test period(s) the apparent tack reading(s)
is(are! determined with either the ba!ance beam.
direct reading attachment, or recorder on the
mechanical Inkometer, or the digital readout or
recorder on the electronic Inkometer.
2.2 The procedure given in this test method is
designed to give a single value for apparent tack
at a given set of conditions and includes a procedure
for periodic calibration of the Inkometer.
3. Description of Terms Specific to This Standard
3.1 tack-a function of the force required to
split a fluid ink film between two rapidly separating
surfaces: it is not a property of a fluid but
of the system: it is not a fixed number, but varies
with test conditions. These include: Inkometer
water bath temperature (that is, roller temperature),
ambient temperature, speed at which the
apparent tack reading is measured. distribution
time at which the apparent tack reading is measured,
quantity of ink applied to the Inkometer.
calibration and zero accuracy of the Inkometer.
mechanical integrity of the Inkometer. and electronic
integrity of electronic models, interaction
of ink with roller covering, type of solvent used
for wash-up, and interaction with roller covering,
long and short term history of the Inkometer
rollers, and their condition.
3.2 appartnt tack-a tack reading obtained at
a specific set of conditions.
4. Significance and Use
4.1 Apparent tack is a relative number that is
useful in quality control. development. and research.
While it does not completely determine
the performance of a printing ink, it is a significant
parameter of an ink. Results from a given
lnkometer must be repeatable on a day-to-day
basis, in order to be significant (see Annex). In
order to obtain such results, all of the test conditions
listed in 3.1 must be controlled. Two or
more lnkometers may not produce identical apparent
tack readings, but if each gives repeatable
results, they may be mathematically correlated
so that results can be compared.
' This lest method is under the jurisdiction 31' ASTM Committee
D-l on Paint and Related Coatings and is the direct
responsibility of Sutxommittee Dol .56 on Printing Inks.
Current edition approved April 27. 1984. Published October
I 984.
372

D4361
5. Interferences
5.1 Inkometer “Squeal”-A high pitched
whine or squeal may be noted when running high
tack inks or at high rotating speeds, orboth.
Inkometer squeal may result in instability of the
balance beam or direct reading attachment of the
mechanical Inkometer, or fluctuation of the digital
readout of the electronic Inkometer, making
definite readings dificult.
6. Apparatus
6.1 Mechanical Inkometer,’ Model B-45 or C-
46, with the option of a direct reading attachment’
or recorder,2 or
6. I. 1 Electronic Inkometer,’ Model 10 I A or
10 I B, with the option of a recorder.’
6.2 Inkometer Rollers,’ one set with a total
surface area of 166 in.’ (1069 cm’), well brokenin
(see Annex) for each major ink system to be
evaluated.
6.3 Suitable Pipette, as an Inkometer pipette,2
1.32 mL volume, or ink mi~ropipette,~ variable
volume, 2-mL capacity, accurate to 0.01 mL.
6.4 Slopwatch or Timer, accurate to 1 s.
6.5 Ink Knife, small, free from nicks and
rough edges.
6.6 Munufucturer’s Current for the
specific model Inkometer.
6.7 Man icfact urer ’s Culibrat ion A ppurur
for the specific model Inkometer.
7. Precautions
7.1 Never allow inks to dry nor oxidative or
reactive inks to complete their chemical reaction
on the Inkometer rollers.
7.2 Take care not to damage the Inkometer
rolls during the cleaning process (see 14.1.1.1) or
by leaving the rolls in contact when the instrument
is not in use.
7.3 Never touch the zero button except during
the ca!ibratiol? PrOrPSs (see Note 7).
8. Reagents and Materials
8.1 Wash-UpSolvent, compatible with the ink
system, fast evaporating, and having minimal
effect on the rollers; it should be acceptable environmentally.
Hydrocarbon solvents with an initial
boiling range of 250 to 350°F (1 20 to 177”C),
a final boiling range of 300 to 400°F (150 to
205°C). a Kauri-Butanol value of 30 to 40 and
less than 1 76 benzene content are appropriate
for many sheet-fed and heat-set inks. Specific
solvents may be required for unique ink systems.
8.2 Rags or Wipers, clean, soft, absorbent,
lint-free.
9. Sampling
9.1 The sample shall be carefully selected to
be representative ofthe entire lot being evaluated;
it must be free of skin and other contamination.
A minimum of 3 mL of ink, sufficient for two
specimens, is required for testing. The ink shall
be kept in a closed clean container with skin
paper.
10. Conditioning
IO. 1 Conduct the tests in a temperature controlled
draft-free environment, preferably 73.5 &
3.5”F (23 & 2°C). If the ink system being tested
may be moisture sensitive, or ink misting or
flying may be a factor, precise humidity control
is necessary.
10.2 The Inkometer rollers must be well broken-in
prior to use (see Annex).
10.3 Prior to calibration of the Inkometer, or
the first test of the day, condition the rollers by
running approximately 1.0 to 1.5 mL of an ink
of the system being tested, at the specified test
speed, for 5 to 10 min. Wash up, as in 14.1.
11. Preparation and Calibration of Apparatus
1 1.1 Calibrate the apparatus periodically, as
needed.
1 I .2 Mechanicul Inkometer:
1 1.2. I Set the Inkometer water bath temperature
to 90.0 & 0.2”F (32.2 f 0.1”C). Activate
the water bath and allow water to circulate
through the system.
11.2.2 Engage the measuring and vibrator
rollers against the brass roller. Set the speed at
400 rpm: turn on the Inkometer. Allow the Inkometer
to run for approximately 30 min to
equlibrate the instrument temperature.
11.2.3 Stop the lnkometer; set the Inkometer
at the specified test speed. Using the manufacturer’s
manual and calibration apparatus, zero
and calibrate the Inkometer (and direct reading
attachment or recorder, if they are to be used) at
the specified test speed.
1 1.3 Electronic lnkometer:
* Available from Thwing-Alben Instrument Company.
10960 Dutton Rd.. Philadelphia. PA. 191 54.
Precision pipette available from Techno-Graphic Instruments.
5321 Bentwood Drive, San Angelo. TX 76901. or Pantone.
Inc., 55 Knickerbocker Road. Moonachie. NJ 07074.
373

D 4361
11.3.1 Set the lnkometer water bath temperature
to 90.0 & 0.2"F (32.2 f 0.1"C). Activate
the water bath and allow water to circulate
through the system.
11.3.2 Engage the measuring and vibrator
rollersagainst the brass roller. Turn on the power,
drive, and temperature switches; turn on the low
speed switch. Allow the Inkometer to run for
approximately 30 min to equilibrate the instrument
temperature.
11.3.3 Turn on the high speed switch, set the
Inkometer at the calibration speed, lo00 rpm.
Using the manufacturer's manual and calibration
apparatus, zero and calibrate the Inkometer (and
recorder, if it is to be used) at the calibration
speed, 1000 rpm.
12. Test Specimen
12. I Remove only enough of the sample from
the container for one test; close or reseal the
container.
12.2 Work a minimum of 2 mL of the sample
on a clean glass plate, with the ink knife: do not
aerate the material during this process.
12.3 Fill the pipette with 1.32 mL of the
worked sample by forcing the ink into the cylinder
with the ink knife, while slowly pulling back
the ram. When the pipette contains 1.32 mL of
ink, scrape the excess ink off the surface of the
pipette.
Nori: 1-1.32 mL of ink gives a 12.3 pm ink film
thickness when distributed on the lnkometer roller
system: smaller specimens (For example, 0.50 to 1.00
mL) may be appropriate if a thinner ink film is desired.
13. Procedure
13.1 Control the water bath to 90.0 +. 02°F
(32.2 f 0.I"C) during all tests (see Annex).
13.2 Set the lnkometer at the specified test
speed and run. If the dry reading differs from
zero by more than k 5 g-m, reclean the rollers in
accordance with i 4. i or recalibrate in accordance
with Section I 1.
Now 2-Commonly specified test speeds for sheetfed
inks are 800 or 1200 rpm and for web-fed inks.
I200 to 2000 rpm.
NOTI; 3-Frequent large zero adjustments should be
considered suspect.
13.3 'Stop the Inkometer and transfer the ink
specimen from the pipette to the middle 5 in. of
the vibrator roller, spreading it evenly. Wipe any
remaining ink from the pipette onto the same
roller. in such a manner as to achieve the most
even distribution.
13.4 Mechanical Inkometer:
13.4.1 Distribute the ink initially by manually
turning the motor coupling approximately ten
revolutions.
13.4.2 Set the Inkometer speed at 400 rpm,
start the Inkometer and the stopwatch simultaneously,
and distribute the ink at 400 rpm for a
minimum of 5 s. Stop th5 lnkometer but do not
stop the stopwatch.
13.4.3 Quickly reset the speed to the specified
test speed, immediately restart the inkometer,
and run the ink at the test speed.
13.4.4 Record the apparent tack reading from
the balance beam, direct reading attachment, or
recorder after 60 s of running the ink at the test
speed. In some instances it may be desirable to
run the ink until the apparent tack begins to
decrease.
13.4.5 When the direct reading attachment or
the recorder, or both, are not being used, measure
the apparent tack by disengaging the balance
beam, moving the sliding weight until the beam
is continuously in balance, and taking the reading
on the balance beam scale at the left of the sliding
weight, using the scale alignment cutout to facilitate
reading. Parallax may be minimized by
aligning the zero indicator and the zero line on
the balance beam with a reflective rear surface
on the beam stop (see Annex).
13.4.6 Disengage the balance beam only when
taking a reading.
I 3.5 Elc~tronic Inko1nc.tc.r:
13.5.1 Distribute the ink initially by manually
turning the brass roller ten revolutions.
No11 4-Turn the brass roller by placing the fingertips
against 1he sides of the roller: do not touch the
ink contact surface.
13.5.2 Set the Inkometer high speed at the
specified lest speed: start the Inkometer at low
speed (125 ipiiij arid the sropwarcn simuitaneously.
and distribute the ink at 125 rpm for a
minimum of 5 s.
13.5.3 Switch the lnkometer to high speed and
run the ink at the test speed.
13.5.4 Record the apparent tack reading from
the digital readout or recorder after 60 s of running
the ink at the test speed. In some instances,
it may be desirable to run the ink until the
apparent tack begins to decrease.
NOTE 5-A single apparent tack reading often does
not give a truly representative picture of the ink; a
374

D 4361
continuous plot for a longer period of time may significantly
increase the resulting information. If a continuous
plot or additional apparent tack readings are
desired, the Inkometer speed may be held constant,
while apparent tack readings are taken at uniform time
intervals or the speed may be vaned stepwise, at uniform
time intervals, with apparent tack readings at each
Speed.
13.6 Stop the Inkometer and clean as in 14.1.
13.7 Measure the apparent tack reading of the
ink under test twice; consecutive readings should
agree within the repeatability given in 16.2.
NOTE 6-The tendency of some inks to “mist” or
“fly”, particularly at high Inkometer speeds, may cause
a significant change in the apparent tack reading, due
to the loss from the rollers.
14. Wash-up
14.1 Inkomeler:
14.1.1 With the Inkometer running at the lowest
speed, apply a small amount of wash-up
solvent to the rollers. Remove most of the ink
from the system by placing pads of the clean,
soft, absorbent lint-free rags or wipers firmly
against the brass roller. Repeat this procedure
with additional solvent and pads until the rollers
are free from ink. If any ink remains on the edges
of the rollers, remove very gently with a solventmoistened
rag. Allow the rollers to dry thoroughly
by running them in contact for a minimum
of 5 min or until all of the solvent has
evaporated.
14.1.1.1 Remove ink directly from the measuring
or vibrator rollers with extreme care. Undue
pressure will cause uneven wear of the rollers
and may place significant strain on the torsion
bar of the electronic Inkometer. Use extreme care
to ensure that the cleaning pad does not go
through the rol?er nip which may cause serious
mechanical problems.
14.1.2 Check the zero of the Inkometer at the
specified test speed; a discrepancy greater than +-
0.5 may indicate residual ink or solvent, or both,
on the rollers.
NOTE 7-The zero calibration and the zero reading
after the calibration are directly related to the condition
of the top roller; therefore, do not turn the zero button.
If zero cannot be reached, it is likely that more cleaning
of the rolls is needed. Remember that each time the
zero button is turned the scale shifts.
14.2 Pipette-Clean the pipette thoroughly
with the wash-up solvent and dry with a clean
rag.
15. Report
15.1 Report the following information:
15.1.1 Complete identification of the sample,
15.1.2 Apparatus used,
15.1.3 Water bath temperature,
15.1.4 Distribution time,
15.1.5 Speed,
15.1.6 Ambient temperature,
15.1.7 Any modifications to this test method,
15.1.8 Whether significant flying or misting of
the ink was observed,
15.1.9 Whether Inkometer squeal was noted
during the test,
15.1.10 Average apparent tack reading of the
determinations, and
15.1.1 1 Any additional apparent tack readings
determined at constant speed-constant time intervals
or varying speeds-constant time intervals.
16. Precision4
16.1 In an interlaboratory study of this test
method six ink batches with a broad range in
tack were measured for apparent tack ten times
at 1-min and 5-min intervals on mechanical
Inkometers in six laboratories and on electronic
Inkometers in eight laboratories. The withinlaboratory
and between-laboratories standard deviations
were found to be as shown in Table l.
Based on these standard deviations the following
criteria should be used for judging the acceptability
of results at the 95 ?& confidence level:
16.1.1 Repeatability-Two individual results
obtained by the same operator should be considered
suspect if they differ by more than the values
given in Table 2.
16.1.2 Reproducibility-Two results, each the
mean of two readings, obtained by operators in
different 1aborst:oiies sho.c;!d be cmsidered swpect
if they differ by more than the values given
in Table 2.
‘Supporting data are available from ASTM Headquarters.
Request RR: DO1 - 1039.
375

D 4361
TABLE I
Inkometer Tvoe _-
St8ndard Deviation of Apparent
Tack Readings a-nr‘
Within-laboratory
laboratories
Between-
I min 5 min I min 5 min
Mechanical 0.49 0.47 0.52 0.97
Electronic 0.31 0.46 0.67 1.26
” Gram-meter.
TABLE 2
lnkometer Type
Precision of Apparent Tack Readings, g-d
Repeatability
Reproducibility
1 min 5 min 1 min 5 min
Mechanical 2.0 I .8 2 .o 1.8
Electronic 1.2 1.8 2.6 5.0
” Gram-meter.
376

D4361
ANNEX
Mandatory Information
AI. INFORMATION CONCERNING INKOMETERS
Al.l Routine Maintenance of the lnkometer
A1.I.I Routine maintenance of the lnkometer is
extremely important to the mechanical integrity of the
instrument; see the manufacturer's current instruction
manual for the specific model.
A1.1.2 The measuring vibrator rollers of the Inkometer
may acquire a "glazed" or shiny appearance
with use, depending on the ink system and the washup
solvent. Thisglaze may result in a significantchange
in the apparent tack reading of an ink.
Al.2 Breaking-in the Inkometer Rollers
A 1.2. I New Inkometer measuring and vibrator rollers
may selectively absorb certain components of some
ink systems, up to a saturation point, at which point
they may be said to be "broken in." Until this selective
absorption is complete, tack determinations made with
these rollers may not be repeatable. Break in new rollers
using the following procedure:
A 1.2.1.1 Place the rollers on the Inkometer. Choose
as break-in inks those representative of the system that
will be evaluated on the rollers. Run approximately I .O
to 1.5 mL of the break-in inks for extended periods of
time, wash-up with the solvent to be used, reapply the
ink. run, wash-up etc.
NOTE A 1.1 -The wash-up is a significant part of the
break-in process.
A 1.2.1 .? Break-in time may vary from several hours
to several days. Reproducible apparent tack readings
on standard inks (see A I .5. I), over a period of several
days. indicate that the rolls are broken in; they ma)
then be put into routine use.
A1.2.2 A major change in ink systems may adversely
affect the lnkometer rollers. When a set of rollers
has been used for one ink system, and they are to be
used for another. this same break-in procedure should
be used. They may then no longer be suitable for the
original ink system.
A1.3 Temperature Control of the Inkometer Water
Bath
A I .3. I Extremely precise temperature control of the
lnkometer water bath is essential for repeatable appar-
ent tack readings.
A 1.3.2 The thermometer furnished with the mechanical
Inkometer, and the temperature gage of the
electronic lnkometer are accurate to +0.5"F (kO.3"C).
AI.3.2.1 It may be advantageous to use a Bomb
Calorimeter Thermometer ASTM 56F. 66.0 to 95.00"F,
with divisions of 0.05"F, or ASTM 56C, 19.00 to
35.Oo"C. with divisions of 0.02"C, in the Inkometer
water bath. The thermometer should be positioned in
such a manner that the bottom of the mercury bulb is
in line with the return inlet from the brass roller.
A I .3.3 The temperature-control system of the Inkometer
is capable of controlling the temperature inside
the brass roller within +0.5"F (+0.3"C).
A I .3.3.1 It may be advantageous, particularly if
high-tack inks are run for extended periods of time. or
if the lnkometer is in constant use, to augment the
temperature control system with a cold-water cooling
coil. A coiled length of '14 in. (6.3 mm) outside diameter
copper tubing may be placed in the water bath reservoir.
in the flow area away from the thermometer. The coil
is connected to a cold-water tap with a pressure regulator
and emptied into a sink or drain.
A 1.4 Parallax Minimization of Mechanical lnkometer
Balance-Beam Readings
A1.4.I Minimization of parallax is necessary for
repeatable apparent tack readings on the mechanical
Inkometer when the balance beam is used. It may be
useful to mount a small reflective surface on the beam
stop. behind the zero indicator and the halance beam.
The zero indicator and the zero line on the balaiice
beam are aligned in the reflective surface when an
apparent tack reading is being taken.
A1.S Standard Test Inks
Ai5.i ir map ix udui iu iicsrgiiaie uaz or iiioie
inks as standards. Inks that are stable and have a good
shelf life without a change in apparent tach reading (for
example. "tack rated" or "tack graded") are appropnate.
Daily apparent tack readings on these inks assures
that the Inkometer is in calibration and Serves as a
check on repeatability.
377

4Tb
Designation: D 4501 - 85
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
SHEAR STRENGTH OF ADHESIVE BONDS BETWEEN RIGID
SUBSTRATES BY THE BLOCK-SHEAR METHOD'
This standard is issued under the fixed designation D 4501; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method describes a procedure
and fixture used to determine shear strengths of
adhesives used to bond materials with moduli
higher than the modulus of the adhesive. The
size and shape of the specimens are variable
within the physical restraints of the fixture.
1.2 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health practices
and determine the applicability of regulatory limitations
prior to use.
2. Applicable Documents
2. I ASTM Standards:
D907 Definitions of Terms Relating to
Adhesives*
E 4 Practices for Verification of Testing Machine~.~
3. Summary of Method
3. I In this test method, blocks, plates, or disks
are bonded together, and the maximum force to
shear them apart is determined.
4. Significance and Use
4.1 This test method provides an estimate of
the shear strength of an adhesive on various
machinable and nonmachinable substrate materials.
It is particularly applicable for testing bonds
between ceramic, glass, magnet moldings, and
plastic parts with one flat face where machining
would be difficult or impractical.
5. Terminology
5.1 For definitions of technical terms pertaining
to adhesives, see Definitions D 907.
6. Apparatus
6.1 Testing Machine, with a capacity of not
less than 44 kN (10 000 Ibf) in tension. Testing
machine shall conform to the requirements of
Test Methods E 4.
6.2 Shearing Fixture-Perform the tests by
using a shearing fixture consisting of a holding
block and a shearing tool (Figs. I and 2). The
holding block can accomodate specimens up to
80 by 80 by I3 mm (3 by 3 by l/2 in.). For small
specimens as shown in Fig. 3B, an adapter plate
(Fig. 4) can be inserted into the holding block to
keep the shearing blade within its guides and to
locate the specimen under the clamp. The shearing
blade can accomodate specimens up to 30 by
30 X 13 mm ( 1 '/E by 1% by '/2 in.)."
7. Test Specimens
7.1 Test specimens can be any size within the
limits of the shearing fixture capacity, as given in
6.2. Suggested sizes are as follows:
7.1.1 Metal Blocks-25 by 25 by 6 mm (I by
l by '14 in.;.
-
' This test method is under the jurisdiction of ASTM Committee
D-14 on Adhesives and is the direct responsibility of
Subcommittee D14.40 on Adhesives for Plastics.
Current edition approved July 26, 1985. Published Novem-
ber 1985.
Annual Book VfASTM Standards, Vol 15.06.
'Annual Book ofASTMStandards. Vols 03.01,04.02,07.01,
and 08.03.
' Detailed drawings of the fixture are available from ASTM
Headquarters, 19 I6 Race St.. Philadelphia, PA 19103. Order
PCN 12-445010-25.
378

ab
7. I .2 ferrite or ceramic blocks-25 by I8 by
13 mm (1 by 3/4 by l/2 in.).
7. I .3 Wood or Plastic Blocks-25 by 25 by 13
mm (1 by 1 by l/2 in.).
7.1.4 Glass Plates-75 by 75 by I3 mm (3 by
3 by ‘12 in.).
7.2 Prepare the adhesive and apply in accordance
with the recommendations of the adhesive
manufacturer. Assemble the adhesive-coated
specimens, and bond them in accordance with
procedure under investigation.
No~~-Assemble the thrust surfaces, where the
straight-sided specimen contacts the fixture, so that they
are parallel to the fixture within 0.005 in./in. (0.005
mm/mm). Center round or shaped specimens within
the shear blade in such a way that a moment is not
applied to the specimen during shearing.
7.3 Remove any flash or fillets on the loaded
side prior to testing. Figure 3 shows typical specimens
after bonding.
7.4 Test at least five specimens for each test
condition.
8. Procedure
8. I Mount the shear fixture in the testing machine
with the holding block on top.
8.2 Place the specimen in the shearing fixture
in such a way that one of the adherends is engaged
by the holding block and the other by the
shearing tool (Fig. 5). Close the toggle clamp on
the rear of the holding block to keep the specimen
located against the back face (Fig. 6). (Some
adjustment of the pad may be necessary to accomodate
varying specimen thickness.)
8.3 Test the specimen using a crosshead speed
of 1.26 mm/min (0.05 in./min). Record the maximum
force sustained by the specimen.
9. Calculations
9.1 All bond strengths shall be expressed in
D 4501
megapascal (MPa) or pound-force per square
inch (psi).
10. Report
10.1 The report shall include the following
information:
10.1.1 Complete identification of the adhesive
tested, including type, source, and manufacturer’s
code numbers.
10. I .2 Complete identification of the adherends
used, including dimensions and orientation
in the test fixture, and the method of cleaning
and preparing the surfaces prior to bonding.
10.1.3 Quantitative application and bonding
conditions used.
10. I .4 Average thickness of adhesive layer
after formation of bond, within 0.2 mm, and the
means of measurement.
10.1.5 The temperature at which the test was
performed.
10.1.6 Number of specimens tested.
10.1.7 The maximum shear stress reached for
each specimen.
10.1.8 Average shear strength.
10.1.9 The nature of the failure: cohesion,
adhesion, or voids in the bondline. Report the
average percent of each.
11. Precision and Bias
11.1 No statement is made about either the
precision or the bias of this test method for
measuring shear stress. Round-robin testing has
not been conducted because fixtures are not
available. Data are being developed for a singlelaboratory
precision statement and another laboratory
is considering construction of a fixture
making a round-robin possible.
379

