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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RELIABILITY Procedure A—The 95 percent confidence limits for an individual analysis of a fresh tank or replenisher sample are estimated to be slightly less than ± 0.05 g/L NaBr. Procedure B—This procedure was specifically designed for current mix formulations and variance due to seasoning. Any change in mix formulation, especially in bromide concentration, may necessitate recalibration. This procedure will accurately analyze bromide in seasoned tank and reconstituted replenisher solutions containing as much as 1.5 g/L sodium bromide in SD-49 developer and 2.10 g/L sodium bromide in SD-50 or SD-51 developer. Analytical results will be low on solutions exceeding these concentrations of sodium bromide. Eight seasoned samples in the appropriate bromide concentration range were analyzed by three analysts. Based on 24 data points obtained, the 95 percent confidence limits for an individual determination are ± 0.05 g/L sodium bromide. SPECIAL APPARATUS pH Meter Reference Electrode, Double Junction, Orion No.900200 or equivalent Indicator Electrode, Silver Billet, Beckman No. 39261 or equivalent Millipore Filter apparatus Millipore Filter membrane (0.45 micron porosity 47 mm) Exhaust Hood Note: Use pipets and volumetric glassware meeting the “Class A” definition by the National Institute of Standards and Technology (NIST). REAGENTS Use ACS Reagent Grade reagents unless specified otherwise. 1.0 M Ammonium Nitrate, NH 4NO3 Celite Silver Halide Developer 0.05 N Silver Nitrate, AgNO 3 (standardized to 4 decimal places) 18 N Sulfuric Acid, H 2SO4 PROCEDURE A For Fresh Tank and Replenisher Note: Prepare the double junction/silver billet electrode pair and calibrate the electrode-instrument system according to the instructions given in Method ULM-0003-01, Potentiometric Titrations for Photoprocessing Solutions or any subsequent revision. Sample Treatment (Perform in an Exhaust Hood) 1. Pipet, wipe the pipes before leveling, 50.0 mL of sample into a 250-mL beaker. Warning ACID. Avoid contact with skin and eyes. In case of contact, flush with water. 2. Stir the sample moderately on a magnetic stirrer and add very slowly from a tip-up pipes, the indicated volume of 18 N sulfuric acid. Titration 1. Using a 25-mL buret, titrate the sample potentiometrically, according to Method ULM-0003-01, with standardized 0.05 N silver nitrate. Note: The titration may be performed most rapidly in the beginning where the potential change is the smallest. Refer to Figures 1 and 2 to determine the increment size to use in the region of the end point and the expected potential change in millivolts. 2. Determine the end point using concentric arcs from Method ULM-0003-01, Potentiometric Titrations for Photoprocessing Solutions. Calculations Process Formula Acid ECN-2 SD-49/49R 25 mL ECP-2B SD-50/50R SD-51/51R 50 mL 50 mL NaBr, g/L = (N AgNO3 )(mL AgNO3 ) x (eq. wt. NaBr) x (1000) = (mL sample) x (1000) (N AgNO 3 )(mL AgNO 3 ) x (102.91) x (1000) (50) x (1000) 2.058(mL AgNO 3)(N AgNO 3) 2 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 =

