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
Note: Avoid unnecessary exposure of the standardized sodium sulfide to air. The reagent should be standardized each week. Discard all unused reagent remaining in any open bottles at the end of each day (60 mL reagent bottles are suggested for storage of 0.06 N sodium sulfide). c. Determine the end point using concentric arcs (refer to Method ULM-0003-01, Potentiometric Titrations for Photoprocessing Solutions or any subsequent revisions.) If a microprocessor controlled titrator is used, the endpoint will be picked automatically. CALCULATIONS For Silver, g/L; g/l Ag = (mL Na2S) (N Na2S) (eq wt Ag) (1000) (mL sample) (1000) Where: mL Na 2 S = NNa 2S = eq. wt. Ag = mL sample volume of sodium sulfide in milliliters required to reach the equivalence point normality of the sodium sulfide in milliequivalents per milliliter (meq/mL) equivalent weight of silver in milligrams per milliequivalents [107.88 for Ag] 1000 = factor to convert milligrams to grams of Ag = milliliters of sample pipetted in step 1 of part A of procedure 1000 = factor to convert mLs of sample to Liters For samples containing less than 1 g/L silver: g/l Ag = (mL Na2S) (N Na2S) (107.88) (1000) (300) (1000) For samples containing 1 to 3 g/L silver: g/l Ag = (mL Na2S) (N Na2S) (107.88) (1000) (100.00) (1000) For samples containing more than 3 g/L silver: g/l Ag = (mL Na2S) (N Na2S) (107.88) (1000) (50.00) (1000) Figure 1 S-shaped Curve F002_1124GC 4 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 MiliLiters 10.00 7.50 5.00 2.50 −400 −550 −700 −850 + MiliVolts −
Determination of Sodium Metabisulfite in Process ECP-2 Accelerator Tank ECP-0025/01 INTRODUCTION The concentration of sodium metabisulfite (Na 2 S 2 O 5 ) in an ECP-2 bleach accelerator sample is determined by a manual or potentiometric titration using an iodine (I 3 -) titrant. In the method an excess of iodine is added to the sample. Sodium metabisulfite and Kodak persulfate bleach accelerator, PBA-1, present in the sample react with a portion of the iodine. The iodine that did not react with sodium metabisulfite and PBA-1 is then titrated with standardized sodium thiosulfate, using manual (starch indicator) or potentiometric endpoint detection. In order to determine the sodium metabisulfite concentration, the contribution of PBA-1 in the titration must be accounted for. This is done by subtracting a factor in the calculation of sodium metabisulfite concentration. The factor is calculated based on the PBA-1 concentration as determined by method ECP-0027-01 and it's iodimetric equivalent weight. The measured level of sodium metabisulfite in the sample may be lower than the amount added during mixing. This is due to either a reaction of PBA-1 and sodium metabisulfite that can result in a lower equilibrium concentration of sodium metabisulfite, or aerial oxidation of sodium metabisulfite. Use of this method requires handling potentially hazardous chemicals. Material Safety Data Sheets (MSDS) should be consulted for each chemical before use. These can be obtained from each chemical supplier. PRECISION AND BIAS Note: Separate statistics presented for potentiometric and visual titration methods. I. Potentiometric 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 0.8080 g/L Na2S2O5 (assay 99.04 percent). 3. A “seasoned” Accelerator tank solution analyzed as received, at 2.2536 g/L Na2S2O5 . 4. The same “seasoned” solution as in number 3, above, reanalyzed after making an analytically weighed, standard addition of 0.7036 g/L Na2S2O5 (assay 99.04 percent). Sample Na 2 S 2 O 5 Mean (g/L Na 2 S 2 O 5 ) N Repeatability Standard Deviation, 1s r (g/L Na 2 S 2 O 5 ) 95 Percent Confidence Estimate (g/L Na 2 S 2 O 5 ) “Fresh” “Fresh” plus 2.39 3 0.038 ± 0.16 Standard Addition “Seasoned”, 3.24 3 0.066 ± 0.29 As Received “Seasoned” 2.18 2 0.008 ± 0.11 plus Standard Addition 2.83 3 0.000 ± 0.00 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 106.28 percent was not statistically significantly different from 100 percent at the 95 percent confidence level. 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 93.23 percent was statistically significantly different from 100 percent at the 95 percent confidence level, but was judged not to be practically significant. Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 1
- Page 137 and 138: Titration of the Developing Agent w
- 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
- Page 153 and 154: Bias Bias is a statistically signif
- 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
- Page 161 and 162: Recovery Recovery is used instead o
- 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
- Page 169 and 170: Potentiometric Determination of Pot
- 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: APPARATUS METROHM 536 Titrator or e
- Page 191 and 192: II. Visual Endpoint Titrations A. R
- 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
- Page 205 and 206: CALCULATIONS mL AgNO 3 that would b
- 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
Note: Avoid unnecessary exposure of the standardized<br />
sodium sulfide to air. The reagent should be standardized<br />
each week. Discard all unused reagent remaining in any open<br />
bottles at the end of each day (60 mL reagent bottles are<br />
suggested for storage of 0.06 N sodium sulfide).<br />
c. Determine the end point using concentric arcs<br />
(refer to Method ULM-0003-01, Potentiometric<br />
Titrations for Photoprocessing Solutions or any<br />
subsequent revisions.) If a microprocessor<br />
controlled titrator is used, the endpoint will be<br />
picked automatically.<br />
CALCULATIONS<br />
For Silver, g/L;<br />
g/l Ag = (mL Na2S) (N Na2S) (eq wt Ag) (1000)<br />
(mL sample) (1000)<br />
Where:<br />
mL Na 2 S =<br />
NNa 2S =<br />
eq. wt. Ag =<br />
mL sample<br />
volume of sodium sulfide in milliliters required<br />
to reach the equivalence point<br />
normality of the sodium sulfide in<br />
milliequivalents per milliliter (meq/mL)<br />
equivalent weight of silver in milligrams per<br />
milliequivalents [107.88 for Ag]<br />
1000 = factor to convert milligrams to grams of Ag<br />
=<br />
milliliters of sample pipetted in step 1 of part A<br />
of procedure<br />
1000 = factor to convert mLs of sample to Liters<br />
For samples containing less than 1 g/L silver:<br />
g/l Ag = (mL Na2S) (N Na2S) (107.88) (1000)<br />
(300) (1000)<br />
For samples containing 1 to 3 g/L silver:<br />
g/l Ag = (mL Na2S) (N Na2S) (107.88) (1000)<br />
(100.00) (1000)<br />
For samples containing more than 3 g/L silver:<br />
g/l Ag = (mL Na2S) (N Na2S) (107.88) (1000)<br />
(50.00) (1000)<br />
Figure 1 S-shaped Curve<br />
F002_1124GC<br />
4 <strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03<br />
MiliLiters<br />
10.00<br />
7.50<br />
5.00<br />
2.50<br />
−400 −550 −700 −850<br />
+ MiliVolts<br />
−