FIG. 1 ShearingTool
FIG. 2 HoklingBlock
380

.-
0
e
0
fi
E
s
Y
.-
6
E
4
h
a E
H
<
s
38 1

382

D4501
FIG. 5 Specimen Loaded in Shearing Fixture
383

D4501
SCREW
FIG. 6 Rear View of Fixture with Specimen Clamped in
Place
The American Societyfor Testing and Materials takes no position respecting the validity of any paient rights asserted in connection
with any item mentioned in this standard. Users ofthis standard are expressly advised that determination of the validity of any such
patent rights. and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject lo revision at any lime by the responsible technical committee and must be reviewed every jive years and
i/ not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you fie1 that your comments have not received a fair hearing you should
make your views known IO the ASTM Committee on Standards, 1916 Race St., Philadelphia, PA 19103.
384

Designation: E 96 - W2
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Methods for
WATER VAPOR TRANSMISSION OF MATERIALS‘
This standard is issued under the fixed designation E 96; the number immediately following the designation indicates the year of
original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e’ NOTE-Table I was editorially corrected in July 1984.
” NoTE-Editonal changes were made throughout this standard in May 1987.
1. scope
1.1 These test methods cover the determination
of water vapor transmission (WVT) of materials
through which the passage of water vapor
may be of importance, such as paper, plastic
films, other sheet materials, fiberboards, gypsum
and plaster products, wood products, and plastics.
The test methods are limited to specimens
not over 1’14 in. (32 mm) in thickness except as
provided in Section 9. Two basic methods, the
Desiccant Method and the Water Method, are
provided for the measurement of permeance, and
two variations include service conditions with
one side wetted and service conditions with low
humidity on one side and high humidity on the
other. Agreement should not be expected between
results obtained by different methods.
That method should be selected which more
nearly approaches the conditions of use.
1.2 The values stated in inch-pound units are
to be regarded as the standard. Metric inchpound
conversion factors for WVT, permeance,
and permeability are stated in Table 1. All conversions
of mm Hg to Pa are made at a temperature
of 0°C.
! -3 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health practices
and determine the applicability of regulatory limitations
prior to use.
2. Referenced Documents
2.1 ASTM Standards:
C 168 Definitions of Terms Relating to Thermal
Insulating Materials*
C677 Recommended Practice for Use of a
Standard Reference Sheet for the Measurement
of the Time-Averaged Vapor Pressure
in a Controlled Humidity Space’
D449 Specification for Asphalt Used in
Dampproofing and Waterproofing3
D2301 Specification for Vinyl Chloride Plastic
Pressure-Sensitive Electrical Insulating
Tape4
3. Terminology
3.1 Definitions of terms used in this standard
will be found in Definitions C 168, from which
the following are quoted:
“water vapor permeability-the time rate of
water vapor transmission through unit area of
flat material of unit thickness induced by unit
vapor pressure difference between two specific
surfaces, under specified temperature and humidity
conditions.”
NOTE-Permeability is a property of a material, but
the permeability of a body that performs like a material
may be used. Permeability is the arithmetic product of
permeance and thickness.
“water vapor permeunce-the time rate of water
vapor transmission through unit area of flat
‘These test methods are under the jurisdiction of ASTM
Committee C-16 on Thermal Insulation and are the direct
responsibility of Subcommittee C16.33 on Thermal Insulation
Finishes and Vapor Transmission.
Current edition approved Oct. 3 I , 1980. Published February
I98 I . Originally published as E 96 - 53 T. Last previous edition
E96-66(1972).
Annual Book of ASTM Standards, Vol04.06.
’Annual Book of ASTM Standards. Vol04.04.
‘Annual Book of ASTM Standards. Vol 10.0 I.
385

~
material or construction induced by unit vapor
pressure difference between two specific surfaces,
under specified temperature and humidity conditions."
NOTE-Permeance is a performance evaluation and
not a property of a material.
"wafer vapor transmission rate-the steady
water vapor flow in unit time through unit area
of a body, normal to specific parallel surfaces,
under specific conditions of temperature and
humidity at each surface."
4. Summary of Test Methods
4.1 In the Desiccant Method the test specimen
is sealed to the open mouth of a test dish containing
a desiccant, and the assembly placed in a
controlled atmosphere. Periodic weighings determine
the rate of water vapor movement through
the specimen into the desiccant.
4.2 In the Water Method, the dish contains
distilled water, and the weighings determine the
rate of vapor movement through the specimen
from the water to the controlled atmosphere. The
vapor pressure difference is nominally the same
in both methods except in the variation, with
extremes of humidity on opposite sides.
5. Significance and Use
5.1 The purpose of these tests is to obtain, by
means of simple apparatus, reliable values of
water vapor transfer through permeable and semipermeable
materials, expressed in suitable units.
These values are for use in design, manufacture,
and marketing. A permeance value obtained under
one set of test conditions may not indicate
the value under a different set of conditions. For
this reason, the test conditions should be selected
that most closely approach the conditions of use.
While any set of conditions may be used and
those conditions reported, standard conditions
that have Seen s;sefs;! are shown in Appfidix
XI.
6. Apparatus
6.1 Test Dish-The test dish shall be of any
noncorroding material, impermeable to water or
water vapor. It may be of any shape. Light weight
is desirable. A large, shallow dish is preferred, but
its size and weight are limited when an analytical
6aIance is chosen to detect small weight changes.
The mouth of the dish shall be as large as practical
and at least 4.65 in.* (3000 mm2). The
E 96
desiccant or water area shall be not less than the
mouth area except if a grid is used, as provided
in 12.1, its effective area shall not exceed 10 %
of the mouth area. An external flange or ledge
around the mouth, to which the specimen may
be attached, is useful when shrinking or warping
OCCUTS. When the specimen area is larger than
the mouth area, this overlay upon the ledge is a
source of error, particularly for thick specimens.
This overlay material should be masked as described
in 10.1 so that the mouth area defines
the t&t area. The overlay material results in a
positive error, indicating excessive water vapor
transmission. The magnitude of the error is a
complex function of the thickness, ledge width,
mouth area, and possibly the permeability. This
error is discussed by Joy and Wilson.' This type
of error should be limited to about 10 to 12 %.
For a thick specimen the ledge should not exceed
3/4 in. (19 mm) for a IO-in. (254-mm) or larger
mouth (square or circular) or '/E in. (3 mm) for a
5-in. (127-mm) mouth (square or circular). For
a 3-in. (76-mm) mouth (square or circular) the
ledge should not exceed 0. I I in. (2.8 mm) wide.
An allowable ledge may be interpolated for intermediate
sizes or calculated according to Joy
and Wilson.' A rim around the ledge (Fig. X2. I)
may be useful. If a rim is provided, it shall be
not more than '14 in. (6 mm) higher than the
specimen as attached. Different depths may be
used for the Desiccant Method and Water
Method, but a 3/4-in. (19-mm) depth (below the
mouth) is satisfactory for either method.
6.2 Test Chamber-The room or cabinet
where the assembled test dishes are to be placed
shall have a controlled temperature and relative
humidity. The temperature chosen shall be between
70 and 90°F (21 and 32"C), and shall be
maintained constant within 1 'F (0.6"C). A temperature
of 90°F (32'C) is recommended (Note
I). The relative humidity shall be maintained at
50 .+ 2 %, except where extremes of humidities
are desired, when the conditions shall be 100 .+
1 "F(38 f 0.6"C) and 90 f 2 % relative humidity.
Both temperature and relative humidity shall be
measured frequently, or preferably recorded continuously.
Air shall be continuously circulated
throughout the chamber, with a velocity SUE-
' Joy, F. A.. and Wilson. H. G., "Standardization ofthe Dish
Method for Measuring Water Vapor Transmissions," National
Research Council of Canada, Research Paper 279. January
1966, p. 263.
386

m
cient to maintain uniform conditions at all test
locations. Its velocity over the specimen, in feet
per minute, shall be (numerically) not less than
ten times the permeance of the specimen, in
perms. but at least 500 ft/min, or in centimetres
per second not less than 7.7 times the permeance,
in metric perms, but at least 250 cm/s.
NOTE I-Simple temperature control by heating
alone is usually made possible at 90°F (32'C). However,
it is very desirable to enter the controlled space, and a
comfortable temperature is more satisfactory for that
arrangement. Temperatures of 73.4"F (23°C) and 80°F
(26.7-C) are in use and are satisfactory for this purpose.
With cyclic control, the average test temperature may
be obtained from a sensitive thermometer in a mass of
dry sand. The temperature of the chamber walls facing
a specimen over water should not be cooler than the
water to avoid condensation on the test specimen.
6.3 Balance and Weights-The balance shall
be sensitive to a change smaller than 1 % of the
weight change during the period when a steady
state is considered to exist. The weights used shall
be accurate to I 76 of the weight change during
the steady-state period. For example: A I-perm
(5.7 x IO-'' kg.Pa-'.s-'.m-2) specimen IO in.
(254 mm) square at 80°F (26.7"C) passes 8.6
grains or 0.56 g/day. In 18 days of steady state,
the transfer is IO g. For this usage, the balance
must have a sensitivity of I % of 10 g or 0.1 g
and the weights must be accurate to 0.1 g. If,
however, the balance has a sensitivity of 0.2 g or
the weights are no better than 0.2 g, the requirements
of this paragraph can be met by continuing
the steady state for 36 days. An analytical balance
that is much more sensitive will permit more
rapid results on specimens below 1 perm (5.7 x
IO-" kg-Pa-'-s-'.m-*) when the assembled dish
is not excessively heavy. A light wire sling may
be substituted for the usual pan to accommodate
a larger and heavier load.
7. Materials
7. i Desiccanr and Facer:
7. I. I For the Desiccant Method, anhydrous
calcium chloride in the form of small lumps that
will pass a No. 8 (2.36-mm) sieve, and free of
fines that will pass a No. 30 (600-pm) sieve, shall
be used (Note 2). It shall be dried at 400°F
(200°C) before use.
NOTE 2-If CaClz will react chemically on the specimen,
an adsorbing desiccant such as silicagel, activated
at 400°F (200°C). may be used; but the moisture gain
by this desiccant during the test must be limited to 4 %.
7.1.2 For the Water Method, distilled water
E 96
shall be used in the test dish.
7.2 Sealant-The sealant used for attaching
the specimen to the dish, in order to be suitable
for this purpose, must be highly resistant to the
passage of water vapor (and water). It.must not
lose weight to, or gain weight from, the atmosphere
in an amount, over the required period of
time, that would affect the test result by more
than 2 %. It must not affect the vapor pressure
in a water-filled dish. Molten asphalt or wax is
required for permeance tests below 4 perms (2.3
x IO-'' kg. Pa-' -s-'- m-I). Sealing methods are
discussed in Appendix X2.
8. Sampling
8.1 The material shall be sampled in accordance
with standard methods of sampling applicable
to the material under test. The sample shall
be of uniform thickness. If the material is of
nonsymmetrical construction, the two faces shall
be designated by distinguishing marks (for example.
on a one-side-coated sample, "1" for the
coated side and "11" for the uncoated side).
9. Test Specimens
9. I Test specimens shall be representative of
the material tested. When a product is designed
for use in only one position. three specimens
shall be tested by the same method with the vapor
flow in the designated direction. When the sides
of a product are indistinguishable, three specimens
shall be tested by the same method. When
the sides of a product are different and either side
may face the vapor source, four specimens shall
be tested by the same method, two being tested
with the vapor flow in each direction and so
reported.
9.2 A slab, produced and used as a laminate
(such as a foamed plastic with natural "skins")
may be tested in the thickness of use. Alternatively,
it may be siicea into two or more sheets.
each being separately tested and so reported as
provided in 9.4, provided also, that the "overlay
upon the cup ledge" (6. I ) of any laminate shall
not exceed '/x in. (3 mm).
9.3 When the material as used has a pitted or
textured surface, the tested thickness shall be that
of use. When it is homogeneous. however, a
thinner slice of the slab may be tested as provided
in 9.4.
9.4 In either case (9.2 or 9.3), the tested overall
thickness, if less than that of use. shall be at least
387

five times the sum of the maximum pit depths
in both its faces, and its tested permeance shall
be not greater than 5 perms (3.3 metric perms).
9.5 The overall thickness of each specimen
shall be measwed at the center of each quadrant
to the nearest 0.002 in. (0.05 mm) and the results
averaged.
NOTE 3-The time required for testing a thick specimen
of low permeability is long, in many cases increasing
as the square of the thickness. When testing a lowpermeance
material that may be expected to lose or
gain weight throughout the test (because of evaporation
or oxidation), it may be advisable to provide an additional
specimen or "dummy" tested exactly like the
others except that no desiccant or water is put in the
dish. For thick hygroscopic specimens of low permability,
the time required lo reach the steady state may be
as long as 60 days. Other materials may reach it quickly.
10. Attachment of Specimen to Test Dish
IO. 1 Attach the specimen to the dish by sealing
(and clamping if desired) in such a manner
that the dish mouth defines the area of the specimen
exposed to the vapor pressure in the dish.
If necessary, mask the specimen top surface,
exposed to conditioned air so that its exposure
duplicates the mouth shape and size and is directly
above it. A template is recommended for
locating the mask. Thoroughly seal the edges of
the specimen to prevent the passage of vapor
into, or out of, or around the specimen edges or
any portion thereof. The same assurance must
apply to any part of the specimen faces outside
their defined areas. Suggested methods of attachment
are described in Appendix X2.
NOTE 4-In order to minimize the risk of condensation
on the interior surface of the sample when it is
placed in the chamber, the temperature of the water
prior to preparation of the test specimen should be
within +2"F (+ 1. I T ) of the test condition.
11. ProyJure for Desiccant Method
1 1.1 Fill the test dish with desiccant within '1'4
in. (6 mmj ofthe specimen. Leave enough space
so that shaking of the dish, which must be done
at each weighing, will mix the desiccant.
1 1.2 Attach the specimen to the dish (see 10.1)
and place it in the controlled chamber, specimen
up, weighing it at once. (This weight may be
helpful to an understanding of the initial moisture
in the specimen.)
1 1.3 Weigh the dish assembly periodically, often
enough to provide eight or ten data points
during the test. A data point is the weight at a
particular time. The time that the weight is made
E96
should be recorded to a precision of approximately
I % of the time span between successive
weighing. Thus, if weighings are made every
hour, record the time to the nearest 30 s; if
recordings are made every day, a time to the
nearest 15 min would be allowed. At first the
weight may change rapidly; later a steady state
will be reached where the rate of change is substantially
constant. Weighings should be accomplished
without removal of the test dishes from
the controlled atmosphere, but if removal is prescribed
necessary, the time the specimens are
kept at different conditions, temperature or relative
humidity, or both, should be kept to a
minimum. Analyze the results as prescribed in
13.1.
11.4 Terminate the test or change the desiccant
before the water added to the desiccant
exceeds 10 % of its starting weight (Notes I and
4). This limit cannot be exactly determined and
judgement is required. The desiccant gain may
be more or less than the dish weight-gain when
the moisture content of the specimen has
changed.
NOTE 5-The WVT of some materials (especially
wood) may depend on the ambient relative humidity
immediately before the test. An apparent hysteresis
results in higher WVT if the prior relative humidity
was above the test conditon and vice versa. It is therefore
recommended that specimens of wood and paper
products be conditioned to constant weight in a 50 95
relative humidity atmosphere before they are tested.
Some specimens may be advantageously preconditioned
to minimize the moisture that the specimen will
give up to the desiccant. This applies when the specimen
is likely to have high moisture content or when it is
coated on the top (vapor source) side.
12. Procedure for Water Method
12. I Fill the test dish with distilled water to a
level 3/4 li: '/4 in. (19 +. 6 mm) from the specimen.
The air space thus allowed has a small vapor
resistance, but it is necessary in order to reduce
the risk ofwater touching the specimen when the
dish is handled. Such contact invalidates a test
on some materials such as paper, wood, or other
hygroscopic materials. The water depth shall be
not less than '/8 in. (3 mm) to ensure coverage of
the dish bottom throughout the test. However, if
the dish is of glass, its bottom must be visibly
covered at all times but no specific depth is
required. Water surges may be reduced in placing
a grid of light noncorroding material in the dish
to break the water surface. This grid shall be at
least 9'4 in. (6 mm) below the specimen, and it
388

shall not reduce the water surface by more than
10 W (Note 5).
NOTE 6-For the Water Method, baking the empty
dish and promptly coating its mouth with sealant before
is “TImendd. The may be added
most conveniently after the specimen is attached,
through a small sealable hole in the dish above the
water line.
12.2 Attach the specimen to the dish (see
10.1). Some specimens are likely to warp and
break the seal during the test. The risk is reduced
by preconditioning the specimen, and by clamping
it to the dish ledge (if one is provided).
12.3 Weigh the dish assembly and place it in
the controlled chamber on a true horizontal surface.
Follow the procedure given in 11.3. If the
test specimen cannot tolerate condensation on
the surface, the dish assembly shall not be exposed
to a temperature that differs by more than
5’F (2.8’C) from the control atmosphere to minimize
the risk of condensation on the specimen.
Analyze the results as prescribed in 13.1.
12.4 Where water is expected to be in contact
with the barrier in service, proceed as in 11.3
except place the dish in an inverted position. The
dish must be sufficiently level so that water covers
the inner surface of the specimen despite any
distortion of the specimen due to the weight of
the water. With highly permcable specimens it is
especially important to locate the test dish so that
air circulates over the exposed surface at the
specified velocity. The test dishes may be placed
on the balance in the upright position for weighing,
but the period during which the wetted surface
of the specimen is not covered with water
must be kept to a minimum.
13. Analysis of Results, Calculations
13.1 The results of the rate of water vapor
transmission may be determined either graphically
or numerically.
13.1.1 Graphic Analysis-Plot the weight
against elapsed time, and inscribe a curve which
tends to become straight. Judgment here is required
and numerous points are helpful. When
a straight line adequately fits the plot of at least
six properly spaced points, with due allowance
for scale sensitivity, a nominally steady state
exists (Note 3), and the slope of the straight line
is the rate of water vapor transmission.
13. I .2 Numerical Analysis-A mathematical
least squares regression analysis of the weight as
a function of time will give the rate of water
vapor transmission. An uncertainty, or standard
deviation of this rate, can also be calculated to
define the confidence band- For very low Permeability
materials, this method can be used to
determine the results after 30 to 60 days when
using an analytical balance, with a sensitivity of
+.I mg, even if the weight change does not meet
the 100 times the sensitivity requirement of 6.3.
Specimens analyzed in this manner must be
clearly identified in the report.
13.2 Calculate the water vapor transmission.
WVT, and permeance as follows:
13.2.1 Water Vapor TranJmission:
WVT = G/tA = (G/t)/A
where:
In inch-pound units:
G = weight change, grains (from the
straight line),
t = time during which G occurred. h,
G/t = slope of the straight line, grains/h.
.4 = test area (cup mouth area), ft2. and
WVT = rate of water vapor transmission.
grains/h. ft’.
In metric units:
G = weight change (from the straight line).
g*
t = time, h.
G/t = slope of the straight line, g/h,
.4 = test area (cup mouth area), m’, and
WVT = rate of water vapor transmission, g/h.
m’.
13.2.2 Permeance:
Permeance = WVT/Ap = WVT/S(R, - R2)
where:
In inch-pound units:
Ap = vapor pressure difference, in. Hg,
S
= saturation vapor pressure at test temperature,
in. Hg,
R, = relative humidity at the source expressed
as a fraction (the test chamber for desiccant
method; in the dish for water
method), and
R, = relative humidity at the vapor sink expressed
as a fraction
In metric units:
Ap = vapor pressure difference, mm Hg ( 1.333
x 10‘ Pa),
S = saturation vapor pressure at test temperature,
mm Hg (1.333 x IO’ Pa),
R, = relative humidity at the source expressed
389

