Processing kodak motion picture films, module 3 analytical procedures

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Example Raw Data µg S 2O 3 =)/cm 2 Absorbance Net Absorbance 0 (blank) 0.0849 0 0 (blank) 0.0821 0 0.5561 0.1196 0.0361 0.5561 0.1205 0.0370 2.224 0.1895 0.1060 2.224 0.1823 0.0988 4.449 0.3000 0.2165 4.449 0.2986 0.2151 8.898 0.5175 0.4340 8.898 0.5088 0.4253 15.571 0.7841 0.7006 15.571 0.8007 0.7172 22.245 1.1138 1.0303 22.245 1.1058 1.0223 33.367 1.5542 1.4707 33.367 1.5661 1.4826 From the data above, a linear regression yields: m (slope) = 22.467 µg S2O =/(cm 3 2 net A) b (intercept) = – 0.309 µg S2O =/cm 3 2 µg S 2O 3 =/cm 2 = 22.467 (net A) – 0.309 4 <strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03
Determination of Silver in Thiosulfate Fixing Baths (A Non-Instrumental Method Using Thioacetamide) 1209D Process ECN-2 ECP-2D VNF-1/LC RVNP Formulas F-34a F-35b F-35c F-36 F-38 PRINCIPLE This technique is basted on the work of Bush, Zuehlke, and Ballard, * but no instrument is required. The silver in a fixing bath is titrated, in effect, by adding graduated amounts of a thioacetamide solution to samples of the bath that have been adjusted to a pH greater than 12. At this alkalinity, thioacetamide decomposes to sulfide which immediately precipitates a chemically equivalent amount of silver sulfide. The silver sulfide is filtered and the filtrate is tested for completeness of silver precipitation by adding more thioacetamide. It is probable that this method will be used most frequently to determine the amount of silver in a fixing bath before and/ or after the fixing bath has passed through the Kodak Chemical Recovery Cartridge and associated Kodak Circulating Unit. A fix which has passed through this silver recovery unfit contains moderate amounts of ferrous iron ion. This method assumes that every fixer contains Iron II ions and includes a step to remove their effect before the conventional silver determination. The fixing solution must not have very much color, although some can be tolerated if a suitable blank is used. The practical extremes of measuring silver concentration by this technique are presented as Procedures A and B. Procedures C and D illustrate very useful specific modifications. Procedure A – Rapid Determination of the Approximate Silver Concentration in Thiosulfate Fixing Baths. Procedure B – Determination of Silver in Thiosulfate Fixing Baths. (This is a more precise procedure making use of pipets and burets.) Procedure C – Determination of Silver in Thiosulfate Fixing Baths When Concentration of Silver is Less Than 0.5 Grams per Liter. Procedure D – Special Application of Procedure C for Determination of Exhaustion of Kodak Chemical Recovery Cartridge. * D. G. Bush, C. W. Zuehlke, and A. E. Ballard, Analytical Chemistry, 31, 1368 (1959). RELIABILITY Eight fixing baths were prepared containing known amounts of silver and varying in pH from 4 to 10. Each contained some of the following items: conventional sequestering agents, sulfite (bisulfite), carbonate (bicarbonate), thiosulfate (sodium or ammonium), formaldehyde, acetate, borate, potassium alum, anti foaming agent, and citrate. The fixers were analyzed using Procedure B. End points were determined to 0.05 g/L. Of 30 results in the range from 0.50 to 6.00 g/L all were within 0.10 g/L of the nominal value and there appeared to be no bias. Ten acid hardening fixes were prepared to contain either 0.50 g or 5.00 g of silver and 0.1 to 10 g of Iron II ions. These were analyzed according to Procedure B and all results were within ± 0.2 g/L of the mix level. SPECIAL APPARATUS 100-ml Glass-Stoppered Graduated Cylinder (VWR Scientific, catalog no. 24760-100) 10-ml Graduated Cylinder (VWR Scientific, catalog no. 24710-044) Filter Paper, Whatman No. 3 (12.5 cm diameter) (VWR Scientific, catalog no. 28456-101) Torsion Balance, sensitivity 0.01 g REAGENTS 6.0 N Accelerator Reagent 0.00926 N Thioacetamide 0.1 M Potassium Ferricyanide 0.2 M Potassium Ferricyanide <strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 1
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©Eastman Kodak Company, 1999 Proce
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ECP-2-1101 Ferrocyanide in Ferricya
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3 Analytical Procedures for Chemica
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Spectrophotometric Determination of
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Potentiometric Determination of Bro
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PROCEDURE B For Seasoned Tank and R
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APPARATUS All volumetric glassware
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APPARATUS All pipettes and volumetr
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Potentiometric Determination of Amm
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PROCEDURE A. Sample Treatment 1. Pi
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Titrimetric Determination of Buffer
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Buffering Capacity Determination of
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Titrimetric Determination of EASTMA
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VISUAL TITRATION STATISTICS Repeata
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Back-Extraction of the Developing A
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Potentiometric Determination of Fer
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Recovery Recovery is used instead o
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CALCULATIONS For Na3Fe(CN) 6 g/L Na
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Cerimetric Determination of Sodium
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Bias Bias is a statistically signif
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APPARATUS Pipet (40-mL) Graduated C
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B. Analysis of Standards 1. Run eac
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Determination of Ferrous Iron in EA
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PROCEDURE Blank 1. Set a double-bea
