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 A Rapid Determination of the Approximate Silver Concentration in Thiosulfate Fixing Baths Note: Use the markings on the cylinders for all measurement. Treatment of Sample 1. Obtain three 100-mL glass-stoppered graduated cylinders (labeled 2, 4, and 6). Add to each graduated cylinder 10 mL of fixing bath sample, 10 mL of 0.1 M potassium ferricyanide, and 10 mL of 6 N accelerator reagent. Swirl to mix. If the resulting color is: a. Reddish-brown, proceed to Step 2. b. Black, add 10 ml more of 0.1 M potassium ferricyanide and swirl to mix. Proceed to Step 2 if the resulting color is reddish-brown. If not, start over again, using a fresh sample and a 0.2 M potassium ferricyanide reagent. 2. Using a polyethylene squeeze bottle, add to the cylinders the following volumes of 0.00926 N thioacetamide: Cylinder mL 0.0926 N Thioacetamide Identification 2 20 4 40 6 60 3. Stopper and shake all cylinders vigorously for 5 seconds. 4. Filter approximately 20 ml of the contents of each cylinder through a Whatman No. 3 (12.5 cm diameter) filter paper and collect the filtrates in beakers containing approximately 5 mL of 0.00926 N thioacetamide. 5. Observe the appearance of the beakers’ contents and refer to Table 1, Decision Sheet for Determining Silver Concentration Range (10 mL Sample) Procedure A. Reporting Results 1. The results from these three cylinders permit the conclusion that the silver content of the fix is: a. less than 2 g/L b. between 2 and 4 g/L c. between 4 and 6 g/L d. over 6 g/L * 2. One more individual trial will suffice to establish the silver content between two silver concentrations 1.0 g/L apart (See PROCEDURE B). * If the silver content is more than 6 g/L, dilute the sample with an equal volume of water and rerun the determinations corresponding to cylinders 2, 4, and 6. Remember to multiply any final answer by 2. Table 1 Decision Sheet for Determining Silver Concentration Range (10 mL Sample) Procedure A Cylinder No. 0.00926 N Thioacetamide Added If the Contents of the Beaker Turns Color, * Amount of Silver in Fix is More Than 1 10 1.0 g/L 2 20 2.0 g/L 3 30 3.0 g/L 4 40 4.0 g/L 5 50 5.0 g/L 6 60 6.0 g/L If the Contents of the Beaker Remains Clear, † Amount of Silver in Fix is Less Than * The color in the beaker is greater than a blank consisting of appropriate amounts of sample, potassium ferricyanide, 6 N NaOH-EDTA reagent and water (in place of 0.00926 N thioacetamide) which have been filtered, the filtrate being collected in about 5 mL of water. † The color in the beaker is not greater than a blank prepared as above. PROCEDURE B Determination of Silver in Thiosulfate Fixing Baths Note: Procedure A has established the approximate silver concentration. If it is desirable to determine the concentration more precisely, it is necessary to “zero-in” on the end point by measuring volumes with pipets and burets and by using smaller increments of 0.00926 N thioacetamide in the end point region. This procedure establishes the silver content between two concentrations 0.1 g/L apart, with three or fewer trials. Treatment of Sample 1. Pipet into 4 100-ml glass-stoppered graduated cylinders 10.0 mL of fixing bath. Using the markings on the cylinders, add to one of the cylinders 10 mL of 0.1 potassium ferricyanide, and 10 mL of 6 N accelerator reagent. Swirl to mix. If the resulting color is: a. reddish-brown, proceed to Step 2. b. black, add 10 mL more of 0.1 N potassium ferricyanide. Swirl to mix. Proceed to Step 2 if the resulting color is reddish-brown. If not, start over again using a fresh sample and a 0.2 M potassium ferricyanide reagent. Prepare the remaining cylinders similarly. 2. Add from a buret the appropriate amount of 0.00926 N thioacetamide to each cylinder. 2 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03