E96
as a fraction (the test chamber for desiccant
method; in the dish for water
method), and
relative humidity at the vapor sink expressed
as a fraction.
13.2.3 In the controlled chamber the relative
humidity and temperature are the average values
actually measured during the test and (unless
continuously recorded) these measurements shall
be made as frequently as the weight measurements.
In the dish the relative humidity is nominally
0 % for the desiccant and 100 % for the
water. These values are usually within 3 % relative
humidity of the actual relative humidity for
specimens below 4 perms (2.3 x g.Pa-'-
s-I m-I) when the required conditions are maintained
(no more than 10 % moisture in CaC12
and no more than 1 in. (25 mm) air space above
water).
13.3 Only when the test specimen is homogeneous
(not laminated) and not less than '12 in.
( 12.5 mm) thick, calculate its average permeability
(perm in.) (metric perm-cm) as follows:
Average permeability = permeance x thickness
NOTE 7: Example-in a desiccant test that ran 288
h ( 12 days) on an exposed area of 100 in? (0.0645 m'),
it was found that the rate of gain was substantially
constant after 48 h and during the subsequent 240 h,
the weight gin was 12 g. The controlled chamber
conditions were measured at 89.O"F (31.7-C) and 49 %
relative humidity.
Required: WVT and permeance
Calculation (inch-pound units):
Permeance =
-
0.77 1 grains/h, -
100 in2 x ft2 - 0.695 ft2,
144 in2
1.378 in. Hg (from standard references
tables),
49 % (in chamber),
0 % (vapor sinkj, and
0.771 grains/h i 0.694 ft2 = 1.1 1
grains/ft2 h.
WVTIbP = WVT/S (R1- Rz)
1.1 1 grains/ft2.h + 1.378 in. Hg
(0.49- 0)
1.64 grains/Ft2.h.in. Hg = 1.64
perms
Calculation (metric units):
Glt = 12 g/240 h = 0.05 g/h,
A = 0.0645 m2,
S = 35 mm Hg (from reference tables),
Rl
R2
WVT
= 35 mm Hg x 1.333 X 102 Pa/"
Hg = 46.66 x lo2 Pa,
= 49 % (in chamber),
= 0 '36 (vapor sink), and
= 0.05 g/h + 0.0645 m2 = 0.775 g/
h - m2.
Permeance = WVT/AP - WVT/S (R, - R2)
= 0.775 g/h.m2 X 1 h/36OOs +
46.66 x lo2 Pa X (0.49 - 0)
= 9.42 x IO-* g/Pa-s-m2
13.4 Metric units and conversion factor are
given in Table 1.
14. Report
14.1 The report shall include the following
14.1.1 Identification of the material tested,
including its thickness.
14.1.2 Test method used (desiccant or water).
14.1.3 Test temperature.
14.1.4 Relative humidity in the test chamber.
14.1.5 Permeance of each specimen in perms
(to two significant figures).
14. I .6 The side of each specimen on which
the higher vapor pressure was applied. (The sides
shall be distinguished as "side A" and "side B"
when there is no obvious difference between
them. When there is an obvious difference, this
difference shall also be stated, such as "side A
waxed" and "side B unwaxed.").
14.1.7 The average permeance of all specimens
tested in each position.
14.1.8 The permeability of each specimen (as
limited by 13.3), and the average permeability of
all specimens tested.
14.1.9 Include a portion of the plot indicating
the section of the curve used to calculate permeability.
14.1.10 State design of cup and type or composition
of sealant.
15. Precision and Bias
15. i Resuits obtained by any one procedure
on several specimens from the same sample may
differ as much as 10 95 from their average. Two
significant figures in water vapor transmission or
permeance will, therefore, usually sufice to characterize
the sample. Nevertheless, careful attention
to all aspects of the procedure is required in
order to obtain test results of acceptable precision.
Possible errors resulting from tolerances are
shown in Table 2. Accuracy of methods and
apparatus may be checked by using Recommended
Practice C 677.
390

~~
TABLE I
Metric Units and Conversion Factors"-'
To Obtain (for
Multiply by the same test
condition)
WVT
g/h. m2 1.43 grains/h. ft2
grains/h. A2 0.697 g/h. m2
Permeance
g/h.s-m' 1.75 X IO' 1 Perm (inch-pound)
1 Perm (inch-pound) 5.72 X IO-8 g/Pa.s.m*
Permeability
g/Pa.s.m 6.88 x 10" 1 Perm inch
I Perm inch 1.45 x IO4 g/Pa.s.m
"These units are used in the construction trade. Other units
may be used in other standards.
'All conversions of mm Hg to Pa are made at a temperature
of O'C.
Section
TABLE 2
Errors Resulting from the Tolerances
Possible Error, %
Wet
Notes :2 CUD
6. I Cup ledge " +I2 +I2
1.2 Sealant gain or loss
f2 f2
6.2 Chamber tempera- ' f3 *3
6.2
ture
Chamber relative ' f4 f4
humidity
6.3 Balance sensitivity +I f l
6.3 Accuracy of ' +.I f l
weights
11. 12 Air in dish -I -3
1 I .4 10 % water in CaC12 -6 ...
" This error applies to a homogeneous specimen I V4 in. (32
mm) thick. The error is smaller for a thin specimen and is
limited to 10% for a laminate by the %in. (3-mm) overlay
provided in 9.2.
'These errors are eliminated by correct measurements and
calculations based thereon.
'This error applied to a 4-perm specimen. and is smaller for
lower permeance.
APPENDIXES
(Nonmandatory Information)
XI. STANDARD TEST CONDITIONS
XI.1 Standard test conditons that have been useful 73.4'F (23°C).
are: X 1. I .4 Prtwdirrc C-Desiccant Method at 90'F
X1.1.1 Procedure A-Desiccant Method at 73.4"F (32.2'C).
(23%). X 1. I .5 Prtwedurc. D-Water Method at 90'F
X1.1.2 Procedure B-Water Method at 73.4"F (32.2T).
(23%). X I. I .6 Procedure. E-Desiccant Method at I WF
X1.1.3 Procedure BW-Inverted Water Method at (37.8"C).
X2. CUP DESIGN AND SEALING METHODS
X2.1 An ideal sealing material has the following
properties:
X2. I. 1 Impermeability to water in either vapor or
liquid form.
X2.1.2 No gain or loss of weight from or to the test
chamber (evaporation. oxidation, hygroscopicity. and
water solubility being undersirable).
X2. I .3 Good adhesion to any specimen and to the
dish (even when wet).
X2.1.4 Coinplete conformity to a rough surface.
X2. I .5 Compatibility with the specimen and no excessive
penetration into it.
X2.1.6 Strength or pliability (or both).
X2.1.7 Easy handleability (including desirable viscosity
and thermal of molten sealant).
X2. I .8 Satisfactory sealants possess these properties
in varying degrees and the choice is a compromise, with
more tolerance in items at the beginning of this list for
the sake ot those at the latter part of the list when the
requirements of 7.2 are met (Note A2). Molten asphalt
or wax is required for permeance tests below 4 perms
(2.6 metric perms). Tests to determine sealant behavior
should include:
X2. I .8. I An impervious specimen (metal) normally
sealed to the dish and so tested. and
X2.1.8.2 The seal normally assembled to an empty
dish with no specimen and so tested.
X2.2 The following materials are recommended for
general use when the test specimen will not be affected
by the temperature of the sealant:
X2.2. I Asphalt, I80 to 2WF (82 to 93°C) softening
point, meeting the requirements of Specification D 449,
Type C. Apply by pouring.
X2.2.2 Beeswax and rosin (equal weights). A temperature
of 275'F ( 135°C) is desirable for brush application.
Pour at lower temperature.
39 1

X2.2.3 Microcrystalline wax6 (60 %), mixed with
refined crystalline paraftin wax (40 %).
X2.3 The materials listed in X2.3.1 are recommended
for particular uses such as those shown in
Figure X2.1. The suggested procedure described in
X2.3.2 applies to an I I-3/8-in. (289-mm) square specimen
if its permeance exceeds 4 perms (2.6 metric
perms) (limited by evaporation of sealants).
X2.3.1 Mutcviuls:
X2.3. I. I Aluminum foil, 0.005 in. (0. I25 mm) minimum
thickness.
X2.3.1.2 Tape, meeting the requirements of Specification
D 230 1, vinyl chloride plastic pressure-sensitive,
electrical insulating tape.
X2.3. I .3 Cement. contact bond, preferably rubber
base.
X2.3.2 Procedurc:
X2.3.2.1 Stcp I-Seal aluminum foil around edges
ofspecimen. leaving a 100-in.' (0.0654-m') exposed test
area on each side. Use contact bond cement as directed
by the manufacturer.
X2.3.2.2 Step 2-Spread sealant on inside of rim
and ledge. Place desiccant (dry), or water and surge
control material (wet) in pan. Press specimen in place.
Avoid squeezing compound into the test area.
X2.3.2.3 Step 3-Coat outside of rim and bottom
of ledge with contact bond cement. and place foil strips
from edge of template. around rim. and bottom of
ledge.
X2.4 A method of using hot asphalt, as appiied to a
IO-in. (254-mm) square-mouth dish with ledge and rim,
is as follows:
X2.4.1 ,4ppururus:
X2.4.I.I Trmnplule-A square frame of brass or
steel, in. (5 mm) thick and V4 in. (19 mm) deep.
The %6-in. (5-mm) thickness is tapered to zero at the
bottom of the frame where it will touch the test specimen
and maintain a IO-in. (254-mm) square test area.
X2.4. I .2 Sculunt-Asphalt (see X2.2.1 used at the
proper pouring consistency of 375 to 450°F (179 to
232°C).
X2.4.1.3 Melting Pot 'for the asphalt, electrically
heated, with one dimension greater than 1 1 in. (289
mm).
X2.4.1.4 Small Ladle for pouring.
X2.4.2 Procedure-Mark the 1 I%n. (289-mm)
square specimen with a line at an equal distance from
each edge. so that the area enclosed by the lines is as
nearly as possible a IO-in. (254-mm) square. The template
may be used for marking. Dip each edge of the
specimen in molten asphalt up to the line, so that the
test area is defined and all edges are coated with a heavy
layer of asphalt. Place the specimen over the pan containing
water or desiccant. Lightly oil the template or
coat with petroleum jelly on its outer side, and place
on the specimen. Pour molten asphalt into the space
between the template and the rim of the pan. After the
asphalt has cooled for a few minutes, the template
should be easily removable.
X2.5 Hot wax may be applied like asphalt. It may
also be applied (freely) with a small brush. Its lower
working temperature may be advantageous when a
specimen contains moisture.
X2.6 Several designs for dishes with supporting rings
and flanges are shown in Fig. X2.2. Various modifica-
tions of these designs may be made provided that the
principle of prevention of edge leakage by means of a
complete seal is retained. The dishes may be constructed
of any rigid, impermeable, corrosion-resistant
material, provided that they can be accommodated on
the available analytical balance. A lightweight metal.
such as aluminum or one of its alloys, is generally used
for larger-size dishes. In some cases when an aluminum
dish is employed and moisture is allowed to condense
on its surface, there may be appreciable oxidation of
the aluminum with a resulting gain in weight. Any gain
in weight will ordinarily depend on the previous history
of the dish and the cleanness of the surface. An empty
dish camed through the test procedure as a control will
help to determine whether any error may be expected
from this cause. When aluminum dishes are used for
the water methods. a pressure may develop inside the
assembly during a test due to corrosion. This can cause
seal failure or otherwise affect the result. Where this is
a problem, it can be overcome by providing inside the
dish a protective coating of baked-on epoxy resin or
similar material. Dishes with flanges or rings that project
from the inner walls of the dish are to be avoided,
as such projections influence the diffusion of the water
vapor. The depth of the dish for the water procedures
is such that there is a 0.80 f 0.20 in. (20 f 5-mm)
distance between the water surface and the under surface
of the specimen, with a water depth of about 0.20
in. (5 mm).
X2.6. I For the desiccant-in-dish procedures. the
dishes need not be as deep as those required for the
water-in-dish procedures. The desiccant is within '/4 in.
(6 mm) of the under surface. and a minimum depth of
only in. (12 mm) of desiccant is required.
X2.6.2 The dishes shown in Fig. X2.2 require a
molten seal.
X2.6.3 A template such as is shown in Fig. X2.3 is
usually used for defining the test area and effecting the
wax seal. It consists of a circular metal dish '/a in. (3.18
mm) or more in thickness with the edge beveled to an
angle of about 45". The diameter of the bottom
(smaller) face of the template is approximately equal
to. but not.greater than, the diameter of the effective
opening of the dish in contact with the specimen. Small
guides may be attached to the template to center it
automatically on the test specimen. A small hole
through the template to admit air. and petrolatum
applied to the beveled edge of the template facilitate its
removal after sealing the test specimen to the dish. In
use, the template is placed over the test specimen and
when it is carefully centered with the dish opening,
molten wax is flowed into the annular space surrounding
the beveled edge of the template. As soon as the
wax has solidified. the template is removed from the
sheet with a twisting motion. The outside flange of the
dish should be high enough to extend over the top of
the specimen. thus allowing the wax to completely
envelop the edge.
X2.6.4 Gasketed types of seals are also in use on
appropriately designed dishes. These simplify the
'Grade Nos. 2305 or 2310 of the Mobil Oil Corp.. or their
equivalent. have been found satisfactory for this purpose.
392

mounting of the specimen, but must be used with
caution, since the possibility of edge leakage is greater
with gasketed seals than with wax seals. Gasketed seals
a~ not permitted for the measurement of permeance
less than 0.044 perms (2.5 ng. Pa-' s-' . m2). As a further
precaution when gasketed seals are used instead of
preferred sealants, a blank test run is suggested using
glass or metal as a dummy specimen.
X2.6.5 A suitable weighing cover consists of a cir-
cular disk of aluminum I/Jz to 3/32 in. (0.8 to 2.4 mm)
in thickness provided with a suitable knob in the center
for lifting. The cover fits over the test specimen when
assembled and makes contact with the inside beveled
surface of the wax seal at, or just above, the plane of
the specimen. The cover is free of sharp edges which
might remove the wax and is numbered or otherwise
identified to facilitate its exclusive use with the same
dish.
Template
Sample
Aluminum Foil
I n
-
Square Pan
Specimen
Specimen
Specimen
Foil
(Tape or Foil)
FIG. X2.1
Apparatus for Water Vapor Transmission Tests of Luge Thick Specimens
FIG. X2.2 Several Types of Dishes for Water Vapor
Transmission Tests of Matedals in Sheet Form
393

FIG. X2.3 Template Suitable for Use in Making the Wax
Seals on Test Dishes
Thc :I miwcan SoiiiJty.liir 7'e.sring and .VaterialY tokev no position revpiwing the validity ifany putiwl rights assi~rti.cl in connixtion
with any item mmrioniJd in this standard. L:si.r,. ofthis standard arc evpriwly advised that dctcvminution oj'rhc validity (?/'any such
putiwt rights, and the risk i?finJringiv"t of mch rights. arc iwtirc$j, their own responsibility.
This .standard is .\ithic't't to riwision at any timil by tha revponsihli> tc~chnicul iwnmitti.e and mii.vt be rivicned evcvy,/iv(~ ycwrs und
if' not riwvid. either riwpproved or withdrann. Your cornmiwts arc invitcxl eithi~r ,/Or ri4sion oJ this standard or jiir udditional
.standard.v and shoitld be oddrevscd to .4ST.M t1eadquarti~r.s. Yoitr comniiwt Y will riwivc cartlfitl consideration at u meciting of the
ri~vponsihli~ tcdinii~ul commiltiv. which j'ou may atrend. l/'jwrc .li.c.l that yoirr irmmmts huvc. not riwived a Juir hcaririg .voir shorcld
muke your vitw:v known to thr .ASTM Commiltc.c. on 9andard.y. lVlb Race SI.. Philadelphia. PA 19103.
394

Designation: E 450 - 82 (Reapproved 1987)"
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition
Standard Test Method for
MEASUREMENT OF COLOR OF LOW-COLORED CLEAR
LIQUIDS USING THE HUNTERLAB COLOR DIFFERENCE
METER'
This standard is issued under the fixed designation E 450 the number immediately following the designation indicates the year of
oenal adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A suprsctipt epsilon ( E) indicates an editorial change since the last revision or reapproval.
NOTE-Editorial changes were incorporated throughout in August 1987.
1. scope
1.1 This test method covers the instrumental
measurement of the color of low-colored, clear,
nonfluorescent and nonmetameric liquids using
water as the reference material. In certain applications
it may be desirable to use another material
as the referende. The color differences between
the sample and reference are expressed in
units of approximately uniform visual color perception
as described by either the Hunter L, a, b
scales or the CIE 1976 L*, a*, b* scales.*
1.2 This test method is intended for the measurement
of the color of lowcolored liquids free
of haze. The test method is applicable to liquids
whose color intensity approximates the range
fiom 0 to 25 platinum-cobalt units, although the
hues of the liquids are not limited to yellow
colors. Colors of higher intensity may be measured
by using cells of shorter light path.
1.3 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purporr to address all of the safety problems
associated with its use. It is the responsibility
ofrhe user of this standard to establish appropriate
safity and health practices and to determine
the applicability of regulatory limitations
prior to use.
2. Refereneed Documents
2.1 ASTM Standards:
D 1209 Test Method for Color of Clear Liquids
(Platinum-Cobalt Scale)'
D2244 Method for Calculation of Color Differences
from Instrumentally Measured
Color Coordinates4
E 180 Practice for Determining the Precision
of ASTM Methods for Analysis and Testing
of Industrial Chemicals'
3. Descriptions of Terms Specific to this Standard
3. I color space-the daylight colors of liquids
are represented by points in a space formed by
three mutually perpendicular unit vectors, E, d,
and 6, having scales, L, a, and b, respectively
(Fig. 1). These scales were chosen so that color
differences in this space correlate with perceived
color differences in an approximately linear fashion.
3.2 L scale-the L scale measures the lightness
or grayness component of the color of the
sample. The color difference due to grayness ( AL)
between the sample and water is described by the
magnitude and algebraic sign of the value. A
positive value indicates less gray (lighter) than
water; a negative value indicates more grayness
(darker) than water.
3.3 a scale-the a scale measures the chro-
' This test method is under the jurisdiction of ASTM Committee
E- I5 on Industrial Chemicals and is the direct responsibility
of Subcommittee E 15.23 on Physical Properties.
Current edition approved March 26, 1982. Published June
1982. Originally published as E 450 - 72 T.Last previous edition
E 450 - 77.
'Hunter, R. S., "Photoelectric Color Difference Meter",
Journal ofthe Optical Society OJAmerica, JOSAA, Vol 12, No.
12. December 1958, pp. 985-995, and Supplement No. 2 to
CIE Publication, No. I5 (May 1976). Official Recommendations
on Uniform Color Spaces, Color-Difference Equations, Maric
Color Terms.
'Annual Book of ASTM Standards, Vols 06.0 I and 06.03.
'Annual Book of ASTM Standards, Vol06.01.
Annual Book ofASTM Standards, Vol 15.05.
395

maticity differences in the red-green components
of the color of the sample. The color difference
due to the red-green component (Aa) between
the sample and water is described by the magnitude
and algebraic sign of the value. A positive
value indicates the sample is redder (less green)
than water; a negative value indicates the sample
is greener (less red) than water.
3.4 b scale-the b scale measures the chromaticity
differences in the yellow-blue components
of the color of the sample. The color difference
due to the yellow-blue component (Ab)
between the sample and water is described by the
magnitude and algebraic sign of the value. A
positive value indicates the sample is yellower
(less blue) than water; a negative value indicates
the sample is bluer (less yellow) than water.
3.5 AE scale-the AE scale is a measure of
the total color difference between the sample and
water. The magnitude of AE gives no indication
of the character of the color of the sample because
it does not indicate the quantity and direction of
the hue, saturation and lightness components.
The AE value is derived from the AL, Aa, and
Ab values.
3.6 Relationship of Color Scales to Tristimu-
Ius Values-The relationships of the Hunter L,
a, b scales and the CIE L*, u*, b* scales to
tristimulus values are given by the following
equations:'
3.6.1 Hunter L, a, b scales:
L = IO JT
u = 17.5 (1.02X - Y)/a
b = 7.0 (Y - 0.847Z)IJY
where X, Y, and 2 are the tristimulus values for
the I93 1 CIE Standard Observer and Source C.
3.6.2 CIE L* a* b* scales:
L* 25Y113 - 16
a* = 107.7 ((1.0291'3 - ~ 113)
b* = 43.09 (Y'13- (0.8472)'13)
where X, Y, and Z are the tristimulus values for
the 193 1 CIE Standard Observer and Source C.
4. Summary of Test Method
4.1 Differences in the color of the sample and
water are determined with Hunterlab Color Difference
Meter.6 The transmission measurements
are made and read directly from the instrument
as units of the L, a, and b color scales. A measure
of total color difference, AE, may be calculated
from the AL, Aa, and Ab values of the sample.
E 450
5. Significance and Use
5.1 This test method provides a means of
objectively measuring the color of low-colored
clear liquids regardless of the hue. Color measurements
of fluorescent liquids are beyond the
scope of this test method. Erroneous results may
be obtained on metameric liquids, but the error
may be expected to be slight at low levels of color
intensity.
5.2 This test method complements Method
D 2244 for the measurement of color differences
of opaque materials.
5.3 This test method permits the use of two
sets of color scales, the older Hunter L, a, b color
scales and the CIE L*, a*, b* scales established
by the CIE in 1976. Each set of color scales
correlate well with average visual judgments of
color appearance.
6. Apparatus
6. I Hunterlab Color Drference Meter, Model
D2Sp6, capable of measuring the L, a, and b
values to the nearest 0.0 1 unit and equipped with
a special cell holder to position a IO-cm cell
parallel to the pivoted light source.
NOTE I-Some models measure color in terms of
the Hunter L, u, b scales; others can use either the
Hunter scales or the CIE L* a* b* scales. Where measurements
by more than one laboratory are involved,
agreement should be reached on which scales are to be
used.
6.2 Absorption Cells, IO-cm light path, 35-
mm outside diameter, and equipped with one or
two stoppered filling' ports. Two matching cells
are required.
7. Reagents and Materials
7.1 Purity of Reagents-Reagent grade chemicals
shall be used in all tests. Unless otherwise
indicated, it is intended that all reagents shall
conform to the specifications of the Committee
on Anaiyticai Reagenrs of the American Cnemical
Society, where such specifications are available.'
Other grades may be used, provided it is
first ascertained that the reagent is of sufficiently
'Model D25P-SS. D25P-2DT. or D25P-9 manufactured by
Hunter Associates Laboratory, Inc., 11495 Sunset Hills Rd.,
Reston, VA 22090, has been found satisfactory for this purpose.
' Reagent Chemicals, American Chemical Society Specifications,
American Chemical Society, Washington, DC. For suggestions
on the testing of reagents not listed by the American
Chemical Society, see *Reagent Chemicals and Standards," by
Joseph Rosin, D. Van Nostrand Co.. Inc., New York, NY. and
the "United States Pharmacopeia."
396