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APPENDIX B This appendix contains t
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Titrimetric Determination of Hypo I
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B. Thiosulfate Determination 1. Sam
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Example Potentiometric Calculations
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APPARATUS Double Beam Spectrophotom
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APPENDIX II This appendix contains
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Calculations a. Range: 0.5-2.5 g/L
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APPENDIX 2 Typical Absorptivity mL
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Procedure Preparation of 10 g/L Iro
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Determination of Total Iron in East
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Determination of Total Iron in East
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Determination of Total Iron in EAST
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12. Press ‘ZERO’. The instrumen
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PROCEDURE A. Spectrophotometer Zero
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Absorptivity of Iron-Thiocyanate Co
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Potentiometric Determination of Unc
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Potentiometric Determination of Kod
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Titrimetric Determination of Persul
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APPARATUS Conical Flask with stoppe
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Potentiometric Determination of Sil
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APPARATUS METROHM 536 Titrator or e
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Potentiometric Determination of Sod
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PROCEDURE Treatment of the Sample 1
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Iodometric Determination of Sodium
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Determination of Sodium Sulfite in
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Procedure Treatment and Titration o
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Iodometric Determination of Sulfite
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Potentiometric Determination of Tot
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Automated Titration An example of a
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Titrimetric Determination of EASTMA
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VISUAL TITRATION STATISTICS Repeata
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Titration of the Developing Agent w
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Cerimetric Determination of CD-2 Co
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Cerimetric Determination of KODAK C
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Back-Extraction of CD-2 1. Add 50 m
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CALCULATIONS For Na3Fe(CN) 6 g/L Na
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Bias Bias is a statistically signif
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Hydroquinone in Sound Track Develop
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B. Thiosulfate Determination 1. Sam
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Examples: Titration mL 0.1 N Na 2S
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Potentiometric Determination of Pot
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PROCEDURE A. Preparation of Sample
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APPARATUS Conical Flask with stoppe
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Determination of the pH of the East
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Determination of the pH of Processe
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Potentiometric Determination of Sil
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Determination of Sodium Metabisulfi
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II. Visual Endpoint Titrations A. R
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Viscosity Determination of Sound-Tr
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Titrimetric Determination Of Benzyl
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PROCEDURE B For Seasoned Tank Note:
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CALCULATIONS mL AgNO 3 that would b
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Titrimetric Determination of Buffer
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Titrimetric Determination of Citraz
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Potentiometric Determination of Eth
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Titrimetric Determination of Ferric
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Iodometric Determination of Ferricy
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Iodometric Determination of Formali
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Potentiometric Determination of Iod
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Potentiometric Determination of Pot
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Titration Note: For preparation of
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APPARATUS Spectrophotometer with a
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APPENDIX B Effect of Temperature in
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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 -
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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
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Page 279 and 280: Low-range pH Measurements (pH 1-7)
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Page 291 and 292: Determination of Residual Thiosulfa
Page 293: APPENDIX A Calibration Procedure Th
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Page 299 and 300: The Determination of Specific Gravi
Page 301 and 302: Instructions for Performance Checks
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