Note: The appropriate amounts of 0.00926 N thioacetamide are selected from Table 2, Decision Sheet for Determining Silver Concentration (10.00 mL Sample) Procedure B, and are based on the silver concentration found in Procedure A. For example, if the concentration was found to be more than 2 but less than 3 grams per liter, the region to explore is between 2 and 3. Increments shown are in 1.0 mL 0.00926 N thioacetamide (equivalent to 0.1 g Ag/1). To obtain greater efficiency, the end point may be approached by trying one at about 2.5 g/L and then one at 2.3 g/L or 2.7 g/L, depending on the result obtained with 2.5 g/L. 3. Stopper and shake all cylinders vigorously for 5 seconds. 4. Filter approximately 20 mL of the contents of each cylinder through a 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. Reporting Results Observe the appearance of the contents of the beakers and refer to Table 2, Decision Sheet for Determining Silver Concentration (10.00 mL Sample) Procedure B, for decisions, and details of further trials, if necessary. Table 2 Decision Sheet for Determining Silver Concentration (10.00 mL Sample) Procedure B Range g/L 0.00926 N Thioacetamide To Add 0 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 1 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00 2 20.00 21.00 22.00 23.00 24.00 25.00 26.00 27.00 28.00 29.00 If the Contents of the Beaker Turns Color, Amount of Silver in Fix is More Than 0.1 g/L 0.2 g/L 0.3 g/L 0.4 g/L 0.5 g/L 0.6 g/L 0.7 g/L 0.8 g/L 0.9 g/L 1.0 g/L 1.1 g/L 1.2 g/L 1.3 g/L 1.4 g/L 1.5 g/L 1.6 g/L 1.7 g/L 1.8 g/L 1.9 g/L 2.0 g/L 2.1 g/L 2.2 g/L 2.3 g/L 2.4 g/L 2.5 g/L 2.6 g/L 2.7 g/L 2.8 g/L 2.9 g/L If the Contents of the Beaker Remains Clear, Amount of Silver in Fix is Less Than Range g/L 0.00926 N Thioacetamide To Add 3 30.00 31.00 32.00 33.00 34.00 35.00 36.00 37.00 38.00 39.00 4 40.00 41.00 42.00 43.00 44.00 45.00 46.00 47.00 48.00 49.00 5 50.00 51.00 52.00 53.00 54.00 55.00 56.00 57.00 58.00 59.00 If the Contents of the Beaker Turns Color, Amount of Silver in Fix is More Than 3.0 g/L 3.1 g/L 3.2 g/L 3.3 g/L 3.4 g/L 3.5 g/L 3.6 g/L 3.7 g/L 3.8 g/L 3.9 g/L 4.0 g/L 4.1 g/L 4.2 g/L 4.3 g/L 4.4 g/L 4.5 g/L 4.6 g/L 4.7 g/L 4.8 g/L 4.9 g/L 5.0 g/L 5.1 g/L 5.2 g/L 5.3 g/L 5.4 g/L 5.5 g/L 5.6 g/L 5.7 g/L 5.8 g/L 5.9 g/L 6 60.00 6.0 g/L If the Contents of the Beaker Remains Clear, Amount of Silver in Fix is Less Than Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3
- Page 245 and 246: Potentiometric Determination of Sod
- 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: Determination of Silver in Thiosulf
- Page 299 and 300: The Determination of Specific Gravi
- Page 301 and 302: Instructions for Performance Checks
- Page 303 and 304: Processing KODAK Motion Picture Fil
Note: The appropriate amounts of 0.00926 N thioacetamide<br />
are selected from Table 2, Decision Sheet for Determining<br />
