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Processing kodak motion picture films, module 3 analytical procedures

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REPRODUCIBILITY<br />

Customer Standard Deviation, 1sc and<br />

95 Percent Confidence Estimate<br />

Reproducibility, or customer standard deviation, (1sc ) is an<br />

estimate of the variability a customer could expect when<br />

submitting a sample to any Photoprocessing Quality<br />

Services laboratory, where any trained analyst could test the<br />

sample using any instrument on any day.<br />

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

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

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

Three Process ECN-2 “UL” bleach samples were<br />

analyzed by four analysts, on two different days. Duplicate<br />

analyses were performed on each sample, on each of the two<br />

days. These samples were:<br />

1. Three fresh “UL” bleach samples were prepared with<br />

all components at their respective working tank aim<br />

concentrations.<br />

2. A seasoned “UL” bleach sample was analyzed<br />

potentiometrically, as received, at 39.9 g/L NH4Br. 3. The same seasoned solution, as in number 2, above,<br />

was reanalyzed after, after making a standard addition<br />

of 8.0 g/L NH4Br. Sample N Mean<br />

“Fresh” at<br />

25 g/L<br />

NH4Br “Fresh” at<br />

50 g/L<br />

NH4Br “Fresh” at<br />

75 g/L<br />

NH4Br “Seasoned”<br />

As<br />

Received<br />

“Seasoned”<br />

with<br />

Standard<br />

Addition<br />

NH 4Br<br />

Reproducibility<br />

Standard<br />

Deviation, 1s c<br />

(g/L NH 4 Br)<br />

95 Percent<br />

Confidence<br />

Estimate<br />

(g/L NH 4 Br)<br />

16 — 0.20 ± 0.43<br />

16 — 0.30 ± 0.63<br />

16 — 0.46 ± 0.98<br />

16 39.9 g/L 0.32 ± 0.69<br />

16 47.8 g/L 0.50 ± 1.07<br />

Bias<br />

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

the known ammonium bromide level at a 95 percent<br />

confidence level. It is determined for fresh samples only.<br />

Bias was not determined for this sample since the component<br />

concentration level was not determined independently of the<br />

test method.<br />

A statistically significant bias was found at all levels for<br />

the Process ECN-2 “fresh” tank bleach samples<br />

(–0.184 g/L for the 25 g/L sample, –0.326 g/L for the 50 g/L<br />

sample, and –0.415 g/L for the 75 g/L sample. However, the<br />

bias was judged not to be practically significant.<br />

Recovery<br />

Recovery is used instead of bias for seasoned samples, since<br />

the component concentration level was not determined<br />

independently of the test method. It is defined as the<br />

calculated mean for the seasoned sample with a standard<br />

addition of the component minus the mean for the seasoned<br />

sample, divided by the actual amount of the standard<br />

addition. It is expressed as a percentage.<br />

The recovery of the standard addition sample was<br />

98.8 percent and found to not be statistically different from<br />

100 percent at the 95 percent confidence level.<br />

APPARATUS<br />

All volumetric glassware should meet all Class A<br />

specifications, as defined by American Society for Testing<br />

and Materials (ASTM) Standards E 287, E 288, and E 969,<br />

unless otherwise stated.<br />

METROHM 536 Titrator or equivalent with a DOSIMAT<br />

and a 20-mL burette<br />

Indicator electrode, Silver/Sulfide Ion Selective, Orion<br />

No. 941600 or equivalent<br />

Double junction reference electrode, ORION Model<br />

900200 or equivalent<br />

Filling solutions:<br />

– ORION No. 900002 (inner chamber)<br />

– ORION No. 900003 (outer chamber)<br />

2 Pipettes, (10.0-mL)<br />

Tip-up pipette, (10-mL)<br />

Volumetric flask, (100-mL)<br />

Beaker, (250-mL)<br />

REAGENTS<br />

All reagents should be ACS Reagent Grade unless otherwise<br />

specified.<br />

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

0.05 N Silver Nitrate, AgNO3 (standardized to 4 decimal places)<br />

Water, Type I Reagent - This method was developed using<br />

reagent water equivalent to or purer than Type I grade, as<br />

defined in ASTM Standard D 1193. Other grades of<br />

water, e.g., reverse osmosis (RO), demineralized, or<br />

distilled water, may give equivalent results, but the effects<br />

of water quality on method performance have not been<br />

studied.<br />

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

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