E450
high purity to permit its use without lessening
the accuracy of the determination.
7.2 Purity of Water-References to water
shall be understood to mean colorless, distilled
water. A recommended procedure for preparing
the water follows:
7.2.1 Into a 3000-mL round bottom borosilicate
flask containing approximately 2500 mL of
distilled or deionized water, add 0.5 g of sodium
hydroxide and 0.2 g of potassium permanganate
for each litre of water.
7.2.2 Attach to the flask a 20-cm by 20-mm
outside diameter glass column packed with glass
helices, and equipped with a water-cooled distillation
head.
7.2.3 Apply heat to the flask by means of a
heating mantle, and distill at a rate of about 5
mL/min. Discard the first 20%, and stop the
distillation with 20 % remaining in the flask.
Store the distillate in a borosilicate glass container.
8. Procedure
8.1 Check to make sure the instrument is
operating correctly in accordance with the manufacturer’s
instruction manual.
8.2 Turn the lamp switch from Standby to
On, and insert the white standard tile at the
outside position of the sphere. Rotate the light
source by pulling out the left knob on the side of
the lamp housing so that the pivoted beam shines
through the entrance port of the sphere and
strikes the interior wall of the sphere. If necessary,
the diameter of the beam must be adjusted so
that none of the beam strikes the edge of the
entrance port or the wall of the IO-cm cell when
the cell is mounted parallel to the beam using
the special cell holder. Refer to the manufacturer’s
instruction manual for details on making
this adjustment.
8.3 Rinse, drain, and fill two clean lO-cm cells
with water. The level of the liquid should extend
up into the filler necks of the cells and there must
be no bubbles in the cell. Carefully wipe the faces
of each cell with lens tissue to remove smudges,
dust, etc.
8.4 Place the reference cell in the instrument,
using the special cell holder to position the cell
parallel to the light beam, with the edge of the
cell touching the face plate of the sphere.
8.5 With the standardizing knobs, standardize
the L scale to 100.00, the a scale to 0.00, and the
b scale to 0.00.
8.6 Replace the reference cell with the sample
cell and measure the L, a, and b values. Record
the L, a, and b values to the nearest 0.01 unit.
8.7 Replace the sample cell with the reference
cell and verify the original set values. If the values
for L, a, and b differ from 100.00,0.00, and 0.00,
respectively, by more than f 0.05 units, a drift
in the instrument is indicated, and 8.4 through
8.6 should be repeated until no instrument drift
is detected. Record the L, a, and b values for the
distilled water in the sample cell versus distilled
water in the reference cell to the nearest 0.01
unit. These values are Lo, a,, and bo in the
calculations.
8.8 Drain the sample cell, rinse the cell with a
solvent suitable for the sample, rinse with small
portions of anhydrous methanol, and dry with a
stream of air. Fill the sample cell with the sample
so that the level of the liquid extends up into the
filler necks of the cell. There must be no air
bubbles in the cell. Carefully wipe the faces of
the cell with lens tissue to remove any smudges,
dust, etc.
8.9 Verify the L, a, and b settings of 100.00,
0.00, and 0.00, respectively, for the reference cell,
and if the readings differ by more than f 0.05
unit from the set values, readjust the instrument
as described in 8.4 through 8.6. Replace the
reference cell with the sample cell and determine
the L, a, and b readings in the same fashion
described previously. Record the L, a, and b
values for the sample. These values are Li, ai, and
6, in the calculations. ReverifL the reference cell
settings, and remeasure the sample if instrument
drift is noted.
9. Calculation
9. I Calculate the color of the sample using the
following equations:
AL=Li-L,
Ab = bj - 6,
where:
L,, a, , and bo refer to the measurements of the
reference solution (water),
Lj, at, and bi refer to the measurements of the
sample, and
AE = total color difference.
10. Report
10.1 Report the values of AL, Au, Ab, and AE
to the nearest 0.01 unit and identi@ the scale
397

used: Hunter L, a, b, or CIE L*, a*, b*.
10.1.1 Duplicates that agree within the values
shown in Table 1 are acceptable for averaging
(95 ?6 confidence level).
11. Precision and Bias
11.1 The following criteria should be used for
judging the acceptability of results:
NOTE 2-The precision statements are based on an
interlaboratory study performed in 1970-7 I on samples
of platinum-cobalt standards covering the range from
0 to 100 units. These standards were prepared as described
in Method D 1209. The data expressed in terms
of Hunter L, a, b scales, were obtained using a model
D25P-SS instrument that is no longer manufactured.
The replacement models (D25P-2DT and D25P-9),
according to the manufacturer, have been improved
with respect to the detecter, electronics, and readout,
and should have a precision at least as good as, and
probably better than, the model used in the 1970-71
study. The manufacturer explains that the D25P identification
was retained because no changes were made
in the vital spectral and geometric optics of the new
instruments. Four laboratories using six instruments
and six analysts measured each sample in duplicate on
each of two days.' Practice E I80 was used in develop
ing these precision statements.
1 1.1.1 Repeatability (Single Analyst)-The
standard deviation of results (each the average of
duplicates), obtained by the same analyst on
different days, has been estimated to be the values
shown in Table 1. Two such results should be
considered suspect (95 % confidence level) if they
differ by more than the values in Table 1.
1 1.1.2 Reproducibility (Multi1aboratov)-
The standard deviation of results (each the average
of duplicates), obtained by analysts in different
laboratories has been estimated to be the
values shown in Table 1. Two such results should
be considered suspect (95 % confidence level) if
they differ by more than the values in Table 1.
* Supporting data giving results of cooperative tests are available
from ASTM Headquarters. Request R R EIS-1014.
Level
AL =010-2
= -2 lo -5
AU =0!0-2
= -2 10 -5
Ab =Olo 14
= 14 to24
AE -0108
= 14 lo25
TABLE 1 ColorplerlsioaIh~bA
Duplicates Repeatability Reproducibility
Standard
Standard 95x
95% Degrees Standard 95% Degrees
Desrees
Deviation Range Freedom Deviation Range Freedom 7:;- Range Freedom
0.026 0.07
0.028 0.08
0.028 0.80
0.029 0.09
0.018 0.05
0.0 I6 0.05
0.012 0.03
0.020 0.06
36
24
32
20
36
22
34
22
0.054 0.16
0.035 0.11
0.030 0.09
0.06 I 0.19
0.029 0.09
0.029 0.09
0.042 0.12
0.033 0. IO
-
18
12
16
10
18
I1
17
I1
0.41 5
0.326 1.19 5
0.169 0.66 4
0.791 3. IO 4
0.076 0.28 5
2.004 7.30 5
0.110 0.40 5
1.923 7.00 5
~-
A For a better appreciation of the visual significance of the L, (I, b, and AE scales, the following approximate relationships may be
helpful. Based on average analyses of platinum-cobalt standards from 0 to 25 units, one unit of L corresponds to about 17 platinumcobalt
units; one unit of a, I7 platinum-cobalt units; one unit of b, 3,4 platinumoobalt units; and one unit of AE, 3.2 platinumcobalt
units.
398

100 White
Yellow
Orange
- 50
-80 a-,
I
0 Black
FIG. 1 Rectangubr Color Solid with Dimenshs L, o, .ad b
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users ofthis standard are expressly advised that determination of the validity of any such
patent rights. and the risk of infringement of such rightso are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every jive years and
i/ not revised- either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addre.ssed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible twhnical committee, which you may attend. If you feel that your comments have not received a.fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race SI., Philadelphia, PA 19103.
399

Designation: E 595 - 84
AlPtERlCAN SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadddphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
TOTAL MASS LOSS AND COLLECTED VOLATILE
CONDENSABLE MATERIALS FROM OUTGASSING IN A
VACUUM ENVIRONMENT'
This standard is issued under the fixed designation E 595; the number immediately following the designation indicates the year of
original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (c) indicates an editorial change since the last revision or reapproval.
1. scope
1.1 This test method covers a screening technique
to determine volatile content of materials
when exposed to a vacuum environment. Two
parameters are measured: total mass loss (TML)
and collected volatile condensable materials
(CVCM). An additional parameter, the amount
of water vapor regained (WVR), can also be
obtained after completion of exposures and measurements
required for TML and CVCM.
1.2 This test method describes the test apparatus
and related operating procedures for evaluating
the mass loss of materials being subjected
to 125°C at less than 7 x Pa (5 X torr)
for 24 h. The overall mass loss can be classified
into noncondensables and condensables. The latter
are characterized herein as being capable of
condensing on a collector at a temperature of
25°C.
NOTE I-Unless otherwise noted, the tolerance on
25'C and 125'C is k1"C and on 23°C is k2T. The
tolerance on relative humidity is +5 %.
1.3 Many types of organic, polymeric, and
inorganic materials can be tested. These include
polymer potting compounds, foams, elastomers,
films, iapes, insulations, shrink tubings, adhesives,
coatings, fabrics, tie cords, and lubricants.
The materials may be tested in the "as-received"
condition or prepared for test by various curing
specifications.
1.4 This test method is primarily a screening
technique for materials and is not necessarily
valid for computing actual contamination on a
system or component because of differences in
configuration, temperatures, and material proc-
essing.
1.5 The criteria used for the acceptance and
rejection of materials shall be determined by the
user and based upon specific component and
system requirements. Historically TML of
1 .OO % and CVCM of 0.10 % have been used as
screening levels for rejection of spacecraft materials.
1.6 The use of materials that are deemed ao
ceptable in accordance with this test method does
not ensure that the system or component will
remain uncontaminated. Therefore, subsequent
functional, developmental, and qualification
tests should be used, as necessary, to ensure that
the material's performance is satisfactory.
1.7 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safity and health practices
and determine the applicability of regulatory limitations
prior to use.
2. Applicable Document
2.1 Am&! Slandard:
E 177 Recommended Practice for Use of the
Terms Precision and Accuracy as Applied to
Measurement of a Property of a Material2
' This test method is under the jurisdiction of ASTM Committee
E-21 on Space Simulation and Applications of Space
Technology.
Current edition approved Oct. 26, 1984. Published April
1985. Originally published as E 595 - 77. Last previous edition
E 595 - 83.
Annual Book of ASTM Standards, Vol 14.02.
400

3. Definitions
3.1 collected volatile condensable material,
CVCM-the quantity of outgassed matter from
a test specimen that condenses on a collector
maintained at a specific constant temperature for
a specified time. CVCM is expressed as a percentage
of the initial specimen mass and is calculated
from the condensate mass determined
from the difference in mass of the collector plate
before and after the test.
3.2 total mass loss, TML-total mass of material
outgassed from a specimen that is maintained
at a specified constant temperature and
operating pressure for a specified time. TML is
calculated from the mass of the specimen as
measured before and after the test and is expressed
as a percentage of the initial specimen
mass.
3.3 water vapor regained, WR-the mass of
the water vapor regained by the specimen after
the optional reconditioning step. WVR is calculated
from the differences in the specimen mass
determined after the test for TML and CVCM
and again after exposure to a 50 % relative humidity
atmosphere at 23°C for 24 h. WVR is
expressed as a percentage of the initial specimen
mass.
4. Summary of Method
4.1 This microvolatile condensable system3
was developed from an earlier system for determination
of macrovolatile condensables that required
much larger samples and a longer test.
4.2 The test specimen is exposed to 23°C and
50 % relative humidity for 24 h in a preformed,
degreased container (boat) that has been weighed.
After this exposure, the boat and specimen are
weighed and put in one of the specimen compartments
in a copper heating-bar that is
part of the test apparatus. The copper heating-
ba- I ~an -- accommdate a ni;mber of specimem
for simultaneous testing. The vacuum chamber
in which the heating bar and other parts of the
test apparatus are placed is then sealed and evacuated
to a vacuum of at least 7 x iw3 Pa (5 x
torr). The heating bar is used to raise the
specimen compartment temperature to 125°C.
This causes vapor from the heated specimen to
stream from the hole in the specimen compartment.
A portion of the vapor passes into a collector
chamber in which some vapor condenses
on a previously-weighed and independently tem-
E 595
perature-controlled, chromium-plated collector
plate that is maintained at 25°C. Each specimen
compartment has a corresponding collector
chamber that is isolated from the others by a
compartmented separator plate to prevent cross
contamination. After 24 h, the test apparatus is
cooled and the vacuum chamber is repressurized
with a dry, inert gas. The specimen and the
collector plates are weighed. From these results
and the specimen mass determined prior to the
vacuum exposure, the percentage TML and percentage
CVCM are obtained. Normally, the reported
values are an average of the percentages
obtained from three samples of the same material.
NOTE 2-It is also possible to conduct infrared and
other analytical tests on the condensates in conjunction
with mass-loss tests. Sodium chloride flats may be used
for infrared analysis. These flats are nominally 24 mm
(1 in.) in diameter by 3.2-mm (0.125-in.) thick, and are
supported edgewise in a metal holder that fits into the
collector plate receptacle. On completion of the test,
the flats are placed into an infrared salt flat holder for
examination by an infrared spectrophotometer. As an
altemative method, the condensate may be dissolved
from the metallic collector, the solvent evaporated, and
the residue deposited on a salt flat for infrared tests.
Sodium chloride flats shall not be used for CVCM
determinations.
4.3 After the specimen has been weighed to
determine the TML, the WVR can be determined,
if desired, as follows: the specimen is
stored for 24 h at 23°C and 50 % relative humidity
to permit sorption of water vapor. The specimen
mass after this exposure is determined.
From these results and the specimen mass determined
after vacuum exposure, the percentage
WVR is obtained.
4.4 Three empty specimen chambers and collector
plates in the heater bar, selected for each
test at random, can be used as controls to ensure
that uniform cleaning procedures have been followed
after each test.
4.5 A typical test apparatus can have 24 specimen
chambers with 24 associated collector
plates so that a number of specimens of different
types can be tested each time the foregoing o p
erations are conducted. Three specimen compartments
can serve as controls and three can be
used for each type of material being tested. The
total time required for specimens requiring no
' Muraca, R. E, and Whinick, J. S., 'Polymers for Spacecraft
Applications," SRI Project ASD-5046, NASA CR-89557, N67-
40270, Stanford Research Institute, September, 1967.
40 1

~
prior preparation is approximately 4 days. The
equipment should be calibrated at least once a
year by using previously tested materials as test
specimens.
4.6 The apparatus may be oriented in any
direction as long as the configuration shown in
Fig. 1 is maintained and bulk material does not
fall from the sample holder nor obstruct the gasexit
hole. The dimensions for critical components
given in Fig. 2 and Table 1 are provided so
that apparatus constructed for the purpose of this
test may provide uniform and comparable results.
5. Significance and Use
5.1 This test method evaluates, under carefully
controlled conditions, the changes in the
mass of a test specimen on exposure under vacuum
to a temperature of 125°C and the mass of
those products that leave the specimen and condense
on a collector at a temperature of 25°C.
5.2 Comparisons of material outgassing prop
erties are valid at 125°C only. Samples tested at
other temperatures may be compared only with
other materials which were tested at that same
temperature.
5.3 The measurements of the collected volatile
condensable material are also comparable
and valid only for similar collector geometry and
surfaces at 25°C.
5.4 The simulation of the vacuum of space in
this test method does not require that the pressure
be as low as that encountered in interplanetary
flight (for example, lo-'* Pa ( torr)).
It is sufficient that the pressure be low enough
that the mean free path of gas molecules be long
in comparison to chamber dimensions.
5.5 This method of screening materials is considered
a conservative one. It is possible that a
few materials will have acceptable properties at
the intended use temperature but will be eliminated
because their properties are not satisfactory
at the test temperature of 125°C. Also, materials
that condense only below 25°C are not detected.
The user may designate additional tests to qualify
materials for a specific application.
5.6 The determinations of TML and WVR
are affected by the capacity of the material to
gain or lose water vapor. Therefore, the weighing
must be accomplished under controlled conditions
of 23°C and 50 % relative humidity.
5.7 Alternatively, all specimens may be put
E 595
into open glass vials during the 24-h temperature
and humidity conditioning. The vials must be
capped prior to removal from the conditioning
chamber. Each specimen must be weighed within
2 min after opening the vial to minimize the loss
or absorption of water vapor while exposed to an
uncontrolled humidity environment. While control
of humidity is not neceSSary at this point,
the temperature for the weang should be controlled
at 23T, the same temperature prescribed
for the 24-h storage test.
6. Apparatus
6.1 The apparatus used in the determination
of TML and CVCM typically contains two resistance-heated
copper bars. Generally, each bar
is 650 mm (25.5 in.) in length with a 25-mm (1-
in.) square cross section, and contains 12 specimen
chambers. The open section of each specimen
chamber allows vapors from the specimen
to pass through a hole into a collector chamber
where it impinges on a removable chromiumplated
collector plate maintained at 25°C
throughout the test. (See Figs. 1 and 2.) Variations
in test apparatus configurations are acceptable
if critical dimensions are maintained as prescribed
in Table 1.
6.2 Typically, a total of 24 specimen chambers
is used for testing during a 24-h vacuum operation;
three of the chambers are maintained as
controls. The test apparatus can be mounted on
the base plate of a vacuum system within a
narrow vacuum bell, 260 mm (10% in.) in diameter,
that rests on a specially adapted feedthrough
collar, also supported by the base plate.
6.3 The operation of the vacuum chamber
system and any device for raising the vacuum
bell can be automatically controlled. Power to
the heating element mounted in the copper bars
is generally controlled by variable transformers
through temperature controllers. Recorders with
an electronic icepoint reference junction feedback
may be used to monitor the heater bar
temperatures. A heat exchanger using a suitable
fluid may be used to maintain the collector plate
at 25°C during the test.4
6.4 It is recommended that the vacuum chamber
system include automatic controls to prevent
' Detailed drawings for a typical installation are available at
a nominal cost from ASTM Headquarters, 19 16 Race St., Phila.,
Pa. 19103. Request Adjunct No. 12-505950-00.
-
402