PROCEDURE B For Seasoned Tank and Reconstituted Replenishers Note: Prepare the double junction/silver billet electrode pair and calibrate the electrode-instrument system according to the instructions given in Method ULM-0003-01, Potentiometric Titrations for Photoprocessing Solutions or any subsequent revision. Sample Treatment (Bromide Enrichment) 1. Pipet, wipe the pipes before leveling, 50.0 mL of sample into a 250-mL Phillips beaker. Stir moderately on a magnetic stirrer in an exhaust hood. Warning ACID. Avoid contact with skin and eyes. In case of contact, flush with water. 2. While stirring add very slowly, from a tip-up pipes, 50 mL of 18 N sulfuric acid to the Phillips beaker. 3. Add approximately 0.2 grams of Celite to the Phillips beaker. (One level scoop from a Coors No. 04 porcelain spatula is approximately 0.2 grams.) 4. Add, from a graduated cylinder, the indicated amount of standardized 0.05 N silver nitrate to the solution as it stirs. Immediately set a timer for 5 minutes and continue to stir during that period. Process Formula Acid ECN-2 SD-49/49R 15 mL ECP-2B SD-50/50R SD-51/51R 20 mL 20 mL 5. As the solution stirs, assemble a Millipore filter holder and filter membrane (type HAWP—0.45 micron porosity, 47 mm) on a 250-mL filter flask. 6. At the end of the five-minute stirring period, connect the aspirator hose and filter the solution through the Millipore apparatus, retaining the stirring bar in the Phillips beaker by means of another may-bar outside the beaker. When filtering is completed, disconnect the aspirator hose. 7. Rinse the sides of the Phillips beaker with 25 mL of 1.0 M ammonium nitrate from a tip-up pipet. Retaining the stirring bar in the Phillips beaker, rinse the sides of the Millipore funnel by pouring the solution through a long, thin-stemmed glass funnel. Reconnect the aspirator hose and filter the solution into the 250-mL filter flask. Disconnect the aspirator hose when the filtering is completed. Save both the long-stemmed funnel and the Phillips beaker. 8. Remove the 250-mL filter flask from the Millipore filter apparatus and discard the filtrate. Do not disassemble the Millipore filter apparatus. 9. Rinse the inside and outside of the stem only of the Millipore funnel with distilled water from a wash bottle, and place the filter apparatus on a clean 250-mL filter flask. Silver Development 1. Add, from a graduated cylinder, 25 mL of silver halide developer to the 250-mL Phillips beaker. Note: Do not expose the silver halide developer to air any longer than necessary When not in use, store the silver-halide developer in a cool, dark place. A developer that has turned brown should not be used. The developer is still usable if it has a light tan color. 2. Swirl the Phillips beaker and immediately rinse the sides of the Millipore funnel (with no applied suction) by pouring the developer through the long-stemmed funnel. Set a timer for five minutes and allow the developer to remain in the Millipore funnel for that period. At one-minute intervals, swirl the Millipore funnel for several seconds. 3. During the five-minute period, add from a tip-up pipet, 25 mL of distilled water to the 250-mL Phillips beaker. 4. At the end of the five-minute period, connect the aspirator hose and filter the solution into the clean 250mL filter flask. (Care must be taken to prevent loss of the filtrate through the aspirator hose.) With the aspirator hose still connected, rinse the sides of the Millipore funnel with the solution in the Phillips beaker by pouring the solution through the longstemmed funnel. Disconnect the aspirator hose when the filtration is completed. 5. Quantitatively transfer the solution in the 250-mL filter flask into a 400-mL beaker using a maximum of 100 mL of distilled water. 6. Stir the solution moderately on a magnetic stirrer in an exhaust hood. Warning ACID. Avoid contact with skin and eyes. In case of contact, flush with water. 7. Add carefully from a tip-up pipet, 50 mL of 18 N sulfuric acid to the beaker. Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3

