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
PROCEDURE Sample Treatment 1. Pipet, wipe the pipet before leveling, 50.0 mL of standardized 0.1 N potassium iodate into a 250-mL Erlenmeyer flask. 2. Add 25 mL of 7.0 N sulfuric acid from a tip-up pipet. 3. Add 25 mL of 0.60 M potassium iodide from a tip-up pipet. 4. Pipet (wipe) 25.0 mL of sample into the flask. Titration 1. Titrate with standardized 0.1 N sodium thiosulfate to a light yellow color. Then, add 5 mL of starch indicator from a tip-up pipet and continue the titration until the blue color disappears. 2. Analyze for RA-1 using Method ECR-0001-1 (or subsequent revision). Calculations 1. Calculate the apparent total sulfite concentration using the following equation: Apparent Total Na 2 SO 3 , g/L = [(N KIO 3 )(mL KIO 3 ) – (N Na 2 S 2 O 3 )(mL Na 2 S 2 O 3 )](eq wt Na 2 SO 3 )(1000) = (mL sample)(1000) [(N KIO 3 )(50.0) – (N Na 2 S 2 O 3 )(mL Na 2 S 2 O 3 )](63.02)(1000) = (1.00)(1000) 2.521[(N KIO 3)(50.0) – (N Na 2S 2O 3)(mL Na 2S 2O 3)] 2. Correct the apparent sulfite concentration for RA-1 using the following equation: Total Na 2SO 3, g/L = (Apparent Na 2 SO 3 , g/L) – [0.0034 (RA-1, mg/L) – 0.001)] 2 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03
Titrimetric Determination of Total Alkalinity of a Processing Solution ECR-702J Process ECN-2 ECP-2D VNF-1/LC RVNP Formulas — — DR-100/101 DR-150/151 DR-105 DR-150 INTRODUCTION A critical appraisal of the pH, specific gravity, and total alkalinity of a developer mix is useful in detecting incorrect amounts of the inorganic constituents and certain of the organic constituents. PRINCIPLE The total alkalinity (T. Alk.) of a processing solution is defined as the millilitres of standardized 0.1 N sulfuric acid required to adjust a specified volume of processing solution to pH 4.3. That pH was selected because most salts derived from weak acids show an inflection point in their titration curves near pH 4.3. Samples that are colored (and some colorless samples) when titrated visually do not give a clear end point, thus causing excessive variability. For this reason, potentiometric titrations are recommended. Complete titration curves need not be plotted routinely. A pH meter can be used with glass and calomel electrodes. The instrument is standardized at the nominal temperature at which pH measurements are obtained. The temperature is usually 25°C (77°F). Table 2, Contribution of Constituents to Total Alkalinity of a Typical Replenisher Solution, shows the contribution of each constituent to the total alkalinity of two developers. The T. Alk. of the negative developer is mainly a measure of the sodium carbonate content. The T. Alk. of the print developers is primarily a measure of the carbonate but also indicates a significant contribution from the sulfite. The sample size is so chosen that the total volume of sulfuric acid consumed falls between 25 and 45 mL. The sample sizes must be specified with all total alkalinity analyses. This method requires handling potentially hazardous chemicals. Consult the Material Safety Data Sheet for each chemical before use. MSDS's are available from your chemical supplier. SPECIAL APPARATUS pH Meter or Automatic Titrator Calomel reference electrode filled with 3.5 N KCl, CORNING Model 476002, or equivalent pH Indicator electrode, CORNING Model 476024, or equivalent 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. 0.1 N Sulfuric Acid, H 2SO 4 (standardized to four decimal places) PROCEDURE Preparation of the Meter Follow Method ULM-191-2, pH Measurement of Photographic Processing Solutions (or any subsequent pH method), for making pH measurements below pH 9 Titration of the Sample and Reporting Results 1. Pipet the sample volume indicated below into a 150-mL beaker containing 50 mL of distilled water. The water should be approximately the same temperature as the buffer used in the cross-check Process Formula Sample Size VNF-1/LC DR-100/101 DR-150/151 4.00 mL 10.0 mL 2. Place the electrode assembly and stirrer in the solution, turn on the stirrer. 3. Titrate to a pH of 4.3 with standardized 0.1 N sulfuric acid, allowing the needle of the pH scale to equilibrate as the acid is slowly added. When the region of pH 5 is reached, add the titrant in 0.l0-mL increments, allowing the needle in the pH meter to equilibrate after each addition. 4. Report the mL of acid required to reach a pH of 4.3. Note: This is, by definition, the total alkalinity. Always indicate the sample size when reporting the results. 5. Remove the sample and rinse the electrode assembly with distilled water. If rinsing does not completely remove sample deposits, wipe the assembly with a cleansing tissue and rerinse. Replace in pH 4.01 potassium acid phthalate buffer. Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 1 RVNP DR-105 DR-150 4.00 mL 10.0 mL
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PROCEDURE<br />
Sample Treatment<br />
1. Pipet, wipe the pipet before leveling, 50.0 mL of<br />
standardized 0.1 N potassium iodate into a 250-mL<br />
Erlenmeyer flask.<br />
2. Add 25 mL of 7.0 N sulfuric acid from a tip-up pipet.<br />
3. Add 25 mL of 0.60 M potassium iodide from a tip-up<br />
pipet.<br />
4. Pipet (wipe) 25.0 mL of sample into the flask.<br />
Titration<br />
1. Titrate with standardized 0.1 N sodium thiosulfate to a<br />
light yellow color. Then, add 5 mL of starch indicator<br />
from a tip-up pipet and continue the titration until the<br />
blue color disappears.<br />
2. Analyze for RA-1 using Method ECR-0001-1 (or<br />
subsequent revision).<br />
Calculations<br />
1. Calculate the apparent total sulfite concentration using<br />
the following equation:<br />
Apparent Total Na 2 SO 3 , g/L =<br />
[(N KIO 3 )(mL KIO 3 ) – (N Na 2 S 2 O 3 )(mL Na 2 S 2 O 3 )](eq wt Na 2 SO 3 )(1000) =<br />
(mL sample)(1000)<br />
[(N KIO 3 )(50.0) – (N Na 2 S 2 O 3 )(mL Na 2 S 2 O 3 )](63.02)(1000) =<br />
(1.00)(1000)<br />
2.521[(N KIO 3)(50.0) – (N Na 2S 2O 3)(mL Na 2S 2O 3)]<br />
2. Correct the apparent sulfite concentration for RA-1<br />
using the following equation:<br />
Total Na 2SO 3, g/L =<br />
(Apparent Na 2 SO 3 , g/L) – [0.0034 (RA-1, mg/L) – 0.001)]<br />
2 <strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03