E 595
damage in the event of power failure or cooling
fluid supply failure when in unattended operation.
Care must be taken to prevent backstreaming
of oil from vacuum or diffusion pumps into
the vacuum chamber.
7. Test Specimen
7.1 Finished products (for example, elastomers,
hardware, and structural parts) are cut into
small pieces on the order of 1.5 to 3.0-mm (*/M
to %-in.) cubes to fit into the specimen boat.
Boats approximately 10 by 6 by 12 mm (3/8 by
Y.4 by l/2 in.) have been found satisfactory.
7.2 Products that require compounding are
normally mixed in 10-g batches to ensure representative
samples. Materials shall be cured as
sheets, thin slabs, or thicker sections to simulate
application in actual use; then they shall be sectioned
in accordance with the foregoing dimensions
for specimen cubes.
7.3 Adhesive tapes shall be applied to a surface,
such as a preweighed aluminum ring or foil,
to simulate actual use. Paints can be applied to
aluminum foil by brushing, dipping, or spraying
to approximate the as-used thickness, then cured
before testing. A paint can also be cured on an
inert surface such as TFE-fluorocarbon, removed
as a film, and treated as bulk material. Some
adhesives or sealants may be applied to preweighed
aluminum foil and cured.
7.4 Greases shall be placed into a boat. Liquids
shall be placed directly in a boat or absorbed
in an ignited neutral filler such as asbestos or
silica and then placed in a boat. The technique
used shall be stated in the report. Liquids and
greases, especially silicones, are prone to creep; if
the material exhibits creep to such an extent that
some flows out of the boat, the test results shall
be disregarded.
7.5 Minimum specimen masses in the order
of 200 mg are required. If smaller quantities are
utilized, the accuracy of the measurements may
be impaired.
7.6 It is absolutely essential that specimen materials
not be contaminated at any step in the
specimen fabrication process. Most importantly,
specimen material shall not be handled with the
bare hands as oils from human skin are volatile
and condensable and thus will cause false TML
and CVCM results.
7.7 The following specimen handling procedures
are recommended to control contamina-
tion:
7.7.1 Wear suitable gloves or finger cots during
all specimen preparation steps.
7.7.2 All previously prepared materials can be
assumed to be contaminated in the “as-received”
condition; and must be cleaned.
7.7.3 Use cleaning solvents that are known to
be nonreactive with the specimen material and
that are known to leave no residue.
7.7.4 When possible, discard exterior surfaces
of materials when preparing specimens. A clean
razor blade can be used to shave off exterior
surfaces of rubbers, foams, and other soft materials.
Exterior surfaces of harder materials can be
removed with a clean jewelers’ saw. A clean
jewelers’ drill can be used to remove specimen
material from the center part of material suspected
of being contaminated.
8. Procedure
8.1 Weigh a prepared aluminum foil boat and
return it to its storage beaker in a glass desiccator
utilizing silica gel desiccant.
8.2 Weigh a prepared collector and mount it
into its cooling-plate receptacle.
8.3 Add the test specimen (100 to 300 mg) to
the boat and condition the sample at 50 % relative
humidity and 23°C for a minimum of 24 h.
8.4 Weigh the conditioned specimen (see 4.6)
using a balance having f 1 pg sensitivity.
8.5 Place the specimen and boat into a specimen
compartment of the heating bar in the microvolatile
condensable sy~tem.~
NOTE 2--Prior to the operation noted in 8.5, the
copper compartment bar, separator, and cooling plate
shall be clean, in position, and awaiting the specimen
boats and collector plates.
8.6 Mount and screw down the respective
cover plates onto the entry end of each specimen
compartment.
8.7 Close the vacuum system and evacuate it
to 7 x Pa (5 x lo-’ torr) or less within 1 h,
using proper operating procedures.
8.8 Control of the collector plate temperature
at 25°C shall be achieved within the first hour of
pumpdown.
8.9 When a pressure of 7 x Pa (5 x IO-’
torr) is reached, turn on the heater bar and adjust
the variable transformers to raise the heater bar
temperature to 125°C within 60 min. Temperature
controllers should maintain bar temperatures
at 125°C.
403

8.10 Maintain the collector plate temperatures
at 25°C.
8.11 Maintain the heater bar temperature at
125°C for 24 h, then close the high vacuum valve
to the pumping system and turn off the heater
bar current.
8.12 Open the vent valve and backfill with
clean, dry nitrogen regulated within a gage pressure
range from 10 to 30 Wa (2 to 4 psi) above
atmosphere to cool the bars rapidly.
8.13 Allow the heater bar to cool sufficiently
to permit handling (nominally 2 h to reach 50'C).
Then turn off the collector-plate heat exchangers,
return the vacuum chamber to room pressure
using the clean, dry nitrogen, and open the chamber.
8.14 Store aluminum boats with specimens
and respective collector plates in desiccators (using
active silica gel desiccant) immediately. After
specimens have cooled to approximately room
temperature, but no longer than '/2 h, remove
and weigh each specimen within 2 min of its
removal from the desiccators. Control collector
plates are used to detect cross contamination or
poor technique. Mass loss of greater than 20 pg
by a control is usually due to poor preparation
and cleaning of the collector plate. Mass gain of
greater than 50 pg is an indication of poor cleaning,
poor bake-out of the heater assembly, cross
contamination, or poor vacuum technique. Any
change of 50 pg (0.05 % of a 100-mg sample
mass) or greater is reason for concern and for a
review of or change in techniques. All data acquired
during runs when this occurs shall be
discarded or retained with a note indicating the
discrepancy.
8.15 Return the foregoing samples to the relative
humidity chamber for 24 h if the WVR is
to be determined. Weigh the conditioned specimens
(see 5.6).
NWE 3-Annex Ai contaifis rmommended cieaning
and storage procedures.
9. Calculations
9.1 Calculate TML as follows:
Initial Mass, g
Final Mass, g
Specimen and Si + Bi SF Bi
boat
Boat BI Bi
Specimen alone (Si + BI) - (SF + Bi) -
Bi = Si
BI = SF
Difference or L = SI - SF
mass loss L/Si X 100 = % TML
Initial Mass, g
Final Mass, g
Specimen on alu- Sl+AI1+& SF + A11 4- &
minum foil
and boat
Aluminum foil All + B, All+ B1
and boat
Specimen alone (Si + A11 + BI) - (SF + A11 + BI) -
(Ah + Bi) = SI (AI1 + BI) SF
Difference or L = SI- SF
mass loss
L/Sf X 100 = % TML
9.2 Calculate CVCM as follows:
Final mass, g, collector plate and condensables, CF
Initial mass, g, collector plate, C1
Mass, g, condensables CO = CF - CI
Condensable mass, g
(G) X 100 = % CVCM
Initial specimen mass, g SI
9.2.1 A correction may be made using control
collector plates when calculating CVCM. This
correction is recommended but not required unless
an excessive mass change occurs as described
in 8.14.
cs = c, - c,
where:
CS = change in mass of control collector plate,
g
CCF = final mass of control collector plate, g,
and
CcI = initial mass of control collector plate, g.
9.3 Calculate WVR as follows:
Reconditioned mass, g, specimen and boat after 24 h at 50 %
relative humidity, SF'
Mass regain&, g SF' - SF = % WVR
Initial specimen mass, g ( SI )
9.4 Calibrate the balance periodically (at least
every 6 months) and apply the appropriate calibration
factors.
10. Report
10.1 The report shall contain the following
information:
IO. I. I Trade name a d iitimki of the material,
the manufacturer, the batch or lot number,
or other such identification.
10.1.2 Summary of the preparation schedule
(mixing proportions, cure time and temperature,
postcure, cleaning procedures), date prepared.
10.1.3 Number of samples (nominally three
for each material).
10.1.4 Samples configuration (size, shape,
etc.). Statement of technique used in handling
liquids or greases (see 7.4).
10.1.5 Statement of sample test temperature
404

( 125”C), collector plate temperature (25”C), and
duration of test and dates of test.
10.1.6 Initial mass of conditioned samples, SI.
10.1.7 Mass of samples as taken from test
chamber, SF.
10.1.8 Final mass of samples after optional
reconditioning for 24 h at 50 % relative humidity
and 23”C, SF’, if WVR determination is conducted.
10.1.9 Percentage of total mass loss, TML
(normally three values for each material and the
average value).
10.1.10 Percentage of water vapor regained,
WVR (normally three values for each material
and the average value), if determined.
10.1.11 Initial mass of the dried collector
plates, C,.
10.1.12 Change in mass of the control collector
plate, Cs, in grams.
10.1.13 Final mass of the collectors, CF.
10.1.14 Percentage of collected volatile condensable
material, CVCM (normally three values
for each material and the average value).
10. I. 15 Infrared spectrum or other analytical
description of the condensed contamination
when determined.
10.1.16 Remarks about any noticeable incident
or deviation from standard conditions observed
during the test.
E 595
11. Precision and Bias
11.1 Bias for this test method has not been
determined.
1 1 .2 Precision of these measurements was established
by interlaboratory tests of 17 materials
by 5 organizations. Precision for particular materials
is affected by the nature of the material as
well as testing variance. For example, monolithic,
homogeneous materials with relatively low TML
and CVCM values will have high precision and
low standard deviation. Materials that are mixed
and cured individually before testing may not be
homogeneous or completely comparable from
organization to organization. Despite such possible
variations, the test can successfully identify
“good” and “bad” lots of materials, and screen
out relatively low outgassing materials from relatively
high outgassing materials. For example,
Celcon acetyl polymer was tested and found to
have an average value of 0.5336 f 0.0832 and
an average CVCM value of 0.0394 f 0.0342 for
the five laboratories. Epon 828/V125 had an
average TML value of 0.4068 k 0.18 19 and an
average CVCM value of 0.0128 f 0.0082. Precison
for this method is +- 10 % (95 % confidence
level) for TML and f20 % for CVCM (95 %
confidence level).
1 1.3 No precision has been estimated for
WVR as of yet.
405

TABLE 1 Test Apparatus Dimensions (See Fie.2)
Letter mm Tolerance in. Tolerance Notes
AA
k0.005 diameteP
BA
io.005 diameter"
CA
DA*c
EA,C
FA,C
GC
HA
JA
K
L
M
N
P
Q
R
S
T
U
V
W
X
Y
Z
6.3 *o. I
11.1 *o. I
33.0 *o. I
13.45 *o. 10
9.65 *o. 10
0.65 *0.10
7. I +0.3
0.75 kO.10
12.7 A0.3
1.6 M.8
8.0 kO.8
16.0 333. I
16.0 *0.8
32.0 rtO.8
50.0 kO.8
25.5 *0.8
0.4 k0.3
12.0 *0.8
25.5 k0.8
25.5 20.8
50.0 kO.8
6.0 kO.8
25.0 kO.8
I .6
kO.8
0.250
0.438
1.300
0.531
0.380
0.026
0.50
0.030
0.500
%6
%6
0.625
'h
1 1/4
2
I
0.0 I5
'h
I
I
2
Y4
1
%6
333.005 diameter"
M.005
k0.005
lt0.005
333.0 I
*0.05 stock size
*o.o 10
*%2
f %2
k0.005
k v32
*%2
k1/32
cover plate must fit snugly
*0.010 half stock thickness
&/32
* Y32
*v32
fV32
*%2
*'/32
*I/32
radius, typical
A Critical dimensions that must be maintained for test results to be comparable.
Diameters must be concentric to *O. 1 mm (+0.005 in.) for test results to be comparable.
Dimensions include plating thickness. Satisfactory surfaces have been produced by making substrate surface finish, 1.6 pm
RMS (63 pin. RMS), highly polished, plated with electroless nickel, 0.0127-mm (0.0005-in.) thick, and finished with electroplated
chromium, 0.005 I -mm (0.0002-in.) thick.
OOLlNG PLATE
COLLECTOR
CHAMBER
COMPARTMENT
COPPERHEATERBAR
SEWRATOR PLATE
FIG. 1 Schematic of Critical Portion of Test Apparatus
(Section A-A of Figure 2)
406

E595
I
FIG. 2 Critical Portion of Test Apparatus (See Table 1 for Dimensions)
407

Cleaning
.2 I. I. 1 General-The components shall be cleaned
after fabrication to remove any residual oils, etc., from
the fabrication process. The cleaning operations in
A 1.1.2 through A I. 1.9 shall be performed before each
test run unless otherwise specified.
A1 . li
A 1.1.2 Aluminum Boats-Vapor degrease the boats
for 5 or more min. A l:l:l by volume chloroform:acetone:ethanol
solvent blend has been used successfully
for this purpose. Dry the boats at 125 k 5°C
for at least 4 h.
A 1.1.3 Collector Plates-Immerse and agitate collector
plates in the solvent. Follow this with vapordegreasing
for 15 min. A 1:1:1 by volume chloroform:acetone:ethanol
solvent blend has been used successfully
for this purpose. Dry the collectors for 4 h
minimum at 125 & 5°C.
A 1.1.4 Specimen Chamber and Heating Bar-Take
special care with the bar between test runs to avoid
contamination during subsequent tests. Wash the bar
cavities and surface with a suitable solvent. A I:l by
volume acetone:ethanol solvent blend has been used
successfully for this purpose. Mount the bar into the
system without specimens. Evacuate the system to 1 x
10-4 Pa (I x IO- torr) and degas the bar at 150" k 5°C
for 4 h minimum. This is 25°C above the normal test
temperature. Then turn off the heater to the bar and
allow the bar to cool under vacuum. Leave the heater
chamber bar in place in the vacuum system. It need
only by removed after the test for recleaning. The
vacuum system can be configured to close off the bell
volume, if necessary, thus permitting the vacuumpumping
system to be off over a weekend.
A 1.1.5 Separator Plate-Wash the separator plate
with a suitable solvent. A I:] by volume acetone:ethanol
solvent blend has been used successfully
for this purpose. Use filtered dry nitrogen gas to remove
particulates and to evaporate solvents.
A 1.1.6 Collector Plate Support-Following the system
degassing described in A 1.1.4, wipe the collector
plate support using a suitable solvent. Ethanol has been
used successfully for this purpose.
A 1.1.7 Vacuum Bell-Poor vacuum is frequently
caused by materiai outgassing from the intemai bell
surface. Wipe down the bell interior with a suitable
solvent as required to restore vacuum-operating efi-
ANNEX
Al. CLEANING AND STORAGE
ciency. Ethanol has been used successfully for this
purpose.
A 1.1.8 Other Items-Various other items such as
brackets and standoffs can be cleaned as required by
wiping with a suitable solvent. A l:1 by volume acetone:ethanol
solvent blend has been used successfully
for this purpose.
A 1.1.9 Cleaning Materials-All wiping materials
and swabs shall be preextracted using solvents with
which they will be used. (See Note Al.) All solvents
shall be of spectro-grade or equivalent purity. The
nitrogen gas shall be 99.9 % pure, or better, and shall
have a dew point of -60°C (-76°F) or less. The gas
shall be filtered using a Molecular Sieve SA or equivalent.
Metal tubing (for example, stainless steel or cop
per) that is used for gas transfer shall be cleaned before
Use.
NOTE A 1-A recommended extraction procedure
for cleaning wiping material is a 24-h treatment in a
Soxhlet extractor charged with a mixture of 90 % chloroform:
IO % ethyl alcohol.
A1.2 Storage
A 1.2.1 Boats-After cleaning, the boats can be
placed in 5-cm3 beakers with designated compartment
numbers, then stored in a desiccator that contains
indicating silica gel. Seal the unit with a low-vapor
pressure grease for ground glass joints. The boats shall
be weighed within one day of being stored.
A1.2.2 Collector Plates-The plates can be
mounted on a circular plate rack and stored in a desiccator
that contains indicating silica gel. Seal the unit
with a low-vapor pressure grease for ground glass joints.
Plates shall be weighed within 1 day of being stored.
A1.2.3 Handling and Storage-Due to the nature
of this method, it is imperative that good cleaning
procedures be followed to minimize handling of cleaned
parts and the introduction of contaminants after cleaning.
Hence, all components that have been cleaned
must be stored in such a manner as to maintain their
clean state.
A1.2.4 Vacuum System-Perform periodic maintenance
in accordance with the manufacturer's recommended
practices in order to ensure good vacuum
system performance.
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject IO revision at any time by the responsible technical committee and must be reviewed everyjive years and
if not revised, either reupproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical commi:?ee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards. 1916 Race St., Philadelphia, Pa. 19103.
408

@ E595
APPENDIX
(Nonmandatory Information)
XI. TEST REPORTING FORM
X 1.1 The following format is suggested for reporting raw data and test results.
OUTGASSING DATA SHEET
Material: (name, part number, lot, etc.)
Description: (material type, sample form, color, etc.)
Condition: (mix and cure, pre or post condition, as received, on substrate, etc.)
Manufacturer:
Requestor:
Date:
Location:
Charge No.:
Telephone:
Blanks:
Heater Position No. ( ) ( ) ( )
Initial holder mass, g ---
Final holder mass, g ---
Initial collector mass, g ---
Final collector mass, g ---
Sample:
Heater Position No. ( ) ( 1
Initial holder mass, g
---
Initial holder plus sample ---
Final holder plus sample ---
Reweighed sample plus holder, 24 h 50 % RH, g" ---
Initial collector mass, g ---
Final collector mass, g ---
~otal mass loss (TML) % ---
Ave. % TML
Total mass gain (CVCM) %
Total water regained"
(Sample WVR)
---
Ave. %
CVCM
---
Ave. % WVR
A WVR measurement is optional
Remarks: (Sample appearance, collector appearance after test, any test anomalies, non-standard conditions,
problems, etc)
Date test begun:
Sample temperature, "C:
Collector temperature, "C:
Date test completed:
Pressure torr:
Time at test temperature hours:
Operator signature:
409

ab
Designation: G 26 - 84
AMERICAN SOCIETY FOR TESTING AND MATERIALS
1916 Raw St., Philadelphia, Pa. 19103
Repriitted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Practice for
OPERATING LIGHT-EXPOSURE APPARATUS (XENON-ARC
TYPE) WITH AND WITHOUT WATER FOR EXPOSURE OF
NONMETALLIC MATERIALS'
This standard is issued under the fixed designation G 26; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. scope
1.1 This practice covers the basic principles
and operating procedure for water- or light-exposure
apparatus, or both, employing a xenonarc
light source.
NOTE 1-This practice combines the practices previously
referred to as G 26 and G 27. Recommended
Practice G 27, for Operating Xenon-Arc Type Apparatus
for Light Exposure of Nonmetallic Materials', is
to be discontinued since it is now covered in this edition
of G 26 under Methods C and D.
NOTE 2-Attention is called to Recommended
Practice G 23, for Operating Light- and Water-Exposure
Apparatus (Carbon-Arc Type) for Exposure of
Nonmetallic Materials: and IS0 Recommendation
No. 759, Document ISO/TC 61 (Secretariat).'
1.2 This practice does not specify the exposure
conditions best suited for the material to be
tested, but is limited to the method of obtaining,
measuring, and controlling the conditions and
procedures of the exposure. Sample preparation,
test conditions, and evaluation of results are covered
in ASTM methods or specifications for specific
materials.
1.3 This practice includes four methods:
1.3.1 Method Z-Continuous exposure to
light and intermittent exposure to w&er spr~y.
1.3.2 Method 2-Alternate exposure to light
and darkness and intermittent exposure to water
spray.
1.3.3 Method 3-Continuous exposure to
light without water spray. Exposure conditions
are characteristic of those specified by AATCC
Test Method 16E 1976.
1.3.4 Method 4-Alternate exposure to light
and darkness without water spray. Exposure conditions
characteristic of those natural conditions
experienced when exposing are in accordance
with Practice G 24.
I .4 This practice may involve hazardous operations
and equipment. This practice does not
purport to address all of the safety problems associated
with its use. It is the responsibility of
whoever uses this practice to consult and establish
appropriate safety and health practices and determine
the applicability of regulatory limitations
prior to use.
1.5 The values stated in SI units are to be
regarded as the standard. The inch-pound equivalents
of the SI units may be approximate.
2. Applicable Documents
2.1 ASTM Standard:
G24 Practice for Conducting Natural Light
Exposures Under Glass2
2.2 AATCC Standard:
Method 16E 1976 Colorfastness to Light, Water-cooled
Xenon-Arc Lamp Continuous
Light4
2.3 CIE Standard:
No. 20 Recommendations for the Integrated
Irradiance and the Spectral Distribution of
' This practice is under the jurisdiction of ASTM Committee
G-3 on Durability of Nonmetallic Materials and is the direct
responsibility of Subcommittee G03.03 on Simulated and Controlled
Environmental Tests.
Current edition approved Aug. 3 I, 1984. Published November
1984. Originally published as E 239 - 64T. Redesignated
G 26 in 1970. Last previous edition G 26 - 83.
'Annual Book ofASTM Stadirds, Vol 14.02.
Available from the American National Standards Institute,
1430 Broadway, New York, N.Y. 10018.
'Available from The secretary, American Association of
Textile Chemists and Colorists, P.O. Box 12215, Research Triangle
Park, N.C. 27709.
410

