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Processing kodak motion picture films, module 3 analytical procedures

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Titrimetric Determination of Total Alkalinity of a <strong>Processing</strong> Solution<br />

ECR-702J<br />

Process ECN-2 ECP-2D VNF-1/LC RVNP<br />

Formulas — —<br />

DR-100/101<br />

DR-150/151<br />

DR-105<br />

DR-150<br />

INTRODUCTION<br />

A critical appraisal of the pH, specific gravity, and total<br />

alkalinity of a developer mix is useful in detecting incorrect<br />

amounts of the inorganic constituents and certain of the<br />

organic constituents.<br />

PRINCIPLE<br />

The total alkalinity (T. Alk.) of a processing solution is<br />

defined as the millilitres of standardized 0.1 N sulfuric acid<br />

required to adjust a specified volume of processing solution<br />

to pH 4.3. That pH was selected because most salts derived<br />

from weak acids show an inflection point in their titration<br />

curves near pH 4.3.<br />

Samples that are colored (and some colorless samples)<br />

when titrated visually do not give a clear end point, thus<br />

causing excessive variability. For this reason, potentiometric<br />

titrations are recommended. Complete titration curves need<br />

not be plotted routinely.<br />

A pH meter can be used with glass and calomel electrodes.<br />

The instrument is standardized at the nominal temperature at<br />

which pH measurements are obtained. The temperature is<br />

usually 25°C (77°F).<br />

Table 2, Contribution of Constituents to Total Alkalinity<br />

of a Typical Replenisher Solution, shows the contribution of<br />

each constituent to the total alkalinity of two developers. The<br />

T. Alk. of the negative developer is mainly a measure of the<br />

sodium carbonate content. The T. Alk. of the print<br />

developers is primarily a measure of the carbonate but also<br />

indicates a significant contribution from the sulfite.<br />

The sample size is so chosen that the total volume of<br />

sulfuric acid consumed falls between 25 and 45 mL. The<br />

sample sizes must be specified with all total alkalinity<br />

analyses.<br />

This method requires handling potentially hazardous<br />

chemicals. Consult the Material Safety Data Sheet for each<br />

chemical before use. MSDS's are available from your<br />

chemical supplier.<br />

SPECIAL APPARATUS<br />

pH Meter or Automatic Titrator<br />

Calomel reference electrode filled with 3.5 N KCl,<br />

CORNING Model 476002, or equivalent<br />

pH Indicator electrode, CORNING Model 476024, or<br />

equivalent<br />

Note: Use pipets and volumetric glassware meeting the<br />

“Class A” definition by the National Institute of Standards<br />

and Technology (NIST)<br />

REAGENTS<br />

Use ACS Reagent Grade reagents unless specified<br />

otherwise.<br />

0.1 N Sulfuric Acid, H 2SO 4<br />

(standardized to four decimal places)<br />

PROCEDURE<br />

Preparation of the Meter<br />

Follow Method ULM-191-2, pH Measurement of<br />

Photographic <strong>Processing</strong> Solutions (or any subsequent pH<br />

method), for making pH measurements below pH 9<br />

Titration of the Sample and Reporting Results<br />

1. Pipet the sample volume indicated below into a<br />

150-mL beaker containing 50 mL of distilled water.<br />

The water should be approximately the same<br />

temperature as the buffer used in the cross-check<br />

Process Formula Sample Size<br />

VNF-1/LC<br />

DR-100/101<br />

DR-150/151<br />

4.00 mL<br />

10.0 mL<br />

2. Place the electrode assembly and stirrer in the solution,<br />

turn on the stirrer.<br />

3. Titrate to a pH of 4.3 with standardized 0.1 N sulfuric<br />

acid, allowing the needle of the pH scale to equilibrate<br />

as the acid is slowly added. When the region of pH 5<br />

is reached, add the titrant in 0.l0-mL increments,<br />

allowing the needle in the pH meter to equilibrate after<br />

each addition.<br />

4. Report the mL of acid required to reach a pH of 4.3.<br />

Note: This is, by definition, the total alkalinity.<br />

Always indicate the sample size when reporting the<br />

results.<br />

5. Remove the sample and rinse the electrode assembly<br />

with distilled water. If rinsing does not completely<br />

remove sample deposits, wipe the assembly with a<br />

cleansing tissue and rerinse. Replace in pH 4.01<br />

potassium acid phthalate buffer.<br />

<strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 1<br />

RVNP<br />

DR-105<br />

DR-150<br />

4.00 mL<br />

10.0 mL

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