Processing kodak motion picture films, module 3 analytical procedures

APPARATUS
All volumetric glassware should meet all Class A
specifications, as defined by American Society for Testing
and Materials (ASTM) Standards E 287, E288, and E969,
unless otherwise stated.
Centrifuge, with rotor to accommodate 50-mL centrifuge
tubes, capable of 1000 rpm.
50-mL centrifuge tubes (polypropylene)
10-mL pipette
Volumetric flask, 100-mL
Beakers, 150- and 250-mL
ORION double-junction reference electrode 900200 or
equivalent with (10% KNO3 outer filling solution)
Silver billet indicator electrode BECKMAN Model 39261
or equivalent
Automatic titrator with stirrer, METROHM E536 with an
E665 Dosimat (20-mL burette) or equivalent.
Whatman fluted filter paper - 32 cm (if needed)
REAGENTS
All reagents should be ACS Reagent Grade unless otherwise
specified.
190 g/L Zinc Sulfate, ZnSO 4
0.10 N Sodium Chloride, NaCl
0.05 N Silver Nitrate, AgNO 3 , standardized to four
significant figures
Celite filter aid
Water, Type I Reagent - This method was developed using
reagent water equivalent to or purer than Type I grade, as
defined in ASTM Standard D 1193. Other grades of water,
e.g., reverse osmosis (RO), demineralized, or distilled
water, may give equivalent results, but the effects of water
quality on method performance have not been studied.
PROCEDURE
Sample Treatment
1. Pipette 5.0 mL of bleach into a 100-mL volumetric
flask.
2. Add 25 mL of zinc sulfate. Dilute to volume with
reagent water. Stopper and invert the flask 6 to 10
times to mix.
Note: If unable to centrifuge, delete steps 3-5 and filter
the treated sample through a 32-cm WHATMAN 2V
fluted filter paper containing 2 g of Celite.
3. Pour nearly equal amounts of the mixture into two 50mL
centrifuge tubes. Do not fill the tubes to more than
one inch from the top.
4. Place the tubes in opposite positions and centrifuge at
maximum speed for at least two minutes. (Observe the
safety precautions for the use of the centrifuge.)
5. Carefully decant the liquid phase from both centrifuge
tubes into a 150-mL beaker.
6. Pipette 50.0-mL of the liquid phase or filtrate into a
250-mL beaker containing approximately 100-mL of
reagent water.
7. Add 1 mL of 0.10 N sodium chloride to the beaker.
Titration
1. Titrate the sample, through the first break, on an
automatic titrator with standardized 0.05 N silver
nitrate. Use a silver billet as the indicator electrode and
a double junction reference electrode
Use the following settings for a METROHM titration
system:
Horizontal chart span = 500 mV
Maximum titration speed = 15
(min/100% volume)
Stop (%U) = OFF
Vertical chart span = 400
(mm/100% volume)
Auto control = OFF
Titration mode = mV/pH
Titration “breaks” from = right to left
2. Determine the end point using the concentric arcs
method. (Refer to Universal Method ULM-0003-01,
Potentiometric Titrations for Photoprocessing
Solutions or any subsequent revisions.)
Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3