G 26
Simulated Solar Radiation for Testing
purposes5
3. Significance and Use
3.1 Several types of apparatus with different
exposure conditions are available for use. No
single operating procedure for lightexposure a p
paratus with and without water can be specified
as a direct simulation of natural exposure. This
practice does not imply expressly or otherwise an
accelerated weathering test.
3.2 Since the natural environment varies with
respect to time, geography, and topography, it
may be expected that the effects of natural exposure
will vary accordingly. All materials are
not affected equally by the same environment.
Results obtained by use of this practice should
not be represented as equivalent to those of any
natural weathering test until the degree of quantitative
correlation has been established for the
material in question.
3.3 Variations in results may be expected
among instruments of different types or when
operating conditions among similar type instruments
vary within the accepted limits of this
practice. Therefore, no rderence should be made
to results from use of this practice unless accompanied
by the report form shown in Fig. 1 or
unless otherwise specified in a referenced procedure.
4. Apparatus
4.1 Water-Cooled Type!
4.1.1 The apparatus employed should utilize
a water-cooled xenon-arc lamp as the source of
radiation and should be one of the following
general types, or their equivalent:
4.1.1.1 Type A-An exposure apparatus in
which the source of radiant energy shall be a
water-cooled xenon-arc vertically located at the
central axis of either a 508-mm (204x1.) diameter
vertical specimen rack, or of a 648-mm (25.5-
in.) diameter inclined rack. Means shall be provided
for automatic programming of temperature
and cycles. Means shall be provided for
adjustment of relative humidity. The specimen
rack shall rotate at 1 2 0.1 rpm.
NOTE 3-In the commercial descriptions of the four
types, the term “cycle” is defined as each time interval
of light, darkness, and water spray that is specified
differently in accordance with the different testing
methods.
4.1.1.2 Type AH-The exposure apparatus
shall be identical to Type A except it shall have
automatic humidity control.
4.1.1.3 Type B-An exposure apparatus in
which the source of radiant energy shall be a
water-cooled xenon-arc vertically located at the
central axis of a 960-mm (37.75-in.) diameter
specimen rack. Means shall be provided for automatic
programming of temperature and cycles.
Means may be provided for adjustment of humidity.
The specimen rack shall rotate at 1 +. 0.1
rpm-
4.1.1.4 Type BH-The exposure apparatus
shall be similar to Type B except it shall have
automatic humidity control.
4.1.2 The xenon-arcs employed shall be of the
“long arc” water-cooled type operated through
suitable reactance transformers and electrical
equipment from a 50 or 60-Hz power supply.
They shall employ cylindrical inner and outer
optical filters to direct the flow of cooling water
and to simulate a designed spectral energy distribution.
4.1.2.1 For the purpose of this practice, the
xenon-arc lamp shall consist of a quartz xenon
burner tube and one of the following optical filter
combination^:'*^
(a) Borosilicate glass inner and outer optical
filter to simulate the spectral power distribution
(SPD) of natural daylight throughout the actinic
region.
(b) Infrared absorbing glass inner optical filter
with quartz outer optical filter to simulate the
SPD of natural daylight (300 to 1000 nm).
(c) Borosilicate glass inner optical filter with
soda lime glass outer optical filter to simulate the
SPD of natural daylight (actinic wavelengths)
filtered through window glass.
(d) Infrared absorbing glass inner and outer
optical filter to simulate the SPD of natural day-
’ Available from Secretary, U.S. National Committee, CIE,
?Wlcna! B me of S&ndards, Gai!hershxg, MD 20899.
Available from Atlas Electric Devices Co., 41 14 N. Ravenswood
Ave., Chicago, Ill. 60613. Model 25-W meets the requirements
of Type A. Models 25-WT and 25-WR meet the requirements
of Type AH apparatus. Model 65-W, 65-SMC, 65-DMC,
and 65-XW meet the requirements of Type B. Models 65-WR,
65-WRC, 65-SMC-R, 65/SMC-RC, 65-DMC-R, 65-DMC-RC,
65-XW-R and 65/XW-RC meet the requirements of Type BH
apparatus.
’ Norton, Kiuntke, and Connor, Canadian Textile Journal,
CTJOA, May 1969.
‘Corning 7740 Pyrex0 (borosilicate), Coming 4601 IR ab
sorbing visible transmitting, Kimble R6 soda lime glass tubing,
and General Electric GA-204 quartz tubing of proper dimensions
have been found suitable for use as xenon-arc optical
filters. Available from Atlas Electric Devices Co., 41 14 N. Ravenswood
Ave., Chicago, Ill. 60613.
41 1

eb
light (310 to 1000 nm) filtered through window
sl=.
(e) Quartz inner and outer optical filter to
approximate sunlight intensities unfiltered by the
earth's atmosphere.'
4.1.2.2 To prevent loss in levels of irradiance
due to excessive solarization and to prevent possible
breakage caused by stresses in optical filters
exposed to high-intensity UV energy, inner op
tical filters9 shall be replaced periodically. Suggested
intervals are 300 and 400 h for Types A
and B, respectively. The outer optical filter shall
be replaced after 1500 and 2000 h for Types A
and B, respectively.
4.1.3 Distilled or deionized water should be
recirculated past the burner at a flow rate SUEcient
to remove excess heat. Passing water
through a cartridge demineralizer installed in the
recirculation line just ahead of the lamp minimizes
contamination of the quartz envelope of
the burner. A heat-exchange unit should be used
to cool the recirculated lamp water.
4.1.4 Since xenon-arc lamps, like all gas discharge
lamps, will have a progressive drop in
radiation output with continued use, and since
optical filters will change in their transmission
characteristics, provision shall be made in the
apparatus (automatically or manually) for progressively
increasing the wattage of the lamp to
minimize changes in the intensity of the radiation
at the face of the sample. The greatest change in
both the xenon burner tube and optical filters
occurs in the first 20 h of use. For this reason,
burners and optical filters preaged by the instrument
manufacturer are recommended for critical
testing when a more rapidly changing rate of
intensity is undesirable. For routine testing on a
comparative basis, the 20 h of preaging may be
omitted.
4.1.5 Many nonmetallic materials are selectively
absorbing. The energy that a molecule
absorbs depends upon the wavelength of the
incident radiation." It is desirable to monitor the
level of irradiance of the photochemically effective
wavelengths if intercomparisons are to be
made among samples not exposed simultaneously.
Samples may then be exposed to known
amounts of irradiation, the time integral of irradiance.
4.1.5.1 Where radiometers capable of monitoring
discrete portions of a continuous spectrum
are available, exposure to a mutually agreedupon
level of irradiation may be specified as the
412
G 26
exposure interval in place of a time interval.
(a) When using the optical filter combination
described in 4.1.2.1 (a), the suggested minimum
spectral irradiance levels are:
.2 W/m2/nm band at 320 nm
.35 W/m'/nm band at 340 nm
.5 W/m2/nm band at 380 nm
.I5 W/m2/nm band at 420 nm
(b) When using the optid filter combination
described in 4.1.2.1 (c), the suggested minimum
spectral irradiance levels are:
.2 W/m2/nm band at 340 nm
.45 W/m'/nm band at 380 nm
.I W/m'/nm band at 420 nm
(c) Operating at the suggested minimum levels
approximates the average daily solar irradiance
under ideal conditions. It is about half of the
maximum values for total irradiance on a horizontal
plane when the sun is at 90" altitude as
reported in CIE No. 20. When irradiance is monitored
and periodic manual adjustment of wattage
is made to compensate for changes of intensity,
no lamp assembly should be used that cannot
maintain the minimum level of irradiance
within a 10 % tolerance at the monitored wavelength.
Irradiation expressed as joules per square
metre is the product of irradiance x exposure
time in seconds.
4.1 S.2 Xenon-arc type equipment not having
a radiometer shall be operated with periodic increases
in wattage to minimize any drift in levels
of irradiation. Such intervals shall be established
by the parties concerned or follow the suggested
schedule below in 4.1 S.2 (a).
NOTE 4-The use of suggested wattage steps does
not imply that irradiance will be maintained at levels
equivalent to those obtained when employing a light
monitor. They are intended as a guide to minimize the
reduction of UV intensity with maximum lamp longevity
when using either Method A or C for 2.5, 6, or 6.5-
kW lamps, respectively.
(a) The fo1:owing are the suggested wattage
settings for each exposure interval of a 2500-W
xenon burner tube based upon the average performance
of xenon burner tubes with borosilicate
filters:
Time, h
Power, W
0 to 20 I600
20 to 200 I800
Kishii, T., and Ooka, IC. Symposium on Coloured Glasses.
International Comm. on Glass of Czech. Sci. & Tech. SOC. of
the Silicate Industry, 1967.
lo Hawkins, W. L., ed., Polymer Stabihtion, Wiley-Interscience,
1972, p. 166.

G 26
Time, h
Power, W
200 to 400 2000
400 to 600 2250
600 to 800 2500
800 to 1000 2600
1000 to 1200 2800
1200to 1500 3000
(b) The following are the suggested wattage
settings for each exposure interval of a 6OOO-W
xenon burner tube based upon the performance
of xenon burner tubes with borosilicate filters in
Method A:
Time, h
Power, W
0 to 20 min
20 to 100 4750
100 to 250 5000
250 to 400 5250
400 to 550 5500
550 to 700 6000
700 to 850 6500
850 to 1000 7000
(c) The following are the suggested wattage
settings for each exposure interval of a 6500-W
xenon burner tube based upon the average performance
of xenon burner tubes with borosilicate
filters in Method A:
Time, h
Power, W
0 to 20 min
20 to 100 5500
100 to 200 6000
200 to 500 6200
500 to 1000 6500
1000 to 1500 7000
1500 to 2000 7500
2000 and over 8500
4.1.6 In Types A and AH apparatus, specimens
in holders should be positioned as follows:
4.1.6.1 At a distance of 244 f 3 mm (10.0 2
0.125 in.) from the vertical axis of the arc and
with no exposed part of the specimen over 100
mm (4 in.) from a horizontal plane passing
through the center of the arc, or
4.1.6.2 At a distanceof310 k 3 mm (12.25
0.125 in.), which shall be a radius about the
horizontal axis of the lamp at which a nonvertical
inclined rack is tangential, and with no exposed
part of the specimen more than 190 mm (7.5 in.)
from a horizontal plane passing through the center
of the arc.
4.1.7 In Types B and BH apparatus, specimens
in holders or otherwise mounted on the
rack should be positioned as follows:
4.1.7.1 At a distance of 480 f 3 mm (18.875
2 0.125 in.) from the vertical axis of the arc, and
with no part over 230 mm (9 in.) from a horizontal
plane passing through the center of the
arc, or
4.1.7.2 At a distance of 470 f 3 mm (18.5 f
0.125 in.), which shall be a radius about the
horizontal axis of the lamp at which a nonvertical
inclined rack is tangential, and with no exposed
part of the specimen more than 195 mm (7.7 in.)
from a horizontal plane passing through the center
of the arc.
4.1.8 Testing temperatures should be measured
and regulated on the basis of a black panel
thermometer unit mounted on the specimen rack
so that the face of the unit is in the same relative
position and is subjected to the same influences
as the test specimens. The black panel thermometer
unit should consist of a stainless steel panel
about 70 by 50 by 0.95 mm (2.750 by 5.875 by
0.0375 in.), to which a stainless steel bimetallic
dial-type thermometer is mechanically fastened.
This thermometer should have a stem approximately
4 mm (0.16 in.) in diameter with a 44.5-
mm ( 1.75411.) dial. The sensitive portion extending
about 38 mm (1.5 in.) from the end of the
stem should be located in the center of the panel
approximately 64 mm (2.5 in.) from the top and
approximately 48 mm (1.875 in.) from the bottom
of the panel. The face of the panel with the
thermometer stem attached should be finished
with a baked-on black infrared-absorbing coating
having good resistance to light.
4.1.8.1 A thermocouple or resistance bulb
thermometer mounted at the center face of the
black panel, which provides temperature values
equivalent to the dial thermometer, may be substituted.
4.1.9 A blower unit in the base of the apparatus
should provide a flow of air through the
test chamber and over the test specimens. Control
of specimen and black-panel temperature
should be accomplished by thermostatic control
of the temperature of the constant volume of air
from the blower. Black-panel temperatures
should be read through the window in the test
ciramki door withoiii ofiiiiiig the boor.
4.1.10 Apparatus operated as a light- and water-exposure
test shall be equipped with a specimen
spray unit as illustrated in Figs. 2 and 3. All
components of the specimen spray unit should
be fabricated from stainless steel, plastic, or other
material that does not contaminate the water.
Apparatus operated only as a light-exposure test
are not required to have the specimen spray unit
or, if present, it should not be used.
4.1.1 1 Types A, AH, BH, and some Type B
apparatus are equipped with an electrically op
413

eb
erated vaporizing unit for adding moisture to the
air as it passes through the conditioning chamber
in the base section prior to its entry into the test
chamber of the apparatus.
4.1,ll.l In Types A and B, the vaporizing
unit, when manually turned on, may operate
continuously while the apparatus is in operation.
Type A and some Type B apparatus may be
programmed to operate the vaporizer during a
dark cycle only. The temperature of the water,
with which the vaporizer is supplied, is not controlled.
In Type B apparatus not supplied with a
vaporizing unit, the relative humidity within the
test chamber is governed by evaporation of water
in the bottom of the chamber and from water
emitted through the specimen spray unit.
4.1.1 1.2 In Types AH and BH apparatus, op
eration of the vaporizer is controlled automatically
by a wet-bulb thermostat. The temperature
of the water supplied to the vaporizer is regulated
automatically by thermostatically-actuated electric
immersion heaters. Control automatically
shifts between two separate sets of thermostats as
the arc lamp is turned on and off by the program
control unit.
4.1.12 In Types A, B, AH, and BH apparatus
containing vaporizing units, relative humidity is
determined from wet- and dry-bulb thermometers
located in the air stream at the vaporizer's
point of exit from the test chamber.
4.1.12.1 Determine the relative humidity for
Type B apparatus not equipped with a vaporizing
unit from wet- and dry-bulb thermometers
mounted in holders on the specimen rack so that
their sensitive portions are in the same relative
position as the face of the test specimen but
shielded from the radiation.
4.1.12.2 Any apparatus with a vaporizing unit
operated with the unit and immersion heaters
turned off will provide essentially the same conditions
of relative humidity as are produced in
Type B apparatus without a vaporizing unit.
4.1.13 The apparatus shall include means for
measuring the following:
4.1.13.1
4.1.13.2
4.1.13.3
4.1.13.4
Wattage of the xenon-arc lamp,
Irradiance at the specimen rack,
Black-panel temperature,
Dry-bulb temperature (test cham-
bed,
4.1.13.5 Wet-bulb temperature (test chambed,
4.1.13.6 Exposure interval, and
G 26
4.1.13.7 Water spray pressure when applicable.
4.1.14 Where specified, the apparatus shall
include means for regulating or controlling the
following:
4.1.14.1 Wattage of the xenon lamp,
4.1.14.2 Irradiance or irradiation, or both, at
the specimen rack,
4.1.14.3 Temperature (test chamber),
4.1.14.4 Relative humidity (test chamber),
4.1.14.5 Lightdark-spray-humidity-temperature
cycles, and
4.1.14.6 Water spray pressure when applicable.
4.2 Air-Cooled Type:' I
4.2.1 The apparatus employed shall use an
air-cooled xenon-arc lamp as the source of radiation
and should be one of the following types, or
their equivalent:
4.2.1.1 Type C-Air-cooled xenon-arc apparatus,
1500 W, 158-mm (6.2-in.) diameter specimen
rack, with automatic programming of cycles
and humidity. The specimen rack should
rotate at 5.2 k 0.1 rpm.
4.2.1.2 Type D-Air-cooled xenon-arc apparatus,
4500 W, 360-mm (14.2-in.) diameter specimen
rack, with automatic programming of temperature,
cycles, and humidity. The specimen
rack should rotate at 3.7 k 0.1 rpm.
4.2.2 The xenon arcs employed in Types C
and D should be of the medium-pressure, aircooled
type and one or more optical filters shall
be fitted between the light source and the samples
to filter out undesired wavelengths of radiation.
A combination of optical filters recommended
by the manufacturer shall be used to simulate (1)
sunlight in the open, (2) sunlight behind window
glass, or (3) any other simulated solar irradiation
condition desired.
4.2.3 All gas discharge lamps have a progressive
drop in radiant output with continued use.
Although Types C and D minimize this drop in
output, these xenon arcs must still be exchanged
for new ones after 1500 h of use. It is recommended
to exchange the IR-optical filters for new
ones after 3500 h of use. Answering the purpose,
not all seven IR-optical filters of the filter lantern
should be exchanged at the same time but each
I' Available from Quadampen GmbH, 6450 Hanau/Main,
West Gmnany. Domestic distributor is Batson Machinery, Inc.,
P.O. Box 3978, Grcendle, S.C. 28608. Model I50 meets the
requirements of Type C. Model 450 meets the requirements of
Type D.
414

should be exchanged after it has been running
for 3500 h.
4.2.4 Specimen holders should rotate around
the arc, describing a cylindrical surface, so that
specimens may face, or be turned opposite to,
the arc. No part of the specimens shall be above
or below the ends of the arc. Repositioning of
specimens in upper, center, or lower positions
can improve the uniformity of intensity of the
exposure.
4.2.5 Testing temperatures should be measured
and regulated on the basis of a black-panel
thermometer unit that is mounted so that the
face of the unit is in the same relative position
and is subjected to the same influences as the test
specimens. The black-panel thermometer unit
should consist of a stainless steel panel approximately
48 by 200 by 1 mm (1.9 by 8.0 by 0.04
in.), to which a stainless steel bimetallic dial-type
thermometer is mechanically fastened. The temperature
at the center of the panel should be
sensed by the thermometer. The face of the panel
should be finished with a baked-on black glossy
enamel having good stability to light.
4.2.6 A blower unit in the base of the apparatus
shall provide a flow of air through the test
chamber and over the test specimens. Control of
the specimen and the black-panel temperature
should be accomplished by thermostatic control
of the temperature of the constant volume of air
from the blower. Black-panel temperature should
be read through the window in the test chamber
door without opening the door.
4.2.7 The apparatus should be equipped with
a system to spray the specimens uniformly with
water. This system should be of stainless steel,
plastic, or other material that does not react with
or contaminate the water employed.
4.2.8 Relative humidity in the test chamber
should be measured and controlled by a contact
hygrometer. Water should be vaporized and diffused
to enrkh the air with water and produce
the required humidity.
4.2.9 The apparatus shall include equipment
necessary for measuring and controlling the same
parameters as listed for water-cooled xenon arcs.
5. General Procedure
5.1 Check to be sure the apparatus is operating
properly at the start of each test. Check the lamp
operation at 100-h intervals to be sure the burner
tube and optical filters are clean and that they
have not exceeded the maximum recommended
G 26
period of use.
5.2 Program the instrument to operate in the
continuous light-on mode without water spray.
Fill the specimen rack with blanks and the blackpanel
thermometer. Operate the instrument in
this mode while regulating the chamber dry-bulb
temperature to provide the desired black-panel
temperature of 63 f 3°C (145 f 5°F).
5.3 When the chamber dry-bulb temperature
has been regulated, adjust instruments with automatic
humidity control to control the chamber
wet-bulb temperature at the level that will ensure
the desired relative humidity.
5.4 In Types A, B, C, and D apparatus, use
the type and number of spray nozzles (Figs. 2
and 3) recommended by the manufacturer and
operate at a pressure of 124 to 172 kPa ( 18 to 25
psi), measured at the nozzle unless otherwise
recommended. The water shall have a pH of 6.0
to 8.0, contain less than 20 ppm solids, and leave
no deposit or stain on the specimens after continued
exposure in the apparatus. The temperature
of the water should be 16 f 5°C (60.8 f 9"F),
and recirculation of the water shall not be permitted
unless the recirculated water meets the
above requirements. Pass the specimens through
the spray once in each minute or revolution of
the rack during the spray cycle. Allow the water
to strike the test specimens in the form of a fine
spray equally distributed over the specimens.
5.5 The temperature of the rack spray water
should be sufficiently low to reduce the specimen
temperature below the dewpoint when the specimen
is continuously sprayed during a dark cycle.
5.6 Reference Standards:
5.6.1 AA TCC Blue Wool Lightfastness Standard~.~
NOTE 5-The eight standards L-2 to L-9 have been
made by blending wool dyed with the fugitive dye Erio
Chrome Azurole B and wool dyed with the fast dye
Indigosol Blue AGG in different proportions. The
Mended wm!s were spun into yams and the yams
woven into cloths. Each standard is approximately
twice as fast as the next lower numbered standard. It
has been found that when new lots of the standards are
produced, the amounts of the dyes required and the
properties of the two wools in the blends are often
different from those used originally. The dyeing
strengths and blending proportions would therefore be
misleading, and they are intentionally not specified.
5.6.2 Any standard sample established by mutual
agreement between the purchaser and the
supplier.
5.6.3 IS0 Gray Scale for Assessing Change in
415

