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
APPARATUS All volumetric glassware should meet all “Class A” specifications, as defined by American Society for Testing and Materials (ASTM) Standards E 287, E 288, and E 969, unless otherwise stated. 3.0, 20.0-mL pipets 250-mL beakers Automatic titrator with stirrer, METROHM E536 or equivalent with a 50-mL buret ORION double-junction reference electrode 900200 or equivalent (10 percent KNO 3 outer filling solution) Platinum inlay electrode, BECKMAN #39273 or equivalent REAGENTS Use ACS Reagent Grade reagents unless otherwise specified. 0.1 N Potassium Iodate, KIO 3 (standardized to 4 decimal places) 0.6 M Potassium Iodide, KI 0.1 N Sodium Thiosulfate, Na 2 S 2 O 3 (standardized to 4 decimal places) 7 N Sulfuric Acid, H 2SO 4 Water, Type I Reagent—This method was developed using reagent water equivalent to 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 1. Pipet 40.0 mL (pipet two 20.0 mL portions) of standardized 0.10 N potassium iodate into a 250-mL beaker containing 50 mL of reagent water and TEFLON-coated stirring bar. 2. While stirring, add 25 mL of 7.0 N sulfuric acid and 25 mL of 0.6 M potassium iodide. 3. While stirring, immediately pipet 3.0 mL of sample near the surface of the liquid. Rinse the sides of the beaker with reagent water. 4. Place the electrodes in the beaker. (NOTE: The titrant delivery tip should be placed so that the titrant flows past the reference electrode before the platinum electrode.) Titrate the solution potentiometrically with standardized 0.10 N sodium thiosulfate solution while stirring. Use the following parameters with a METROHM E536 Potentiograph: Titration Rate: 15 min/100% volume Auto Control: OFF Selector Switch: mV/pH Measuring Span: 500 mV Buret Size: 50 mL Paper Drive: 400mm/100% volume Cut-off: OFF Counter Voltage: 0 mV Zero-Point Shift: left margin 5. Determine the volume, in mL, of 0.10 N sodium thiosulfate added to reach the end point using concentric arcs Method ULM-0003-01, Potentiometric Titrations for Photoprocessing Solutions, (or subsequent revision). This is mL A. 6. Repeat Steps 1-5, pipetting 40.0 mL (pipet two 20.0 mL portions) of standardized 0.10 N potassium iodate and substituting reagent water for the sample. This is the blank (mL B). 2 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03
CALCULATIONS Na2SO3 , g/L = (mL B – mL A) x (N Na2SO3 ) x (eq. wt.) x (1000) (mL sample) x (1000) Where: Example: = (mL B – mL A) x (N Na 2SO 3) x (63.02) x (1000) (3) x (1000) mL A = mL of Na2SO3 consumed by sample mL B = mL of Na2SO3 consumed by blank N Na2SO3 = Normality of Na2SO3 in milleq./mL used for titration eq. wt. Na2SO3 = 63.02 mg/meq mL sample = 3.0 mL 1000 = factor to convert mg to g in the numerator and mL to L in the denominator Na2SO3 , g/L = (40.32 – 21.98) x (0.0996 N Na2SO3) x (63.02) x (1000) (3)(1000) = 38.4 g/L Na 2 SO 3 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3
- Page 203 and 204: Potentiometric Determination of Bro
- Page 205 and 206: CALCULATIONS mL AgNO 3 that would b
- Page 207 and 208: Titrimetric Determination of Buffer
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- Page 211 and 212: Spectrophotometric Determination of
- Page 213 and 214: Titrimetric Determination of Citraz
- Page 215 and 216: Potentiometric Determination of Eth
- Page 217 and 218: Titrimetric Determination of Ferric
- Page 219 and 220: Iodometric Determination of Ferricy
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- Page 227 and 228: Titrimetric Determination of Hypo I
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- Page 233 and 234: Titration Note: For preparation of
- Page 235 and 236: Titrimetric Determination of Persul
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- Page 239 and 240: APPARATUS Spectrophotometer with a
- Page 241 and 242: APPENDIX B Effect of Temperature in
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- 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: Determination of Sulfite in KODAK R
- 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
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- Page 273 and 274: Table 1 Required Tolerance for Volu
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- Page 279 and 280: Low-range pH Measurements (pH 1-7)
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- Page 297 and 298: Note: The appropriate amounts of 0.
- Page 299 and 300: The Determination of Specific Gravi
- Page 301 and 302: Instructions for Performance Checks
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CALCULATIONS<br />
Na2SO3 , g/L = (mL B – mL A) x (N Na2SO3 ) x (eq. wt.) x (1000)<br />
(mL sample) x (1000)<br />
Where:<br />
Example:<br />
= (mL B – mL A) x (N Na 2SO 3) x (63.02) x (1000)<br />
(3) x (1000)<br />
mL A = mL of Na2SO3 consumed by sample<br />
mL B = mL of Na2SO3 consumed by blank<br />
N Na2SO3 = Normality of Na2SO3 in milleq./mL used<br />
for titration<br />
eq. wt. Na2SO3 = 63.02 mg/meq<br />
mL sample = 3.0 mL<br />
1000 = factor to convert mg to g in the numerator<br />
and mL to L in the denominator<br />
Na2SO3 , g/L = (40.32 – 21.98) x (0.0996 N Na2SO3) x (63.02) x (1000)<br />
(3)(1000)<br />
= 38.4 g/L Na 2 SO 3<br />
<strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3