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

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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

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

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