Color. '*
METHOD A-CONTINUOUS EXPOSURE TO
LIGHT AND INTERMITENT EXPOSURE TO
WATER SPRAY
6. Procedure
6.1 Apparatus shall be Type A, B, AH, BH,
C, or D light-exposure device.
6.2 Program the instrument for continuous
light and intermittent water spray in accordance
with the manufacturer's instructions. Choice of
the program selected will be by mutual agreement
among the interested parties. Historical
convention has established a cycle of 102 min of
light followed by a cycle of 18 min of light and
water spray as a commonly accepted program
that permits the attainment of the maximum
black-panel temperature during the light-only
portion of the cycle.
6.3 In Types AH and BH apparatus, adjust
dry- and wet-bulb temperature controls, humidifier,
and immersion heater controls to maintain
the desired conditions as specified in Section
5.
6.4 In Types A and B with humidifier, humidity
may be adjusted but not controlled.
6.4.1 Type B instruments without a humidifier
must operate with whatever humidity
occurs from the evaporation of water in the
bottom of the test chamber and from specimen
spray.
METHOD B-ALTERNATE EXPOSURE TO
LIGHT AND DARKNESS AND INTERMITTENT
EXPOSURE TO WATER SPRAY
7. Procedure
7.1 Apparatus shall be Type A, B, AH, or BH
light-exposure device
7.1.1 Types AH and BIi apparatus with automatic
humidity csntrois may be operated on
alternate light and dark cycles. Types C and D
may be operated with 18U-deg specimen rotation
per revolution about the lamp.
7.1.1.1 Operation during the light-on cycle
shall be as described in Section 6.
7. I. 1.2 Separate controls for temperatures and
humidification may be adjusted during the dark
cycle for automatic control as the program alternates
from light to dark. In Type BH apparatus,
a rack spray to cool the specimens by wetting the
Unexposed back surface can result in development
of condensation on the exposed specimen
surface during the dark cycle.
7.1.2 Types A, B, AH, and BH may be pro-
0 26
grammed to operate on alternate light and dark
cycles without control of relative humidity.
METHOD C-CONTINUOUS EXPOSURE TO
LIGHT WITHOUT WATER SPRAY
8. Procedure
8.1 Apparatus shall be Types A, B, AH, BH,
C, or D light-exposure devices programmed for
continuous light only, in accordance with the
manufacturers instructions. Optical filters C or
D described in 4.1.2.1 should be used.
8. I. I Adjust the controls on the apparatus so
that the black-panel temperature is 63 f 3°C
(145 f 5°F) and the relative humidity is 30 f
5 % when the xenon lamp is operated at a wattage
that provides 20 AATCC Fading Units of exposure
in about 15 to 25 clock hours. Check at
regular intervals and, when necessary, readjust
the controls to maintain the specified values for
these variables. Target values for black panel
temperature, 20 AATCC Fading Units, and relative
humidity should be 63"C, 20 clock hours,
and 30 %, respectively.
NOTE 6-20 AATCC Fading Units is equivalent to
a 1.5 f 0.2 ANLAB(40) unit change in Blue Wool L-4
(#4 on the IS0 Gray Scale). Irradiation of about 110
H/m2 (1.5 W/mZ.20-h exposure) at 420 nm has been
found sufficient to produce the specified condition.
8.1.2 Expose the material to be tested as determined
by mutual agreement among the concerned
parties or, when not otherwise specified,
in accordance with one of the following:
8.1.2.1 Versus One AA TCC Blue Wool Light-
.fastness Standard-Expose the test specimen and
any mutually agreed-upon AATCC Blue Wool
Lightfastness Standard until the selected standard
between its exposed and unexposed portion exhibits
a color change equal to Step 4 of the IS0
Gray Scale. Report the results by any mutually
agreed-upon method of measuring change in the
test specimen.
8.1.2.2 Versus Set of AATCC Blue Wool
Lightfastness Standards-Expose the test specimen
and a set of AATCC Blue Wool Lightfastness
Standards until a maximum permissible
amount of change, as determined by any specified
or mutually agreed-upon method of measurement,
occurs in the test specimen. Assign it
'*Reference DraR Is0 Recommendation No. 177, Document
ISO/TC-38 (Secretariat 102) 186. Scales with instructions
for use are available from Is0 member bodies in the various
countries of the world. In the USA they may be obtained from
The Secretary, American Association of Textile Chemists and
Colorists, P.O. Box 122 IS, Research Triangle Park, N.C. 27709.
416

G 26
a classification number equal to that of the numbered
standard that most nearly exhibits a change
in color equal to Step 4 on the IS0 Gray Scale
between its exposed and unexposed portion.
Where one standard shows a color change greater
than Step 4 and the next higher number standard
shows less than a Step 4 color change, an intermediate
or half-grade rating may be used.
8.1.2.3 Versus Other Standard Sample--Expose
the test specimen and any mutually agreedupon
standard sample until either, by any specified
or mutually agreed-upon method of measurement,
shows an agreed-upon amount of
change. Report the results on the basis of a
comparison of the specimen with the standard
sample.
METHOD D-ALTERNATE EXPOSURE TO
LIGHT AND DARKNESS WITHOUT WATER
SPRAY
9. Procedure
9.1 Apparatus shall be Types A, B, AH, or BH
programmed to predetermined cycles of light and
darkness by turning off the xenon arc, or apparatus
shall be Type C and D programmed for
light and dark cycles by rotating the exposed face
of the specimen 180 deg away from the arc. The
method will be determined by the apparatus used
and results may not be comparable between the
two.
NOTE 7-Type B instruments not equipped with a
vaporizing unit do not meet the requirements of
Method D. In Type A and Type B apparatus with
intermittent blower operation during the light-off cycle
and the atomizer in continuous operation, the test
chamber air temperature will drop to that of room air
less the heat removed by vaporation of water from
wicks and atomizer.
9.1.1 Unless otherwise specified, exposure
conditions shall be identical to Method B except
that during the light-on cycle the equilibrium
condition for relative humidity shall be 35 k 5 %
and during periods of darkness equilibrium conditions
shall be 90 f 5 % relative humidity at a
dry-bulb temperature of 35 k 3°C (95 & 5°F).
10. Report
10.1 The report shall include the following:
10.1.1 Type and model of exposure device,
10.1.2 Type of light source and wattage,
10.1.3 Type and age of filters,
10.1.4 Spectral irradiance at sample location,
W/m2-nm (see Note 9),
10.1.5 Irradiation, kJ/m2,
10.1.6 Elapsed exposure time, h,
10.1.7 Light- or dark-water-humidity program
employed,
10.1.8 Operating black-panel temperature,
10.1.9 Operating relative humidity,
10.1.10 Type of spray water,
10.1.1 1 Type of spray nozzle, and
10.1.12 Specimen relocation procedure.
NOTE 8-When direct measurement of irradiation
and spectral irradiance cannot be made, data supplied
by the manufacturer shall be substituted. Irradiation in
kilojoules per square metre may be calculated by multiplying
the product of the irradiance in watts per square
metre and the exposure time in hours by the factor 3.6.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyjive years and
is not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, I916 Race St., Philadelphia, Pa. 1910.3.
417

Material
G 26 Test Method No.
Reference Standard Used:
Other ASTM Test No.
Method No.
Exposure Apparatus: ASTM Type
Mfr. Model
Serial No.
Light Source: Water-cooled -W, Air-Cooled -W
Method Used to Regulate Wattage to Lamp
Optical Filters: Type , Age h
Spectral Irradiance: W/m2 at nm
Irradiation Units: L / m * How Monitored:
Elapsed Exposure Time: -h
Exposure Conditions: Program -h
Light -min
Dark -min
Black-Panel Temperature -“C (“F)
Air Temperature -“C (“F)
Dry Bulb Temperature -‘C (“F) -‘C (“F)
Relative Humidity -% -%
Specimen Water Spray -min cycle -min cycle
Specimen Nonspray -min cycle -min cycle
Specimen Spray Water Type:
Specimen Spray Nozzle Type: Mfg. Designation
Specimen Relocation Procedure During Exposure:
Identify properties to be determined on test specimens and identify test procedures or methods used for property measurement.
-r- *---- - ~
Supervisor/Date:
Company:
FIG. 1 ReportForm
418

SPRAY
ANGLE-
/'
\
\
\
80°
/
/
/
SPRAY AREA APPROX 4''
Of CIHCIJMFERFGCF Of
SPECIMEN RACK.
PINTS OF WATER PtP MIhUlF FOR
5PEC:MEN SPRAf ONI i EOUIPPF-D
WIlH 2 NOZZLES CpFHATFD &T A
PRESSURE OF18 T225 OS!, F-90
NOZZLE - 23 TS 32 FINTS/MIN
' i
ji I
I /
I
1
I
i) \.
Metric Equivalents
23~a in. 60.325 mm
4 in. 101.6 mm
20 in. 508 mm
18 psi
124 kPa
25 psi
172 kPa
0.23 pt 0.109 liter
0.32 pt 0.152 liter
FIG. 2 Specimen Spray Arrangement for Type A and AH Appnratus
419

SPECIMEN TO FACE OF /‘ \
\v
/ FACE
-7
OF SPEClMEN /
DIRECTION X/\,
AOTATI ON
1 RPM
>
SPRAY AREA APPROX.
1“
19 T OF CIRCUMFERENCE
OF SPECMEN RACK.
r NOZZLE
ADAPTER
4 NOZZLES EMPLOYED
1 TYPE EMPLOYED- F-80
I
FINT< OF WATER PER MINUTE FOR
SFECIMEN SPRAY UN’i EO’JIr,FIED WllH
4 hCLZLES CGERATED AT A hOZZLF
FIRESSURE OF TH TG 25 PS, 46 ro 64
PINTS PER MINUTE
t 55’*
t-
t
c..
Metric Equivalents
4 in. 101.6 mm
18 psi 124 kPa
4’16 in. 117.48 mm
25 psi 172 kPa
5”l~ in. 136.52 mm 0.46 pt 0.218 liter
IO‘/2 in. 266.7 mm
0.64 pt
0.304 liter
3731r in.
958.85 mm
FIG. 3 Specimen Spray Arrangement for Type B and BH Apparatus
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users ofthis standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infiingement of such rights, are entirely their own responsibility.
420

ab
AMERICAN
Designation: G 53 - 84
SOCIETY FOR TESTING AND MATERIALS
1916 Race St., Philadelphia, Pa. 19103
Reprinted from the Annual Book of ASTM Standards, Copyright ASTM
If not listed in the current combined index, will appear in the Rext edition
Standard Practice for
OPERATING LIGHT- AND WATER-EXPOSURE APPARATUS
(FLUORESCENT UV-CONDENSATION TYPE) FOR
EXPOSURE OF NONMETALLIC MATERIALS'
This standard is issued under the fixed designation G 53; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval.
A superscript epsilon (0 indicates an editorial change since the last revision or reapproval.
This practice has been approvedfor use by agencies of the Department of Defense and for listing in the DoD Index of Specijications
and Standards.
1. scope
1.1 This practice covers the basic principles
and operating procedures for using fluorescent
ultraviolet (UV) and condensation apparatus to
simulate the deterioration caused by sunlight and
water as rain or dew.
1.2 This practice is limited to the method of
obtaining, measuring, and controlling the conditions
and procedures of exposure. It does not
specify the exposure conditions best suited for
the material to be tested. Specimen preparation
and evaluation of the results are covered in
ASTM methods or specifications for specific materials.
1.3 The values stated in SI units are to be
regarded as the standard.
1.4 This standard may involve hazardous materials,
operations, and equipment. This standard
does not purport to address all of the safety problems
associated with its use. It is the responsibility
of whoever uses this standard to consult and
establish appropriate safety and health practices
and determine the applicability of regulatory limitations
prior to use.
2. Applicable Documents
2.1 ASTM Standards:
E 220 Method for Calibration of Thermocouples
by Comparison Techniques2
G 7 Practice for Atmospheric Environmental
Exposure Testing of Nonmetallic Material?
2.2 CIE Standard:
No. 20 Recommendations for the Integrated
Irradiance and the Spectral Distribution of
Simulated Solar Radiation for Testing
Purposes4
3. Description of Terms Specific to This Standard
3.1 irradiance-the radiation incident on a
surface expressed in W/m2. Irradiance is the total
of the incident radiation at all wavelengths. Forty
watt fluorescent lamps of the UV-B and UV-A
types generate similar amounts of irradiance.
However, since this irradiance is distributed at
different wavelengths, the photochemical effects
caused by these different lamps vary greatly.
Therefore, irradiance should not be used to compare
UV light sources.
3.2 spectral irradiance-the distribution of irradiance
as a function of wavelength. It is expressed
in W/mZ per wavelength band. The spectral
irradiance of sunlight is often shown as W/
mz per 10 nm band. The spectral irradiance of
fluorescent UV lamps should be shown in bands
1 or 2 nm wide. Spectral irradiance is the proper
method for comparing sources with different energy
distributions.
3.3 spectrai energy distribution (SED j-a
general term for the characterization of the
amount of radiation present at each wavelength.
' This practice is under the jurisdiction of ASTM Committee
G-3 on Durability of Nonmetallic Materials, and is the direct
responsibility of Subcommittee 03.03 on Simulated and Controlled
Environmental Tests.
Current edition approved Aug. 3 I , 1984. Published October
1984. Originally published as G 53 - 77. Last previous edition
G 53 - 83.
Annual Book oJASTM Standards, Vol 14.01.
'Annual Book oJASTM Standards. Vol 14.02.
' Available from Secretary, U.S. National Committee, CIE,
National Bureau of Standards, Gaithersburg, MD 20899.
42 1

G 53
SEDs can be expressed by power in watts, irradiance
in watts/m2, or energy in joules. The
shape of the SED would be identical in all of
these units. Fluorescent lamps are frequently described
by relative SEDs which show the amount
of radiation at each wavelength as a percentage
of the amount of radiation at the peak wavelength.
Fig. 1 is a relative SED.
3.4 ultraviolet regions-CIE Publication No.
20 (1 972) divides the ultraviolet spectrum into
three regions: UV-A, radiation in wavelengths
between 3 15 nm and 400 nm; UV-B, radiation
in wavelengths between 280 nm and 315 nm;
and UV-C, radiation in wavelengths shorter than
280 nm.
3.5 Juorescent UV lamp-a lamp in which
radiation at 254 nm from a low-pressure mercury
arc is transformed to longer wavelength UV by a
phosphor. The spectral energy distribution of a
fluorescent UV lamp is determined by the emission
spectrum of the phosphor and the UV transmission
of the glass tube.
4. Summary of Practice
4.1 Specimens are alternately exposed to ultraviolet
light alone and to condensation alone
in a repetitive cycle.
4.2 The UV source is an array of fluorescent
lamps, with lamp emission concentrated in the
UV range.
4.3 Condensation is produced by exposing the
test surface to a heated, saturated mixture of air
and water vapor, while the reverse side of the test
specimen is exposed to the cooling influence of
ambient room air.
4.4 The exposure condition may be varied by
selection ofi the fluorescent UV lamp; the timing
of the UV and condensation exposure; the temperature
of UV exposure; and the temperature of
condensation exposure.
5. Stgnificanee and Use
5.1 The use of the apparatus under this practice
is intended to simulate the deterioration
caused by water as rain or dew and the ultraviolet
energy in sunlight. It is not intended to simulate
the deterioration caused by localized weather
phenomena, such as atmospheric pollution, biological
attack, and salt water exposure.
5.2 Variation in results may be expected when
operating conditions are varied within the accepted
limits of this practice. Therefore, no reference
shall be made to results from use of this
practice unless accompanied by a report detailing
the specific operating conditions in conformance
with Section 1 1.
5.3 Any report correlating results from use of
this practice to results from a period of natural
weathering shall specify in detail the conditions
of natural exposure, since sunlight and water
effects upon materials exposed to the weather
will vary from year to year and also vary with
location, latitude, time of year, temperature,
proximity to water sources, etc.
NOTE I-Practice G 7 lists the information required
to describe a particular condition of outdoor exposure.
5.4 Correlations established and reported in
conformance with 5.2 and 5.3 shall not be extrapolated
to other test conditions permitted by
this practice, to other conditions of natural exposure,
or to materials other than those tested.
6. Apparatus5
6.1 Test Chamber, (see Fig. 2) constructed of
corrosion-resistant materials enclosing eight fluorescent
UV lamps, a heated water pan, test
specimen racks, and provisions for controlling
and indicating operating times and temperatures.
6.2 Lamps, rapid start, medium bipin fluorescent
UV lamps with a length of 1220 mm, and a
nominal rating of 40 W when operated from a
ballast providing a controlled current of 430 mA
at 102V.
6.2.1 Unless otherwise specified, the lamps
shall be UV-B lamps with a peak emission at 3 13
nm and a spectral energy distribution as shown
in Fig. 1.
6.2.2 Other fluorescent UV lamps meeting the
size and electrical characteristics in 6.2 may be
used, provided that the lamp and spectral energy
distribution are reported in conformance with
Section 11.
6.3 Lamp Spacing and Arrangement-The
lamps shall be mounted in two banks of four
lamps each as shown in Fig. 2. The lamps in each
bank shall be mounted parallel in a flat plane on
70-mm centers.
6.4 Specimen Mounting and Arrangement-
The test specimens shall be mounted in stationary
racks with the plane of the test surface parallel
to the plane of the lamps at a distance of 50 mm
from the nearest surface of the lamps, as shown
JApparatus and lamps from QPanel Co., 26200 First St.,
Cleveland, OH 44145, and from Atlas Electric Devices Co.,
4 I I4 N. Ravenswood Ave., Chicago, IL 606 13, have been found
satisfactory.
422

G 53
in Fig. 2.
6.4.1 The test specimens shall be exposed
within an area 210 mm in height by 900 mm
wide on each side of the apparatus located as
shown in Fig. 4.
NOTE 2-It is possible to mount specimens above,
below, and beside the 210 by 900 mm area, but specimens
so mounted will be exposed to lower UV intensities.
6.5 Condensation Mechanism-Water vapor
shall be generated by heating a water pan extending
under the entire sample area and containing
a minimum water depth of 25 mm. Specimen
racks and the test specimens themselves shall
constitute the Side walls of the chamber. The
back side of the specimens shall be exposed to
cooling effects of ambient room air. The resulting
heat transfer causes water to condense on the test
surface.
6.5.1 The specimens shall be arranged so that
condensate runs off the test surface by gravity
and is replaced by fresh condensate in a continuous
process. Vents along the bottom of the test
chamber shall be provided to permit an exchange
of ambient air and water vapor to prevent oxygen
depletion of the condensate.
5.6 Water Supply, with an automatic control
to regulate the level in the water pan shall be
provided. Distilled, deionized, or potable tap water
are equally acceptable for purposes of the test,
since the condensation process itself distills water
onto the test surface.
6.7 Cycle Timer, A continuously operating
cycle time, for programming the selected cycle of
UV periods and condensation periods.
6.7.1 Hour meters shall be provided to record
total time of operation and total time of UV
exposure.
6.8 Specimen Temperature Measurement:
6.8.1 Specimen temperature shall be measured
by a thermometer with a remote sensor
attached to a black aluminum panel 75 by 100
by 2.5 mm thick. The thermometer shall be
precise to f 1°C through a range from 30" to
80°C. The indicator dial shall be located outside
the test chamber.
6.8.2 The black aluminum panel with the
thermometer sensor shall be positioned in the
center of the exposure area so that the sensor is
subject to the same conditions as the specimens.
6.9 Specimen Temperature Control:
6.9.1 During UV exposure, the selected equilibrium
temperature shall be maintained within
k 3°C by supplying heated air to the test chamber.
6.9.2 During condensation exposure, the selected
equilibrium temperature shall be maintained
within -+ 3°C by heating the water in the
water pan.
6.9.3 The UV and condensation temperature
controls shall be independent of each other.
6.9.4 Doors shall be located on the room air
side of the specimen racks to act as insulation
during the UV exposure and to minimize drafts.
Such doors shall not interfere with the room air
cooling of the specimen during the condensation
exposure.
6.10 Test Chamber Location:
6.10.1 The apparatus shall be located in an
area maintained at a temperature between 20°C
and 30°C. The room temperature shall be measured
by thermometers mounted on interior
walls or column approximately 1500 mm above
the floor level and at least 300 mm from any
heated apparatus. Three or more thermometers
located at various points will show any temperature
variation in the area.
6.10.2 It is recommended that the apparatus
be located at least 300 mm from walls or other
apparatus. Nearby heat sources, such as ovens or
heated test apparatus, should be avoided or
shielded, because such heat sources can reduce
the cooling required for condensation.
6.10.3 The room where the apparatus is located
shall be ventilated to remove the heat and
moisture produced and to maintain the temperatures
specified in 6.10.1. Two to four air changes
per hour will normally provide sufficient ventilation.
7. Test Specimens
7.1 Replicate specimens are desirable to provide
a record of degradation at different time
intervals. Retention of an unexposed specimen
is recommended as ir is difiiculi io mask a specimen
to prevent exposure to condensation.
7.2 For specimens of insulating materials,
such as wood, plastic, or porous laminates, maximum
specimen thickness should be 20 mm to
allow adequate heat transfer for condensation.
7.3 To provide rigidity, flexible specimens
may be attached to a backing panel made of
aluminum or other noncorrosive heat conductive
material.
7.4 Cut edges of coated steel specimens shall
be protected so that rust does not contaminate
423

