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
B. REPRODUCIBILITY Customer Standard Deviation, 1sc & 95 Percent Confidence Estimate (not including bias) Reproducibility or customer standard deviation (1sc ) is an estimate of the variability a customer could expect when submitting a sample to any Photoprocessing Quality Services laboratory, where any trained analyst could test the sample using any instrument on any day. The 95 percent confidence estimate (calculated using the customer standard deviation) around a single test result will include the mean value 95 percent of the time. Four analysts analyzed four Accelerator tank samples, on two different days. Duplicate analyses were performed on each sample, on each of the two days. These samples were: 1. A “fresh” Accelerator tank solution prepared with all components at their respective “working tank” aim concentrations. 2. The same “fresh” solution as in number 1, above, reanalyzed in the same manner, after making a standard addition of 1.2038 g/L Na2S2O5 (assay 99.04 percent). 3. A “seasoned” Accelerator tank solution analyzed as received as 2.2705 g/L Na2S2O5. 4. The same “seasoned” solution, as in number 3, above, analyzed in the same manner, after making a standard addition of 1.0296 g/L Na2S2O5 (assay 99.04 percent). Sample Mean (g/L Na 2S 2O 5) N Na 2 S 2 O 5 Reproducibility Standard Deviation, 1s c (g/L Na 2 S 2 O 5 ) 95 Percent Confidence Estimate (g/L Na 2 S 2 O 5 ) “Fresh” “Fresh” plus 2.10 16 0.115 ± 0.24 Standard Addition “Seasoned”, 3.17 16 0.087 ± 0.19 As Received “Seasoned” 2.27 16 0.111 ± 0.24 plus Standard Addition 3.30 15 0.128 ± 0.27 Bias Bias is a statistically significant deviation of the mean from the known mix level at a 95 percent confidence level. It is determined for fresh samples only. Bias was not determined for this sample because the component concentration level was not determined independently of the test method. An equilibrium is established between sodium metabisulfite and PBA-1 that effectively lowers the concentration of sodium metabisulfite in freshly mixed solutions. Therefore bias is estimated for fresh solutions by spiking a known amount of sodium metabisulfite to a fresh mix that has been allowed to sit overnight, and the recovery is then calculated. The recovery of 88.59 percent was statistically significantly different from 100 percent at the 95 percent confidence level, but was judged not to be practically significant. Recovery Recovery is used for seasoned samples, since the component concentration level was not determined independently of the test method. It is defined as the calculated mean for the seasoned sample with a standard addition of the component minus the mean for the seasoned sample, divided by the actual amount of the standard addition. It is expressed as a percentage. The recovery of 100.05 percent was not statistically significantly different from 100 percent at the 95 percent confidence level. 2 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03
II. Visual Endpoint Titrations A. Repeatability Standard Deviation, 1sr and 95 Percent Confidence Estimate (not including Bias) Repeatability standard deviation is an estimate of the variability one trained analyst should be able to obtain under favorable conditions (analyzing a sample, with one instrument, within one day). The 95 percent confidence estimate (calculated using the repeatability standard deviation) around a single test result will include the mean value 95 percent of the time. To obtain the repeatability data, a single skilled analyst performed three (3) replicates on each of the following solutions during methods development. 1. A “fresh” Accelerator tank solution prepared with all components at their respective “working tank” aim concentrations. 2. The same “fresh” solution as in number 1, above, reanalyzed after making an analytically weighed, standard addition of 0.6552 g/L Na2S2O5 (assay 99.04 percent). 3. A “seasoned” Accelerator tank solution analyzed as received, at 1.9093 g/L Na2S2O5. 4. The same “seasoned” solution as in number 3, above, reanalyzed after making an analytically weighed, standard addition of 0.6106 g/L Na2S2O5 (assay 99.04 percent). Sample Na 2 S 2 O 5 Mean (g/L Na 2S 2O 5) N Repeatability Standard Deviation, 1s r (g/L Na 2S 2O 5) 95 Percent Confidence Estimate (g/L Na 2S 2O 5) “Fresh” “Fresh” plus 2.08 5 0.018 ± 0.05 Standard Addition “Seasoned”, 2.69 5 0.024 ± 0.07 As Received “Seasoned” 1.91 3 0.017 ± 0.07 plus Standard Addition 2.53 3 0.010 ± 0.04 Bias Bias is a statistically significant deviation of the mean from the known mix level at a 95 percent confidence level. It is determined for fresh samples only. Bias was not determined for this sample because the component concentration level was not determined independently of the test method. An equilibrium is established between sodium metabisulfite and PBA-1 that effectively lowers the concentration of sodium metabisulfite in freshly mixed solutions. Therefore bias is estimated for fresh solutions by spiking a known amount of sodium metabisulfite to a fresh mix that has been allowed to sit overnight, and the recovery is then calculated. The recovery of 94.57 percent was statistically significantly different from 100 percent at the 95 percent confidence level, but was judged not to be practically significant. Recovery Recovery is used for seasoned samples, since the component concentration level was not determined independently of the test method. It is defined as the calculated mean for the seasoned sample with a standard addition of the component minus the mean for the seasoned sample, divided by the actual amount of the standard addition. It is expressed as a percentage. The recovery of 101.86 percent was not statistically significantly different from 100 percent at the 95 percent confidence level. Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3
