Processing kodak motion picture films, module 3 analytical procedures
Processing kodak motion picture films, module 3 analytical procedures Processing kodak motion picture films, module 3 analytical procedures
PROCEDURE C Determination of Silver in Thiosulfate Fixing Baths When Concentration of Silver is Less Than 0.5 Grams per Liter. Note: When the concentration of silver is less than 0.5 g/L, it is possible to establish the silver content between two concentrations 0.05 g/L apart, using only graduated cylinders and the markings on the cylinders for all measurements. Treatment of Sample 1. Obtain several 100-mL glass-stoppered graduated cylinders. Add to each 40 mL of fixing bath sample, 20 mL of 0.2 M potassium ferricyanide, and 20 mL of 6 N accelerator reagent. Stopper and shake to mix. 2. Add from a polyethylene squeeze bottle to one of the cylinders, 20 mL of 0.00926 N thioacetamide, and to a second cylinder, add 10 mL. Note: 20 mL of 0.00926 N thioacetamide is equivalent to 0.5 g/L of silver and 10 mL is equivalent to 0.25 g/L of silver. 3. Stopper and shake the cylinders vigorously for 5 seconds. 4. Filter approximately 20 mL of the contents of each cylinder through Whatman No. 3 (12.5 cm diameter) filter paper and collect the filtrates in beakers containing approximately 5 mL of 0.00926 N thioacetamide each. 5. Observe the appearance of the contents and refer to Table 3, Decision Sheet for Procedure C (40 mL Sample), to make the next decision. Reporting Results 1. These two trials determine that: a. The procedure is not applicable (silver content is greater than 0.5 g/L) b. The silver content is below 0.25 g/L c. The silver content is between 0.25 and 0.5 g/L 2. If the procedure is applicable, three or fewer trials will establish the silver content between two silver concentrations 0.05 grams per liter apart. Table 3 Decision Sheet for Procedure C (40 mL Sample) mL of 0.00926 N Thioacetamide Added If the Contents of the Beaker Turns Color, Amount of Silver in Fix is More Than 2 0.05 g/L 4 0.10 g/L 6 0.15 g/L 8 0.20 g/L 10 0.25 g/L 12 0.30 g/L 14 0.35 g/L 16 0.40 g/L 18 0.45 g/L 20 0.50 g/L If the Contents of the Beaker Remains Clear, Amount of Silver in Fix is Less Than PROCEDURE D Determination of Exhaustion of Kodak Chemical Recovery Cartridge Note: When the concentration of silver in the effluent from the Recovery Cartridge exceeds 0.25 grams per litre, it can be assumed that the capacity of the cartridge has been exceeded. By selecting the 10 mL of 0.00926 thioacetamide (equivalent to 0.25 g/L of silver) and making only the one trial, a decision on exhaustion can be reached. Treatment of Sample 1. Place in a 100-mL glass-stoppered graduated cylinder 40 mL of fixing bath sample, 20 mL of 0.2 M potassium ferricyanide, and 20 mL of 6 N accelerator reagent. Stopper and shake to mix. 2. Add 10 mL of 0.00926 N thioacetamide, stopper, and shake for 5 seconds. 3. Filter approximately 20 mL of the mixture through a Whatman No. 3 filter paper into a beaker containing approximately 5 mL of 0.00926 N thioacetamide. Reporting Results 1. Colored, the recovery cartridge is exhausted. 2. Clear, the recovery cartridge is still serviceable. 4 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03
The Determination of Specific Gravity for Photoprocessing Solutions Using Hydrometers ULM-0002/1 Process ECN-2 ECP-2D VNF-1/LC RVNP Formulas All All All All INTRODUCTION Specific gravity is the ratio of the mass of a body to the mass of an equal volume of some other substance taken as the standard or unit, the measurements being made at the same temperature or, as is sometimes the case, at a stated reference temperature. * Or stated more simply for liquids, specific gravity is the ratio of a mass of a body to the mass of an equal volume of water at a specified temperature. † The standard or unit for the measurement of the specific gravity of liquids is commonly gas-free, pure (e.g., distilled) water. Specific gravity can be used as a measure of the total amount of dissolved material in a solution. “Specific gravity may be determined at any temperature and referred to water at the same temperature or at any desired temperature.” * The temperature of measurement should be controlled and specified in all specific gravity measurements because the specific gravity of a solution is affected by temperature. Specific gravity should be stated as follows: Specific gravity, x/y °C Where x = temperature of the material being measured y = temperature of the water e.g., 1.050, 25.0/15.56°C In historical analytical methods related to photographic processing