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Processing kodak motion picture films, module 3 analytical procedures

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Titrimetric Determination of EASTMAN Color Developing Agent, CD-2, in Process ECP-2<br />

Developer with Sulfato Cerate<br />

ECP-0003/1<br />

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

Formulas — SD-50/51 — —<br />

INTRODUCTION<br />

This method describes an <strong>analytical</strong> procedure for measuring<br />

EASTMAN Color Developing Agent, CD-2, in Process<br />

ECP-2 Developer. CD-2 in the aqueous developer sample is<br />

extracted with an organic solvent (butyl acetate). An<br />

inorganic salt (NaCI) and a surfactant (polystyrene<br />

sulfonate) are added to minimize the formation of emulsion<br />

layers during the extraction of CD-2. In seasoned samples,<br />

an emulsion layer is usually present. If the layer does not<br />

transfer to the sulfuric acid, no significant error is<br />

introduced. The CD-2 in the solvent layer is then backextracted<br />

with sulfuric acid. This acid layer can then be<br />

titrated with sulfato cerate, using either an automatic titrator<br />

to record a potentiometric end point or manually titrated<br />

using ferroin indicator, to detect the end point visually.<br />

The potentiometric titration is recommended over the<br />

visual end point titration. However, for those unable to use<br />

instrumentation, the manual titrimetric technique, using the<br />

visual ferroin indicator, is included. Judging end points with<br />

a visual color change, especially if the samples are highly<br />

seasoned and highly colored, can differ from person to<br />

person. The potentiometric method overcomes this problem<br />

because the end point is detected potentiometrically and<br />

displayed graphically by the titrator.<br />

For the potentiometric measurement, a METROHM<br />

Potentiograph, Model E536 or equivalent should be used.<br />

The potentiometric titration requires a platinum indicator<br />

electrode and a double-junction reference electrode.<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 />

PRECISION AND BIAS<br />

Repeatability<br />

To obtain the repeatability data, a single skilled analyst<br />

performed five (5) replicates on each of the following<br />

solutions during methods development (this procedure was<br />

performed by both potentiometric and visual end point<br />

detection):<br />

a. A “fresh” EASTMAN Color Films, Process ECP-2<br />

developer prepared with all components at their<br />

respective working tank aim concentrations<br />

(2.9590 g/L CD-2).<br />

b. A “seasoned” EASTMAN Color Films, Process ECP-2<br />

developer analyzed as received at 1.0537 g/L CD-2<br />

(potentiometrically) and 1.1041 g/L CD-2 (visually).<br />

c. The same “seasoned” solution as in number b, above,<br />

reanalyzed after making an <strong>analytical</strong>ly weighed,<br />

standard addition of 1.0216 g/L CD-2 for the<br />

potentiometric study and 1.0108 g/L CD-2 for the visual<br />

study.<br />

Reproducibility<br />

Three EASTMAN Color Films, Process ECP-2 developer<br />

samples were analyzed by four analysts, each using different<br />

titration stations, on two different days. Each analyst<br />

analyzed each sample by both the potentiometric and the<br />

visual end point technique. Duplicate analyses were<br />

performed on each sample, on each of the two days. These<br />

samples were:<br />

a. A “fresh” tank solution prepared at 2.9620 g/L CD-2.<br />

b. An EASTMAN Color Films, Process ECP-2 “seasoned”<br />

tank developer sample analyzed, as received, in the<br />

same manner as the “fresh” developer. The “seasoned”<br />

sample of EASTMAN Color Films, Process ECP-2<br />

developer, analyzed to be 2.5321 g/L CD-2<br />

potentiometrically and 2.568 g/L CD-2 visually.<br />

c. The same (as in #2, above) EASTMAN Color Films,<br />

Process ECP-2 “seasoned” tank developer sample<br />

reanalyzed in the same manner as the “fresh” developer,<br />

after a standard addition of CD-2 was made. A standard<br />

addition of 0.8406 g/L CD-2 was made to that<br />

“seasoned” sample for the potentiometric and visual<br />

calibration study.<br />

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

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