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Processing kodak motion picture films, module 3 analytical procedures

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Potentiometric Determination of Sodium Chloride in EASTMAN Color Films, Persulfate<br />

Bleach<br />

ECN-0009/1<br />

ECP-0009/1<br />

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

Formulas SR-31 SR-30 — —<br />

INTRODUCTION<br />

The chloride concentration of an Eastman Color Films,<br />

Process ECN-2 or ECP-2D persulfate bleach sample is<br />

determined by potentiometric titration with silver nitrate<br />

solution after acidification with acetic acid. See Figure 1,<br />

Chloride Titration Curve for ECN-2 Persulfate Bleach, and<br />

Figure 2, Chloride Titration Curve for ECP-2D Persulfate<br />

Bleach, for typical titration curves.<br />

This method was developed using a 50-mL burette. If a<br />

20-mL burette is utilized, the burette will refill at 20 mL,<br />

depending on sample chloride concentration. No studies<br />

have been performed to determine the impact of this<br />

substitution.<br />

Use of this method requires handling potentially<br />

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

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

your chemical supplier.<br />

PRECISION AND BIAS<br />

Repeatability Standard Deviation, 1sr & 95 Percent<br />

Confidence Estimate (not including bias)<br />

Repeatability standard deviation is an estimate of the<br />

variability one trained analyst should be able to obtain under<br />

favorable conditions (analyzing a sample, with one<br />

instrument, within one day).<br />

The 95 percent confidence estimate (calculated using the<br />

repeatability standard deviation) around a single test will<br />

include the mean value 95 percent of the time.<br />

To obtain the repeatability data, the analyst who<br />

developed this method performed five (5) replicates on each<br />

of the following solutions:<br />

1. A “fresh” persulfate bleach prepared with all<br />

components at their respective aim “working tank”<br />

concentrations:<br />

15.052 g/L NaCl for Process ECN-2<br />

15.016 g/L NaCl for Process ECP-2D<br />

2. A “seasoned” persulfate bleach analyzed, as received at:<br />

17.547 g/L NaCl for Process ECN-2<br />

23.021 g/L NaCl for Process ECP-2D<br />

3. The same “seasoned” solution as in number 2, above,<br />

reanalyzed after making a standard addition of:<br />

5.291 g/L NaCl for Process ECN-2<br />

6.943 g/L NaCl for Process ECP-2D<br />

Samples<br />

(Process<br />

ECN-2)<br />

“Fresh” at<br />

“Aim”<br />

(15.052 g/L<br />

NaCl)<br />

“Seasoned”,<br />

as received<br />

“Seasoned”<br />

with<br />

Standard<br />

Addition<br />

Samples<br />

(Process<br />

ECP-2D)<br />

“Fresh” at<br />

“Aim”<br />

(15.016 g/L<br />

NaCl)<br />

“Seasoned”,<br />

as received<br />

“Seasoned”<br />

with<br />

Standard<br />

Addition<br />

Mean<br />

(g/L NaCl)<br />

Bias<br />

Bias is a statistically significant deviation of the mean from<br />

the known mix level at a 95 percent confidence level. It is<br />

determined for “fresh” samples only. Bias is not determined<br />

for “seasoned” samples, since the component concentration<br />

level was not determined independently of the test method.<br />

A statistically significant positive bias for NaCl of<br />

(0.16 percent) was found for a Process ECN-2 “fresh”<br />

persulfate bleach tank sample. However, this bias was<br />

judged not to be practically significant.<br />

A statistically significant negative bias for NaCl of<br />

(-0.37 percent) was found for a Process ECP-2D “fresh”<br />

persulfate bleach tank sample. However, this was judged not<br />

to be practically significant.<br />

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

(N)<br />

Repeatability<br />

Standard<br />

Deviation, 1S r<br />

(g/L NaCl)<br />

95 Percent<br />

Confidence<br />

Estimate<br />

(g/L NaCl)<br />

15.076 5 0.018 ± 0.05<br />

17.547 5 0.050 ± 0.14<br />

22.815 5 0.015 ± 0.04<br />

Mean<br />

(g/L NaCl)<br />

(N)<br />

Repeatability<br />

Standard<br />

Deviation, 1S r<br />

(g/L NaCl)<br />

95 Percent<br />

Confidence<br />

Estimate<br />

(g/L NaCl)<br />

14.961 5 0.040 ± 0.11<br />

23.021 5 0.024 ± 0.07<br />

29.855 5 0.022 ± 0.06

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