Silver Concentration (10.00 mL Sample) Procedure B, and<br />
are based on the silver concentration found in Procedure A.<br />
For example, if the concentration was found to be more<br />
than 2 but less than 3 grams per liter, the region to explore is<br />
between 2 and 3. Increments shown are in 1.0 mL 0.00926 N<br />
thioacetamide (equivalent to 0.1 g Ag/1). To obtain greater<br />
efficiency, the end point may be approached by trying one at<br />
about 2.5 g/L and then one at 2.3 g/L or 2.7 g/L, depending<br />
on the result obtained with 2.5 g/L.<br />
3. Stopper and shake all cylinders vigorously for<br />
5 seconds.<br />
4. Filter approximately 20 mL of the contents of each<br />
cylinder through a 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 />
Reporting Results<br />
Observe the appearance of the contents of the beakers and<br />
refer to Table 2, Decision Sheet for Determining Silver<br />
Concentration (10.00 mL Sample) Procedure B, for<br />
decisions, and details of further trials, if necessary.<br />
Table 2 Decision Sheet for Determining Silver<br />
Concentration (10.00 mL Sample) Procedure B<br />
Range<br />
g/L<br />
0.00926 N<br />
Thioacetamide<br />
To Add<br />
0 1.00<br />
2.00<br />
3.00<br />
4.00<br />
5.00<br />
6.00<br />
7.00<br />
8.00<br />
9.00<br />
1 10.00<br />
11.00<br />
12.00<br />
13.00<br />
14.00<br />
15.00<br />
16.00<br />
17.00<br />
18.00<br />
19.00<br />
2 20.00<br />
21.00<br />
22.00<br />
23.00<br />
24.00<br />
25.00<br />
26.00<br />
27.00<br />
28.00<br />
29.00<br />
If the Contents<br />
of the Beaker<br />
Turns Color,<br />
Amount of<br />
Silver in Fix is<br />
More Than<br />
0.1 g/L<br />
0.2 g/L<br />
0.3 g/L<br />
0.4 g/L<br />
0.5 g/L<br />
0.6 g/L<br />
0.7 g/L<br />
0.8 g/L<br />
0.9 g/L<br />
1.0 g/L<br />
1.1 g/L<br />
1.2 g/L<br />
1.3 g/L<br />
1.4 g/L<br />
1.5 g/L<br />
1.6 g/L<br />
1.7 g/L<br />
1.8 g/L<br />
1.9 g/L<br />
2.0 g/L<br />
2.1 g/L<br />
2.2 g/L<br />
2.3 g/L<br />
2.4 g/L<br />
2.5 g/L<br />
2.6 g/L<br />
2.7 g/L<br />
2.8 g/L<br />
2.9 g/L<br />
If the Contents<br />
of the Beaker<br />
Remains Clear,<br />
Amount of<br />
Silver in Fix is<br />
Less Than<br />
Range<br />
g/L<br />
0.00926 N<br />
Thioacetamide<br />
To Add<br />
3 30.00<br />
31.00<br />
32.00<br />
33.00<br />
34.00<br />
35.00<br />
36.00<br />
37.00<br />
38.00<br />
39.00<br />
4 40.00<br />
41.00<br />
42.00<br />
43.00<br />
44.00<br />
45.00<br />
46.00<br />
47.00<br />
48.00<br />
49.00<br />
5 50.00<br />
51.00<br />
52.00<br />
53.00<br />
54.00<br />
55.00<br />
56.00<br />
57.00<br />
58.00<br />
59.00<br />
If the Contents<br />
of the Beaker<br />
Turns Color,<br />
Amount of<br />
Silver in Fix is<br />
More Than<br />
3.0 g/L<br />
3.1 g/L<br />
3.2 g/L<br />
3.3 g/L<br />
3.4 g/L<br />
3.5 g/L<br />
3.6 g/L<br />
3.7 g/L<br />
3.8 g/L<br />
3.9 g/L<br />
4.0 g/L<br />
4.1 g/L<br />
4.2 g/L<br />
4.3 g/L<br />
4.4 g/L<br />
4.5 g/L<br />
4.6 g/L<br />
4.7 g/L<br />
4.8 g/L<br />
4.9 g/L<br />
5.0 g/L<br />
5.1 g/L<br />
5.2 g/L<br />
5.3 g/L<br />
5.4 g/L<br />
5.5 g/L<br />
5.6 g/L<br />
5.7 g/L<br />
5.8 g/L<br />
5.9 g/L<br />
6 60.00 6.0 g/L<br />
If the Contents<br />
of the Beaker<br />
Remains Clear,<br />
Amount of<br />
Silver in Fix is<br />
Less Than<br />
<strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3