- Page 139 and 140: Cerimetric Determination of CD-2 Co
- Page 141 and 142: Cerimetric Determination of KODAK C
- Page 143 and 144: Back-Extraction of CD-2 1. Add 50 m
- Page 145 and 146: Potentiometric Determination of Fer
- Page 147 and 148: Recovery Recovery is used instead o
- Page 149 and 150: CALCULATIONS For Na3Fe(CN) 6 g/L Na
- Page 151 and 152: Potentiometric Determination of Fer
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- Page 155 and 156: Spectrophotometric Determination of
- Page 157 and 158: Hydroquinone in Sound Track Develop
- Page 159 and 160: Titrimetric Determination of Hypo I
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- Page 163 and 164: Recovery Recovery is used instead o
- Page 165 and 166: B. Thiosulfate Determination 1. Sam
- Page 167 and 168: Examples: Titration mL 0.1 N Na 2S
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- Page 171 and 172: APPARATUS All volumetric glassware
- Page 173 and 174: Potentiometric Determination of Kod
- Page 175 and 176: PROCEDURE A. Preparation of Sample
- Page 177 and 178: Titrimetric Determination of Persul
- Page 179 and 180: APPARATUS Conical Flask with stoppe
- Page 181 and 182: Determination of the pH of the East
- Page 183 and 184: Determination of the pH of Processe
- Page 185 and 186: Potentiometric Determination of Sil
- Page 187 and 188: APPARATUS METROHM 536 Titrator or e
- Page 189: Determination of Sodium Metabisulfi
- Page 193 and 194: APPARATUS METROHM 536 Titrator or e
- Page 195 and 196: Viscosity Determination of Sound-Tr
- Page 197 and 198: Titrimetric Determination Of Benzyl
- Page 199 and 200: Potentiometric Determination of Bro
- Page 201 and 202: PROCEDURE B For Seasoned Tank Note:
- Page 203 and 204: Potentiometric Determination of Bro
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- Page 207 and 208: Titrimetric Determination of Buffer
- Page 209 and 210: Potentiometric Determination of Kod
- Page 211 and 212: Spectrophotometric Determination of
- Page 213 and 214: Titrimetric Determination of Citraz
- Page 215 and 216: Potentiometric Determination of Eth
- Page 217 and 218: Titrimetric Determination of Ferric
- Page 219 and 220: Iodometric Determination of Ferricy
- Page 221 and 222: Potentiometric Determination of Fer
- Page 223 and 224: Iodometric Determination of Formali
- Page 225 and 226: Spectrophotometric Determination of
- Page 227 and 228: Titrimetric Determination of Hypo I
- Page 229 and 230: Potentiometric Determination of Iod
- Page 231 and 232: Potentiometric Determination of Pot
- Page 233 and 234: Titration Note: For preparation of
- Page 235 and 236: Titrimetric Determination of Persul
- Page 237 and 238: Spectrophotometric Determination of
- Page 239 and 240: APPARATUS Spectrophotometer with a
II. Visual Endpoint Titrations<br />
A. Repeatability Standard Deviation, 1sr and<br />
95 Percent 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 result<br />
will include the mean value 95 percent of the time.<br />
To obtain the repeatability data, a single skilled analyst<br />
performed three (3) replicates on each of the following<br />
solutions during methods development.<br />
1. A “fresh” Accelerator tank solution prepared with all<br />
components at their respective “working tank” aim<br />
concentrations.<br />
2. The same “fresh” solution as in number 1, above,<br />
reanalyzed after making an <strong>analytical</strong>ly weighed,<br />
standard addition of 0.6552 g/L Na2S2O5 (assay<br />
99.04 percent).<br />
3. A “seasoned” Accelerator tank solution analyzed as<br />
received, at 1.9093 g/L Na2S2O5. 4. The same “seasoned” solution as in number 3, above,<br />
reanalyzed after making an <strong>analytical</strong>ly weighed,<br />
standard addition of 0.6106 g/L Na2S2O5 (assay<br />
99.04 percent).<br />
Sample<br />
Na 2 S 2 O 5<br />
Mean<br />
(g/L Na 2S 2O 5) N<br />
Repeatability<br />
Standard<br />
Deviation, 1s r<br />
(g/L Na 2S 2O 5)<br />
95 Percent<br />
Confidence<br />
Estimate<br />
(g/L Na 2S 2O 5)<br />
“Fresh”<br />
“Fresh” plus<br />
2.08 5 0.018 ± 0.05<br />
Standard<br />
Addition<br />
“Seasoned”,<br />
2.69 5 0.024 ± 0.07<br />
As<br />
Received<br />
“Seasoned”<br />
1.91 3 0.017 ± 0.07<br />
plus<br />
Standard<br />
Addition<br />
2.53 3 0.010 ± 0.04<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 was not determined<br />
for this sample because the component concentration level<br />
was not determined independently of the test method. An<br />
equilibrium is established between sodium metabisulfite and<br />
PBA-1 that effectively lowers the concentration of sodium<br />
metabisulfite in freshly mixed solutions. Therefore bias is<br />
estimated for fresh solutions by spiking a known amount of<br />
sodium metabisulfite to a fresh mix that has been allowed to<br />
sit overnight, and the recovery is then calculated.<br />
The recovery of 94.57 percent was statistically<br />
significantly different from 100 percent at the 95 percent<br />
confidence level, but was judged not to be practically<br />
significant.<br />
Recovery<br />
Recovery is used for seasoned samples, since the component<br />
concentration level was not determined independently of the<br />
test method. It is defined as the calculated mean for the<br />
seasoned sample with a standard addition of the component<br />
minus the mean for the seasoned sample, divided by the<br />
actual amount of the standard addition. It is expressed as a<br />
percentage.<br />
The recovery of 101.86 percent was not statistically<br />
significantly different from 100 percent at the 95 percent<br />
confidence level.<br />
<strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3