G 53
the test surface.
7.5 Holes in specimens and any openings
larger than 1 mm around irregularly shaped specimens
shall be sealed to prevent loss of water
vapor. Porous specimens, such as textiles or wood
shall be backed with a vapor barrier such as metal
or plastic.
8. Calibration and Standardization
8.1 The thermometer or thermocouple which
indicates test temperature shall be calibrated by
immersing the sensing element and a liquid-inglass
thermometer in water heated to approximately
70°C and comparing the two temperatures
as in Method E 220.
8.2 The formation of condensation may be
observed by using clear glass or plastic blanks in
the specimen holders or rack. One large sheet of
plastic may also be used for this purpose. The
condensate that forms on a given area during a
period of condensation may be collected and
then measured.
8.3 The fading and other changes caused by
the fluorescent UV lamps may be observed by
exposing lightfastness standards in the apparatus
using UV alone without condensation.
8.3.1 The AATCC Blue Wool Lightfastness
reference materials6 may be used to measure the
changes caused by UV. The L2 Blue Wool has
been found satisfactory for evaluating fluorescent
UV lamps.
8.3.2 Other lightfastness reference materials
may be used by agreement.
8.4 Reference standards for calibrating the o p
eration of the apparatus in alternate exposure to
UV light and condensation may be prepared
from painted metal, plastics, or other materials.
Painted metal specimens produced by the coilcoating
process have been found suitable for such
reference standards.
9. Rwdare
9.1 Mount the test specimens in the specimen
racks with the test surfaces facing the lamp. When
the test specimens do not completely fill the
racks, fill the empty spaces with blank panels to
maintain the test conditions within the chamber.
9.2 Program the selected test conditions. Op
erate continuously, repeating the cycle, except
for servicing the instrument and inspection of
specimens.
9.3 Various test conditions may be used. If no
conditions are specified, the following cycle and
temperatures are suggested: 4 h UV at 60"C, 4 h
Condensation at 50°C.
NOTE 3-Prior versions of this practice recommended
a condensation temperature of 40'C in 9.3.
When operating in room conditions that do not comply
with those set forth in 6.10, a 40°C condensation temperature
can result in inadequate condensation. Therefore,
a 50°C condensation temperature is now suggested.
9.3.1 Any test temperature that can be maintained
within the limits specified in 6.9.1 and
6.9.2 may be used. UV test temperature of 50°C,
60", and 70°C are widely used. A condensation
test temperature of 50°C is commonly used.
9.3.2 The following time cycles are widely
used: 4 h UV/4 h CON, and 8 h UV/4 hr CON.
Use UV and condensation periods of at least 2-
h duration to allow sufficient time to reach equilibrium.
9.3.3 The severity of the UV exposure is influenced
by test temperatures and time cycles. Photochemical
reaction begins as soon as the UV
lamps are turned on. The rate of UV degradation
is proportional to the time of UV exposure or
the temperature of UV exposure, or both. UV
exposures at temperatures higher than those expected
in the service environment can cause abnormal
thermal degradation.
9.3.4 Water reactions during condensation exposure
are affected by the permeability of the
specimen and require time to initiate.The rate of
water degradation is increased by increased temperature.
However, long hot condensation exposures
can cause abnormal degradation. Fourhour
condensation exposures are often used for
paints on metals, while condensation exposures
of 20 h duration may be used on wood.
9.4 Maintenance-Periodic maintenance is
required to maintain uniform UV and condensation
exposure conditions.
9.4.1 After 400 to 450 h of lamp operating
the, replace one !amp in each bank d!amps,
and rotate the other lamps as shown in Fig. 3.
This procedure provides a useful lamp life of
1600 to 1800 h.
9.4.2 Drain water and clean water pan when
conducting lamp replacement and rotation procedure.
Scum on the top of the water can inhibit
water vaporization.
9.5 Inspect specimens daily in tests with a
Available from American Association of Textile Chemists
and Colorists, P.O. Box 12215, Research Triangle Park, NC
27709.
424

G 53
length of 1 week or less. Tests for longer periods
should be inspected weekly. In order to minimize
any effects from temperature or UV light variation,
samples may be repositioned on a regular
schedule, if such procedure is reported as a specific
condition of the test in accordance with
11.1.5.
9.5.1 A permanent record of degradation at
various times may be obtained by using three
replicate specimens and removing the replicates
sequentially at intervals equal to one third of the
test length.
9.6 Conclude the test when either a mutually
agreed-upon number of total test hours or a
mutually agreed-upon change has occurred in
the test specimen or a standard test specimen.
For convenience in inspecting and concluding
tests during normal working hours, the following
test durations are recommended:
96 h = 4 days
168 h = 1 week
336 h = 2 weeks
504 h = 3 weeks
672 h = 4 weeks
1008 h = 6 weeks
1512 h = 9 weeks
2016 h = 12 weeks
10. Interpretation of Results
10.1 This practice is intended to simulate the
deterioration caused by natural weathering.
However, the rate of degradation in natural
weathering varies from year to year. Laboratory
accelerated weathering is more consistent in rate.
Therefore, in comparing natural and laboratory
weathering one should not attempt to predict the
number of hours of laboratory exposure that
might equal a year of natural weathering. Even
if the details of the natural exposure are fully
reported as required by 5.3, any time to time
comparison would apply only to a given year at
a particular site.
10.2 It is possible to correlate the deterioration
resulting from a period of natural weathering,
such as 1 year, to the deterioration resulting from
a period of laboratory accelerated weathering.
Spearman rank correlation, which is discussed in
most basic statistical texts, has proved to be a
useful method for this. A minimum of seven
variables must be ranked by both test methods
to obtain statistical validity from Spearman rank
correlation. Ranking 10 to 15 variables by both
methods will improve the reliability of such correlations.
10.3 It is frequently not possible to predict
how many hours or weeks of accelerated testing
will yield the best correlation to some period of
outdoor testing. Therefore, laboratory tests
should be measured periodically, such as weekly
or biweekly, so that the correlation coefficient
may be calculated at several points during the
accelerated test.
11. Report
1 1.1 The report shall include the following:
11.1.1 Manufacturer and model of fluorescent
UV/condensation apparatus,
I 1.1.2 Manufacturer's designation for the fluorescent
UV lamp, the wavelength (nm) at which
peak emission occurs, and the short wavelength
at which 1 % of peak emission occurs (for example,
FS-40 313/280 nm),
11.1.3 Cycle of UV exposure time and temperature,
condensation time and temperature
(for example 4 h UV/6o"C, 4 h CON/SO"C),
1 1.1.4 Total exposure time,
1 1.1.5 Special conditions of test, such as rotation
of test specimens, and
1 1.2 A sample report form is shown in Fig. 5.
UAVELEUGTH
(nanometers)
FIG. 1 Typical Relative SED of UV-B Lamp
425

A
Controll
LAMP ROTATION
sp.ri..n
Door -
DISCARD
NEW 0
LAMP
FIG. 3
\
Lamp Rotation
0 NEW
LAMP
FIG. 2 Apparatus %hematic Cross Section
I_- POOmm -7
FIG. 4 Limits of Area of Uniform Intensity
426

APPARATUS
Type and Modal
TEST
TIME
hrr.
LAMP
MANUFACTURER
TYPE
PEAK EMISSION
CYCLE
hrr UV ai -"C. I - hrr COND at ' C .
SPECIAL TEST CONDITIONS
nn
LOW CUTGFF (1% of pwlrl
nm
START
DATE:
TIMER HRS. START TIMER HRS. STOP LAMP SERVICE
END
DATE: mt hrr.
1.
2.
3.
FIG. 5 Sample Report Form
The American Societyjbr Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users ofthis standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed everyjive years and
tf not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional
standards and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you fie1 that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, 1916 Race St., Philadelphia, Pa. 19103.
427

APPENDIX 14
Common Abbreviations and Symbols
NAME
Angstrom unit
American Society for Testing Materials
Avoirdupois (unit of weight based on 1 pound = 16 ounces)
British Thermal Unit
Celsius, degree
Centimeter
Centipoise
Coefficient of Friction
Cubic centimeter
Degree
Electron beam
Fahrenheit, degree
Feet
Feet per minute
Gallon
Glass transition temperature
Gram
Hour
Inch
Kilowatt
Liters
Mercury
Meter
Methyl ethyl ketone
Micron
Milligram
Milliliter
Nanometer
Poise
Pounds
Pounds per square inch
Pounds per square inch per gram
Revolutions per minute
Seconds
Time
Ultraviolet
Volatile Organic Compound
ABBREVIATIONS
b;
ASTM
avdp
Btu
"C
cm
CP
COF
cc
deg. ,"
EB
OF
ft.,
fpm
gal
Tg
g
hr
in., "
kW
1, L
Hg
m
MEK
Ccm
mg
ml, mL
nm
P
lbs., #
psi
Psig
'pm
sec., s
t
uv
voc
kilocentimillimicronano-
Prefixes and Their Numerical Value
k
C
m
IC
n
1 o3
lo-*
10-~
10-9

APPENDIX 15
Common Units and Conversion Factors
To Convert From To Multiply By
Centimeters
ri
rr
rr
Centipoise
Cubic centimeter
rr
rr
Cubic inch
Cubic meter
Feet
rr
rr
Gallons, (U.S., liquid)
Grams
ir
ir
I1
Inches
I1
ri
rr
Kilograms
Liters
rr
I1
Meters
ir
rr
ir
tr
Microns
Milligrams
Milliliters
Mils
rr
rr
Ounces (avdp.)
rr
Poise
Pwiids (zfdij.)
rr
Feet
Inches
Meters
Mils
Poises
Cubic inches
Cubic meters
Liters
Cubic centimeter
Cubic centimeter
Centimeters
Inches
Meters
Liters
Kilograms
Milligrams
Ounces (avdp.)'
Pounds (avdp.)
Centimeters
Feet
Meters
Mils
Grams
Cubic centimeters
Gallons, (U.S., fluid)
Milliliters
Centimeters
Feet
Inches
Microns
Millimeters
Meters
Grams
Liters
Meters
Centimeters
Inches
Grams
Pounds (advp.)
Centipoise
Grams
Ounces (avdp.)
0.0328
0.3937
0.01
393.7
0.01
0.0610
0.000001
0.0010
16.387
1 ,oO0,oO0.0
30.48
12
0.3048
3.7853
0.001
1000
0.0353
0.0022
2.54
0.0833
0.0254
1000
1000
1000.028
0.2642
1000
100
3.2808
39.37
1,000,000.0
1000
0.00000 1
0.001
0.001
0.001
0.0025
0.001
28.35
0.0625
100
453.59
16
'avdp. - Avoirdupois (unit of weight based on 1 pound = 16 ounces)
429

APPENDIX 16
TEMPERATURE CONVERSION TABLE
To
"C
- 17.78
- 17.22
- 16.67
-16.11
- 15.56
- 15
- 14.44
- 13.89
- 13.33
- 12.78
- 12.22
-11.67
-11.11
- 10.56
- 10
-9.44
-8.89
-8.33
-7.78
-7.22
-6.67
-6.11
-5.56
-5
-4.44
-3.89
-3.33
-2.78
-2.22
-1.67
-1.11
-0.56
0
.56
1.11
1.67
2.22
2.78
3.33
3.89
4.44
5
5.56
6.11
6.67
To Conver
+ "F or "C +
0
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
To
"F
32
33.8
35.6
37.4
39.2
41
42.8
44.6
46.4
48.2
50
51.8
53.6
55.4
57.2
59
60.8
62.6
64.4
66.2
68
69.8
71.6
73.4
75.2
77
78.8
80.6
82.4
84.2
86
87.8
89.6
91.4
93.2
95
96.8
98.6
100.4
102.2
104
105.8
107.6
109.4
111.2
430
To
"C
7.22
7.78
8.33
8.89
9.44
10
10.56
11.11
11.67
12.22
12.78
13.33
13.89
14.44
15
15.56
16.11
16.67
17.22
17.78
18.33
18.89
19.44
20
20.56
21.11
21.67
22.22
22.78
23.33
23.89
24.44
25
25.50
26.11
26.67
27.22
27.78
28.33
28.89
29.44
30
30.56
31.11
31.67
To Convert
+ "F or "C +
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
To
"F
113
114.8
116.6
118.4
120.2
122
123.8
125.6
127.4
129.2
131
132.8
134.8
136.4
138.2
140
141.8
143.6
145.4
147.2
149
150.8
152.6
154.4
156.2
158
159.8
161.6
163.4
165.2
167
168.8
170.6
172.4
174.2
176
177.8
179.6
181.4
183.2
185
186.8
188.6
190.4
192.2

TEMPERATURE CONVERSION TABLE (cont.)
To
"C
32.22
32.78
33.33
33.89
34.44
35
35.56
36.11
36.67
37.22
37.78
38.33
38.89
39.44
40
40.56
41.11
41.67
42.22
42.78
43.33
43.89
44.44
45
45.56
46.11
46.67
47.22
47.78
48.33
48.89
49.44
50
50.56
51.11
51.67
52.22
52.78
53.33
53.89
54.44
55
55.56
56.11
56.67
To Convert
+ O F or "C +
90
91
92
93
94
95
96
97
98
99
100
101
102
103
104
105
106
107
108
109
110
111
112
113
114
115
116
117
118
119
120
121
122
123
124
125
126
127
128
129
130
131
132
133
134
To
OF
194
195.8
197.6
199.4
201.2
203
204.8
206.6
208.4
210.2
212
213.8
215.6
217.4
219.2
22 1
222.8
224.6
226.4
228.2
230 ,p
231.8
233.6
235.4
237.2
239
240.8
242.6
244.4
246.2
248
249.8
251.6
253.4
255.2
257
258.5
260.6
262.4
264.2
266
267.8
269.6
271.4
273.2
To
"C
57.22
57.78
58.33
58.89
59.44
60
60.56
61.11
61.67
62.22
62.78
63.33
63.89
64.44
65
65.56
66.11
66.67
67.22
67.78
68.33
68.89
69.44
70
70.56
71.11
71.67
72.22
72.78
73.33
73.89
74.44
75
75.56
76.11
76.67
77.22
77.78
78.33
78.89
79.44
80
80.56
81.11
81.67
To Convert
+ OF or "c +
135
136
137
138
139
140
141
142
143
144
145
146
147
148
149
150
151
152
153
154
155
156
157
158
159
160
161
162
163
164
165
166
167
168
i65
170
171
172
173
1 74
175
176
177
178
179
To
OF
275
276.8
278.6
280.4
282.2
284
285.8
287.6
289.4
291.2
293
294.8
296.6
298.4
300.2
302
303.8
305.6
307.4
309.2
311
312.8
314.6
316.4
318.2
320
321.8
323.6
325.4
327.2
329
330.8
332.6
334.4
336.2
338
339.8
341.6
343.4
345.2
347
348.8
350.6
352.4
354.2
43 1

TEMPERATURE CONVERSION TABLE (cont.)
To
"C
82.22
82.78
83.33
83.89
84.44
85
85.56
86.11
86.67
87.22
87.78
88.33
88.89
89.44
90
90.56
91.11
91.67
92.22
92.78
93.33
93.89
94.44
95
95.56
96.11
96.67
97.22
97.78
98.33
98.89
99.44
100
100.56
101.11
101.67
102.22
102.78
103.33
103.89
104.44
105
105.56
106.11
106.67
To Conver
+ "F or "C +
180
181
182
183
184
185
186
187
188
189
190
191
192
193
194
195
196
197
198
199
200
201
202
203
204
205
206
207
208
209
210
21 1
212
213
214
215
216
217
218
2 19
220
22 1
222
223
224
To
OF
356
357.8
359.6
361.4
363.2
365
366.8
368.6
370.4
372.2
374
375.8
377.6
379.4
381.2
383
384.8
386.6
388.4
390.2
392
393.8
395.6
397.4
399.2
40 1
402.8
404.6
406.4
408.2
410
411.8
413.6
415.4
417.2
419
420.8
422.6
424.4
426.2
428
429.8
431.6
433.4
435.2
432
To
"C
107.22
107.78
108.33
108.89
109.44
110
110.56
111.11
111.67
112.22
112.78
113.33
113.89
114.44
115
115.56
116.11
116.67
117.22
117.78
118.33
118.89
119.44
120
120.56
121.11
121.67
122.22
122.78
123.33
123.89
124.44
125
125.56
126.11
126.67
127.22
127.78
128.33
128.89
129.44
130
130.56
131.11
131.67
To Conver
+ OF or "C -+
225
226
227
228
229
230
23 1
232
233
234
235
236
237
238
239
240
24 1
242
243
244
245
246
247
248
249
250
25 1
252
253
254
255
256
257
258
259
260
26 1
262
263
264
265
266
267
268
269
To
OF
437
438.8
440.6
442.4
444.2
446
447.8
449.6
451.4
453.2
455
456.8
458.6
460.4
462.2
464
465.8
467.6
469.4
471.2
473
474.8
476.6
478.4
480.2
482
483.8
485.6
487.4
489.2
49 1
492.8
494.6
496.4
498.2
500
501.8
503.6
505.4
507.2
509
510.8
512.6
514.4
516.2

APPENDIX 17
ADVERTISER INDEX
Acme Printing Ink Co ......................................... 27
American Ultraviolet Co ..................................... 24
B orden ................................................................. 11
Ciba-Geigy .......................................................... vi
Ciba-Geigy .......................................................... 42
DeSoto. Inc .......................................................... 3
EM Industries ....................................................... 5
Energy Sciences. Inc ............................................ 9
Fusion UV Curing Systems ................................ 12
Goldschmidt Chemical Co .................................. 27
Henkel Corp ........................................................ 24
Henkel Corp ......................................................... 7
Interez. Inc .......................................................... 16
Pierce & Stevens Corp ......................................... 3
PPG Industries ..................................................... v
Radcure Specialties. Inc ........................
RPC Industries .................................................... 19
S artomer Co ......................................................... 9
Union Carbide Corp ............................................ 12
Inside Front Cover
The Upjohn Co ................................................... 23
UV Process Supply. Inc .............................. Back Cover
433

DEPTH OF CURE COMPARATOR
#N008-001
This gage has precisely
graduated, clearly marked paths
ranging from 0.3 to 125 mils
milled into its surface. The
formulation to be tested is
applied to the level end of the
comparator and drawn into the
fhs with the supplied scraper.
hen sent through the curing
chamber, the thickness range
of the cured film is easily
determined.
INTENSITY LABELS #NO10401 I
ROLL (1000)
These phdochromic labels are a
simple, reliable low cost method
of monitoring UV and EB radiation.
Upon irradiation the labels
undergo a color change which
can be easily measured with a
densitometer or colorimeter. The
color change can be related to
radiation dose. Especially useful
where an instrument is not
practical such as 3-0 parts, web
coating or printing.
CONTINUOUS DISPLAY
RADIOMETER #Myuoo8-001
This radiometer has been
specifically designed to address
long-term UV process problems.
Once properly installed, it
provides the means of continuously
monitoring the output
from your particular UV processor.
It is an important tool
used to detect early equipment
deterioration or failure. It also
conIributes in the recording of
equipment and process history.
DRY FILM THICKNESS OAGE
#MWl.MIt
Provides precision measurements
on any flat surface,
without having to cut into the
cured film. Readings are taken
by zeroing the linear transducer
probe on the surface and
movin the probe so it steps
onto tfe ink or coating. The
difference in thickness is read
directly in standard or metric
units ranging from 0.05 to O.ooO1
inch (0.05 to O.OGO5mm)
COMPUTAK TACHOMETER
IM(004-001
The world's first computer
tachometer. A digital, hand held,
battery operated tachometer
which is programmed to compute
and readd in any one of
13 different standard uniIs of
measurement. Speeds ranging
from 0.1 to IO00 FPM can be
measured accurately using the
rubber tread wheel supplied.
Also includes concave and convex
rubber tips for shaft contact.
DUAL FUNCTION DIGITAL
TACHOMETER #M004-002
This tachometer is a dual
function instrument providing
contact and non-contact
measurement of rotational and
linear mdions. Wflh an accuracy
of +I- ,03546 of indicated
reading, it is ideal for uses in
production, engineering, inspection,
quality control and
maintenance. The unit comes
with a convex tip and lOcm linear
measuring wheel.
DIGISTROBE XMOO4-003
This digital stroboscopeltachometer
is a high quality, versatile
hand held instrument suited to a
wide range d, motion analysis, as
well as to image inspection.
Optically slows or stops the
motion of any moving object.
Useful for printing, packaging,
general production and quality
control.
Flashrate range: 20.00 to 29,999
FPM
Tachometer range: 120.00 to
99,999 RPM
DUROMETER IN006-002
This durometer is designed to
measure the indentation hardness
of rubber, soft plastics and
other elastomers. Dependable,
built of ruggsd construction, with
all park totally enclosed and
machined to a high tolerance
that provides precision gage
movement. Portable, easily read
and used anywhere, can be
mounted in any orientation. A
marked, calibrated test block is
included with each unit.
.. (.__ ..+__ .. --
PAPER THERMOMETERS
(Iy005-001 to 00B/sET (16)
These self adhering paper Ihermometers
are lowcost. accurate
heat indicators for inaccessible
areas. Based on the heat sensitivity
d calibrated coatings on
the paper base, this product is
formulated to react within 1
second of exposure to heat by a
distinct color change from white
to black. Available in 8 different
temperature sets.
WET FILM THICKNESS GAGE
A direct reading, precision instrument
for accurately measurin
the wet film thickness 3
coatings, inks, adhesives,
varnishes, lacquers and many
other products. Can be used on
a flat or curved substrate.
Simply roll over a wet film.
Available in two ranges:
#MOO2402 (measures between
0 and 2 mils) and #M002-003
(measures between 0 and 4 mils)
SPECTROLINE DIGITAL RADIOMETERS
These advanced meters are the
most reliable instruments available
in their price range with an
accuracy of +I- 5%. They
provide automatic full range
readin s on an LCD displa
SHOJ WAVE RADIO METE^
#MOO712 (Spectral band width
around 254nm) MEDIUM
WAVE RADIOMETER WMW-
014 (Spectral ran e of 280 to
anm) LONG ~AVE RADIO-
METER YM007-013 (Soectral
range of 320 to 380nni) '
VARIABLE SCRAPERS
Determining desired film
thickness is easy to do with
these multi-thickness wet film
applicators. Each variable
scraper provides a predetermined
thickness range for
testing formulations. A small
quantity of the material is
placed in the channel and
scraped across a Hat substrate
for evaluation. Available in 2 or
8 paths and a variety of widths.
Featured above is ryNOO8-002
(graduated 0 to 10 mil).