PROCEDURE B<br />

For Seasoned Tank and Reconstituted<br />

Replenishers<br />

Note: Prepare the double junction/silver billet electrode pair<br />

and calibrate the electrode-instrument system according to<br />

the instructions given in Method ULM-0003-01,<br />

Potentiometric Titrations for Photoprocessing Solutions or<br />

any subsequent revision.<br />

Sample Treatment<br />

(Bromide Enrichment)<br />

1. Pipet, wipe the pipes before leveling, 50.0 mL of<br />

sample into a 250-mL Phillips beaker. Stir moderately<br />

on a magnetic stirrer in an exhaust hood.<br />

Warning<br />

ACID. Avoid contact with skin and eyes. In case of<br />

contact, flush with water.<br />

2. While stirring add very slowly, from a tip-up pipes, 50<br />

mL of 18 N sulfuric acid to the Phillips beaker.<br />

3. Add approximately 0.2 grams of Celite to the Phillips<br />

beaker. (One level scoop from a Coors No. 04<br />

porcelain spatula is approximately 0.2 grams.)<br />

4. Add, from a graduated cylinder, the indicated amount<br />

of standardized 0.05 N silver nitrate to the solution as<br />

it stirs. Immediately set a timer for 5 minutes and<br />

continue to stir during that period.<br />

Process Formula Acid<br />

ECN-2 SD-49/49R 15 mL<br />

ECP-2B<br />

SD-50/50R<br />

SD-51/51R<br />

20 mL<br />

20 mL<br />

5. As the solution stirs, assemble a Millipore filter holder<br />

and filter membrane (type HAWP—0.45 micron<br />

porosity, 47 mm) on a 250-mL filter flask.<br />

6. At the end of the five-minute stirring period, connect<br />

the aspirator hose and filter the solution through the<br />

Millipore apparatus, retaining the stirring bar in the<br />

Phillips beaker by means of another may-bar outside<br />

the beaker. When filtering is completed, disconnect<br />

the aspirator hose.<br />

7. Rinse the sides of the Phillips beaker with 25 mL of 1.0<br />

M ammonium nitrate from a tip-up pipet. Retaining<br />

the stirring bar in the Phillips beaker, rinse the sides of<br />

the Millipore funnel by pouring the solution through a<br />

long, thin-stemmed glass funnel. Reconnect the<br />

aspirator hose and filter the solution into the 250-mL<br />

filter flask. Disconnect the aspirator hose when the<br />

filtering is completed. Save both the long-stemmed<br />

funnel and the Phillips beaker.<br />

8. Remove the 250-mL filter flask from the Millipore<br />

filter apparatus and discard the filtrate. Do not<br />

disassemble the Millipore filter apparatus.<br />

9. Rinse the inside and outside of the stem only of the<br />

Millipore funnel with distilled water from a wash<br />

bottle, and place the filter apparatus on a clean 250-mL<br />

filter flask.<br />

Silver Development<br />

1. Add, from a graduated cylinder, 25 mL of silver halide<br />

developer to the 250-mL Phillips beaker.<br />

Note: Do not expose the silver halide developer to air<br />

any longer than necessary When not in use, store the<br />

silver-halide developer in a cool, dark place. A<br />

developer that has turned brown should not be used.<br />

The developer is still usable if it has a light tan color.<br />

2. Swirl the Phillips beaker and immediately rinse the<br />

sides of the Millipore funnel (with no applied suction)<br />

by pouring the developer through the long-stemmed<br />

funnel. Set a timer for five minutes and allow the<br />

developer to remain in the Millipore funnel for that<br />

period. At one-minute intervals, swirl the Millipore<br />

funnel for several seconds.<br />

3. During the five-minute period, add from a tip-up pipet,<br />

25 mL of distilled water to the 250-mL Phillips beaker.<br />

4. At the end of the five-minute period, connect the<br />

aspirator hose and filter the solution into the clean 250mL<br />

filter flask. (Care must be taken to prevent loss of<br />

the filtrate through the aspirator hose.) With the<br />

aspirator hose still connected, rinse the sides of the<br />

Millipore funnel with the solution in the Phillips<br />

beaker by pouring the solution through the longstemmed<br />

funnel. Disconnect the aspirator hose when<br />

the filtration is completed.<br />

5. Quantitatively transfer the solution in the 250-mL<br />

filter flask into a 400-mL beaker using a maximum of<br />

100 mL of distilled water.<br />

6. Stir the solution moderately on a magnetic stirrer in an<br />

exhaust hood.<br />

Warning<br />

ACID. Avoid contact with skin and eyes. In case of<br />

contact, flush with water.<br />

7. Add carefully from a tip-up pipet, 50 mL of 18 N<br />

sulfuric acid to the beaker.<br />

<strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3

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