solutions, ‡ an increase of 3°C causes a decrease of 0.001 (0.00033/°C) in the specific gravity of most photographic processing solutions. Standards of specific gravity for photographic processing solutions are set by analyzing standard mixes at 25°C. The superseded version of this method ‡ specified the determination of specific gravity at 27°C. The temperature change to 25°C was made to be consistent with the method currently recommended for the measurement of pH in photographic processing solutions. § A calculation described in Appendix A, Estimation of Specific Gravity Conversion From One Temperature to Another, * Taylor, john K. in Treatise on Analytical Chemistry, 1st ec.; Kolthoff, I.M.; Elving, P.J.; Part 1, Theory and Practice, Interscience: New York, 1967; Volume 7, Chapter 81, p. 4563. † Handbook of Chemistry and Physics, 3tth ed.; Hodgeman, Charles D., ed. In Chief; Chemical Rubber Publishing Co.; Cleveland, OH, 1995; p. 2831. ‡ Determination of Specific Gravity of Processing Solutions; ECP-2-701, TR Accession No. 206210L, 1974; Eastman Kodak Co., Rochester, NY. § Mevs, Judith M.; Jansen, Kathryn L. pH Measurement of Photographic Processing Solutions; KPCQ-A-PR-G-191-2, TR Accession No. 266951E, 1992; Eastman Kodak Co., Rochester, NY. estimates the effect of the temperature change from 27°C to 25°C on specific gravity. PRECISION AND BIAS Precision All specific gravity readings for photographic processing solutions are made at 25 ± 0.25°C. Historically, ‡ the variability of measurement has been expected to fall within ±± 0.002, 95 percent of the time. ASTM Standard D891-95 states that the precision of specific gravity by hydrometer should be determined for each chemical. For photoprocessing control, this is not practical. ASTM gives the following examples, however: Repeatability (one analyst/one day): With-in Laboratory/ Between Days: Bias The bias of this test method has not been determined due to the unavailability of suitable reference materials. However, bias is dependent upon the calibration of the hydrometer and the degree of control of the temperature of the hydrometer bath. APPARATUS 1sr (single det’n.) = 0.00020 (24 DF) 95% Conf. Est. = ± 0.0005 1s (single analyst) = 0.0016 (12 DF) 95% Conf. Est. = ± 0.005 Hydrometers Hydrometers should meet the specifications in ASTM Standard E 100, ** as follows: Specific Gravity Range ASTM Number 1.000 - 1.050 111H - 62 1.050 - 1.100 112H - 62 1.100 - 1.150 113H - 62 1.150 - 1.200 114H - 62 1.200 - 1.250 115H - 62 1.250 - 1.300 116H - 62 Note: The hydrometers recommended for determining specific gravity: a. Are calibrated with reference to gas-free, distilled water at 60° F (15.56°C), although measurements are made at 25°C. b. Have subdivisions at 0.0005. c. Have intermediate lines at 0.001. Standard Test Methods for Specific Gravity, Apparent, of Liquid Industrial Chemicals; American Society for Testing and Materials: ASTM Designation D 891-95, Philadelphia, PA, August, 1995. ** Specification for ASTM Hydometers; American Society for Testing and Materials: ASTM Designation D 100-95, Philadelphia, PA, April, 1995. Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 1
- Page 247 and 248: Iodometric Determination of Total S
- Page 249 and 250: Titrimetric Determination of Total
- Page 251 and 252: Table 2 Contribution of Constituent
- Page 253 and 254: Determination of Sulfite in KODAK R
- Page 255 and 256: CALCULATIONS Na2SO3 , g/L = (mL B -
- Page 257 and 258: Colorimetric Determination of Thioc
- Page 259 and 260: APPENDIX A Calibration of Spectroph
- Page 261 and 262: Analysis Order for Photographic Pro
- Page 263 and 264: Procedure for Electroplating a Silv
- Page 265 and 266: The Selection, Care, and Use of Vol
- Page 267 and 268: In observing the lowest point on th
- Page 269 and 270: 4. Graduated Cylinders and Tip-up P
- Page 271 and 272: 6. Microburets Microburets equipped
- Page 273 and 274: Table 1 Required Tolerance for Volu
- Page 275 and 276: pH Measurement of Photographic Proc
- Page 277 and 278: Temperature Equilibration All sampl
- Page 279 and 280: Low-range pH Measurements (pH 1-7)
- Page 281 and 282: Preparation of Control Buffers 1. p
- Page 283 and 284: Standardization of pH Meter - Low p
- Page 285 and 286: Reference Electrode Care/Rejuvenati
- Page 287 and 288: Potentiometric Titrations for Photo
- Page 289 and 290: difference corresponds to the poten
- Page 291 and 292: Determination of Residual Thiosulfa
- Page 293 and 294: APPENDIX A Calibration Procedure Th
- Page 295 and 296: Determination of Silver in Thiosulf
- Page 297: Note: The appropriate amounts of 0.
