Processing kodak motion picture films, module 3 analytical procedures

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12. Substitute the following sample sizes in Step 8. Sample size A std 13. Each of the standards needs to be analyzed at least three times. Calculation of the Absorptivity Where: 4 mL A std #2 5 mL A std #3 10 mL A std #4 Absorptivity, L/(g-cm) = A x DF Assay A = absorbance measured at 474 rnm Assay = the value determined below DF = the dilution factor, Absorptivity for std. #1 = Absorptivity for std. #2 = Absorptivity for std. #3 = Absorptivity for std. #4 = ( 500 100 x ) 5 sample size 3333 for std. #1 2500 for std. #2 2000 for std. #3 1000 for std. #4 3333 x A std #1 Assay 2500 x A std #2 Assay 2000 x A std #3 Assay 1000 x A std #4 Assay A typical absorptivity is 190.0 L/(g-cm) (see APPENDIX 2, Typical Absorptivity). Calculate a mean absorptivity using the data from the triplicate analysis of the standards. The mean value should have a RSD < 1.0%. Mean = RSD = s A A = A n ; x 100% Standard Deviation(s) = (A - A) n-1 where: A = individual absorbance measurements n = 12 See APPENDIX 2, Typical Absorptivity for an example of sample data. 2 Assay of 5 g/L Iron Solution 1. This assay procedure should be performed in triplicate. 2. Pipet 25.0 mL of the stock solution of 5 g/L Fe into a 500-mL glass stoppered ERLEMMEYER flask containing 100 mL of distilled water. 3. Add 5 mL of concentrated Hydrochloric Acid and 3 ± 0.1 g of Potassium Iodide. 4. Stopper and swirl the flask to dissolve the Potassium Iodide. Store in a dark place for 30 minutes. 5. After the 30 minutes, remove the flask from the dark and titrate with standardized 0.1 N Sodium Thiosulfate (50-mL buret) from a red color to a yellow-red color change. 6. Add 3 mL Starch indicator solution and continue titrating until the blue to colorless endpoint persists for 15 seconds. This is mLspl . 7. Into another 500-mL ERLENMEYER flask, add 100 mL distilled water, 5 mL concentrated Hydrochloric Acid and 3 g Potassium Iodide. 8. Stopper the flask and swirl as in Step 4. Store in the dark for 30 minutes. 9. After 30 minutes, add 3 mL Starch indicator solution. 10. Swirl and titrate with standardized 0.1 N Sodium Thiosulfate (50-mL beret). Titrate to the same persistent color observed in step 6, above. This is mLblk . 11. Each of the standards needs to be analyzed at least three times. Calculation of the Absorptivity g/L Fe) = Where: Calculate the mean, standard deviation and RSD of the assay. The RSD should be < 0.5%. Where: mL x Ew x N 25.0 Ew = Equivalent weight of Iron, 55.85 25.0 = Sample size in mL N = Normality of the Sodium Thiosulfate mL = mLSpl - mLblk Mean = X = RSD = x 100% Ew = the individual result n = the number of replicates (3) F010_0088 4 <strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 s X n X Standard Deviation(s) = (X - X) n-1 2
APPENDIX 2 Typical Absorptivity mL Diluted Stock Absorbance Absorptivity 3 0.279 189.48 3 0.279 189.48 3 0.286 192.19 4 0.381 192.04 4 0.374 188.50 4 0.381 192.04 5 0.467 188.31 5 0. 475 191.53 5 0.475 191.53 10 0.935 188.51 10 0.939 189.31 10 0.939 189.31 X = 190.2 S = ± 1.5 RSD = ± 0.8% <strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 5
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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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Page 35 and 36: Potentiometric Determination of Fer
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Page 39 and 40: CALCULATIONS For Na3Fe(CN) 6 g/L Na
Page 41 and 42: Cerimetric Determination of Sodium
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Page 47 and 48: Spectrophotometric Determination of
Page 49 and 50: APPARATUS Pipet (40-mL) Graduated C
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Page 53 and 54: Determination of Ferrous Iron in EA
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Page 85 and 86: Procedure Preparation of 10 g/L Iro
Page 87 and 88: Determination of Total Iron in East
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Page 105 and 106: Titrimetric Determination of Persul
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Page 115 and 116: PROCEDURE Treatment of the Sample 1
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Buffering Capacity Determination of
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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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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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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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Bias Bias is a statistically signif
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Hydroquinone in Sound Track Develop
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Titrimetric Determination of Hypo I
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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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APPARATUS All volumetric glassware
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Potentiometric Determination of Kod
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PROCEDURE A. Preparation of Sample
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Titrimetric Determination of Persul
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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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APPARATUS METROHM 536 Titrator or e
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Determination of Sodium Metabisulfi
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II. Visual Endpoint Titrations A. R
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APPARATUS METROHM 536 Titrator or e
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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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Potentiometric Determination of Kod
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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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Titrimetric Determination of Hypo I
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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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Titrimetric Determination of Persul
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APPARATUS Spectrophotometer with a
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APPENDIX B Effect of Temperature in
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Potentiometric Determination of Sil
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Potentiometric Determination of Sod
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Iodometric Determination of Total S
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Titrimetric Determination of Total
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Table 2 Contribution of Constituent
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Determination of Sulfite in KODAK R
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CALCULATIONS Na2SO3 , g/L = (mL B -
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Colorimetric Determination of Thioc
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APPENDIX A Calibration of Spectroph
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Analysis Order for Photographic Pro
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Procedure for Electroplating a Silv
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The Selection, Care, and Use of Vol
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In observing the lowest point on th
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4. Graduated Cylinders and Tip-up P
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6. Microburets Microburets equipped
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Table 1 Required Tolerance for Volu
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pH Measurement of Photographic Proc
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Temperature Equilibration All sampl
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Low-range pH Measurements (pH 1-7)
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Preparation of Control Buffers 1. p
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Standardization of pH Meter - Low p
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Reference Electrode Care/Rejuvenati
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Potentiometric Titrations for Photo
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difference corresponds to the poten
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Determination of Residual Thiosulfa
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APPENDIX A Calibration Procedure Th
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Determination of Silver in Thiosulf
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Note: The appropriate amounts of 0.
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The Determination of Specific Gravi
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Instructions for Performance Checks
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Processing KODAK Motion Picture Fil
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