- Page 301 and 302: Instructions for Performance Checks
- Page 303 and 304: Processing KODAK Motion Picture Fil
PROCEDURE C<br />
Determination of Silver in Thiosulfate Fixing Baths<br />
When Concentration of Silver is Less Than<br />
0.5 Grams per Liter.<br />
Note: When the concentration of silver is less than 0.5 g/L,<br />
it is possible to establish the silver content between two<br />
concentrations 0.05 g/L apart, using only graduated<br />
cylinders and the markings on the cylinders for all<br />
measurements.<br />
Treatment of Sample<br />
1. Obtain several 100-mL glass-stoppered graduated<br />
cylinders. Add to each 40 mL of fixing bath sample,<br />
20 mL of 0.2 M potassium ferricyanide, and 20 mL of<br />
6 N accelerator reagent. Stopper and shake to mix.<br />
2. Add from a polyethylene squeeze bottle to one of the<br />
cylinders, 20 mL of 0.00926 N thioacetamide, and to a<br />
second cylinder, add 10 mL.<br />
Note: 20 mL of 0.00926 N thioacetamide is equivalent<br />
to 0.5 g/L of silver and 10 mL is equivalent to<br />
0.25 g/L of silver.<br />
3. Stopper and shake the cylinders vigorously for 5<br />
seconds.<br />
4. Filter approximately 20 mL of the contents of each<br />
cylinder through Whatman No. 3 (12.5 cm diameter)<br />
filter paper and collect the filtrates in beakers<br />
containing approximately 5 mL of 0.00926 N<br />
thioacetamide each.<br />
5. Observe the appearance of the contents and refer to<br />
Table 3, Decision Sheet for Procedure C<br />
(40 mL Sample), to make the next decision.<br />
Reporting Results<br />
1. These two trials determine that:<br />
a. The procedure is not applicable (silver content is<br />
greater than 0.5 g/L)<br />
b. The silver content is below 0.25 g/L<br />
c. The silver content is between 0.25 and 0.5 g/L<br />
2. If the procedure is applicable, three or fewer trials will<br />
establish the silver content between two silver<br />
concentrations 0.05 grams per liter apart.<br />
Table 3 Decision Sheet for Procedure C (40 mL Sample)<br />
mL of<br />
0.00926 N<br />
Thioacetamide<br />
Added<br />
If the Contents of<br />
the Beaker<br />
Turns Color,<br />
Amount of Silver in<br />
Fix is More Than<br />
2 0.05 g/L<br />
4 0.10 g/L<br />
6 0.15 g/L<br />
8 0.20 g/L<br />
10 0.25 g/L<br />
12 0.30 g/L<br />
14 0.35 g/L<br />
16 0.40 g/L<br />
18 0.45 g/L<br />
20 0.50 g/L<br />
If the Contents of<br />
the Beaker<br />
Remains Clear,<br />
Amount of Silver in<br />
Fix is Less Than<br />
PROCEDURE D<br />
Determination of Exhaustion of Kodak Chemical<br />
Recovery Cartridge<br />
Note: When the concentration of silver in the effluent from<br />
the Recovery Cartridge exceeds 0.25 grams per litre, it can<br />
be assumed that the capacity of the cartridge has been<br />
exceeded. By selecting the 10 mL of 0.00926 thioacetamide<br />
(equivalent to 0.25 g/L of silver) and making only the one<br />
trial, a decision on exhaustion can be reached.<br />
Treatment of Sample<br />
1. Place in a 100-mL glass-stoppered graduated cylinder<br />
40 mL of fixing bath sample, 20 mL of 0.2 M<br />
potassium ferricyanide, and 20 mL of 6 N accelerator<br />
reagent. Stopper and shake to mix.<br />
2. Add 10 mL of 0.00926 N thioacetamide, stopper, and<br />
shake for 5 seconds.<br />
3. Filter approximately 20 mL of the mixture through a<br />
Whatman No. 3 filter paper into a beaker containing<br />
approximately 5 mL of 0.00926 N thioacetamide.<br />
Reporting Results<br />
1. Colored, the recovery cartridge is exhausted.<br />
2. Clear, the recovery cartridge is still serviceable.<br />
4 <strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03