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
Ferricyanide Determination 1. Add from a tip-up pipes 5 mL of 7.0 N sulfuric acid to the precipitate remaining after Step 10 of the Separation from Persulfate section above. 2. Add 6 g of potassium iodide crystals. 3. Stopper the tube and shake it until the precipitate is completely dispersed. 4. Quantitatively transfer the mixture into a 250-mL conical flask, using distilled water from a wash bottle 5. Rinse the stopper and sides of the centrifuge tube with distilled water and add the rinses to the flask. 6. Add distilled water to the 250-mL conical flask to attain an approximate volume of 125 mL. 7. Titrate with standardized 0.1 N sodium thiosulfate to a light yellow color. 8. Add 5 mL of starch indicator and continue the titration until the blue color just disappears. Any precipitate present does not interfere. Calculations Na 3Fe(CN) 6, g/L = (N Na 2S 2O 3)(mL Na 2S 2O 3)[eq wt Na 3Fe(CN) 6](1000) = (mL sample)(l000) (N Na 2 S 2 O 3 )(mL Na 2 S 2 O 3 )[280.6](1000) (5.00)(l000) 56.12(N Na 2 S 2 0 3 )(mL Na 2 S 2 O 3 ) Persulfate Determination 1. Pipet (wipe the pipet before leveling) 4.00 mL of 0.10 N ferrous ammonium sulfate into the 250-mL conical flask containing the decanted liquid from Step 10 of the Separation from Persulfate section. 2. Swirl the flask and allow it to stand for one minute. 3. Add 10 mL of 7.0 N sulfuric acid from a tip-up pipet. 4. Add four drops of Ferroin indicator to the flask. 5. Titrate with standardized 0.01 N sulfato cerate to the first blue color that persists for 15 seconds. The volume of sulfato cerate required is “B” in the calculations below. Note: If the volume of titrant required for the decanted liquid is 5 mL or less, repeat the Separation from Persulfate section and this section, pipetting 10.0 mL of 0.10 N ferrous ammonium sulfate. = 6. Once daily, determine the strength of the ferrous ammonium sulfate using approximately 20 mL of distilled water in place of the decanted liquid. Repeat Steps 1 through 5 of this section as you did with the decanted liquid. The volume of sulfato cerate required is “A” in the calculations below. Calculations Potassium Persulfate K 2 S 2 O 8 , g/L = (N sulfato cerate)(A - B)(eq wt K 2 S 2 O 8 )(1000) Ammonium Persulfate (NH 4 ) 2 S 2 O 8 , g/L = (mL sample)(l000) (N sulfato cerate)(A - B)(135)(1000) = (5.00)(l000) 27(N sulfato cerate)(A - B) (N sulfato cerate)(A - B)[eq wt (NH 4 ) 2 S 2 O 8 ](1000) (mL sample)(l000) (N sulfato cerate)(A - B)(114)(1000) = (5.00)(l000) 22.8(N sulfato cerate)(A - B) 2 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 = =
Iodometric Determination of Ferricyanide in Ferricyanide Bleach ECR-1100G Process ECN-2 ECP-2D VNF-1/LC RVNP Formulas — — SR-40 — PRINCIPLE Excess iodide ions and a zinc reagent are added to the bleach sample. The ferricyanide reacts with the iodide to produce an equivalent amount of iodine. The iodine is titrated with standard sodium thiosulfate. The reaction of ferricyanide and iodide is quantitative as long as zinc ions are present in excess. Any ferrocyanide present in the bleach, as well as the ferrocyanide produced by the reduction of ferricyanide, is precipitated as zinc ferrocyanide. Carbowax is not separated out of the sample in this method, and if present in your solution, may interfere with the iodine end point. Persulfate ions and some other oxidizing agents will also oxidize iodide. Thus, if present, they will be measured as ferricyanide by this method. This method requires handling potentially hazardous chemicals. Consult the Material Safety Data Sheet for each chemical before use. MSDS's are available from your chemical supplier. Note: Use pipets and volumetric glassware meeting the “Class A” definition by the National Institute of Standards and Technology (NIST). REAGENTS Use ACS Reagent Grade reagents unless specified otherwise. 0.60 M Potassium iodide, KI Zinc Sulfate/7.0 N Sulfuric Acid Reagent 0.1 N Sodium Thiosulfate, Na 2 S 2 O 3 (standardized to 4 decimal places) Starch Indicator PROCEDURE Removal of Interfering Constituents 1. Pipet (wipe the pipet before leveling) the indicated sample size into a 250-mL conical flask. 2. Add 25 mL of 0.60 M potassium iodide from a tip-up pipet. 3. Add 20 mL of zinc sulfate/7.0 N sulfuric acid reagent from a tip-up pipet; mix thoroughly. Titration 1. Titrate with standardized 0.1 N sodium thiosulfate to a light yellow color. 2. Add 5 mL of starch indicator from a tip-up pipes, and continue the titration until the blue color just disappears. Calculations VNF-1/LC (5-mL sample) K 3 Fe(CN) 6 , g/L = Process Sample Size VNF-1/LC 5.00 mL (N Na 2S 2O 3)(mL Na 2S 2O 3)[eq wt K 3Fe(CN) 6](1000) Na 3 Fe(CN) 6 , g/L = (mL sample)(1000) (N Na 2 S 2 O 3 )(mL Na 2 S 2 O 3 )(329.25)(1000) = (5.00)(1000) 65.85(N Na 2 S 2 0 3 )(mL Na 2 S 2 O 3 ) (N Na 2 S 2 O 3 )(mL Na 2 S 2 O 3 )[eq wt Na 3 Fe(CN) 6 ](1000) = (mL sample)(1000) (N Na 2 S 2 O 3 )(mL Na 2 S 2 O 3 )(280.92)(1000) = (5.00)(1000) 56.18(N Na 2S 20 3)(mL Na 2S 2O 3) Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 1 =
- 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 and 188: APPARATUS METROHM 536 Titrator or e
- Page 189 and 190: Determination of Sodium Metabisulfi
- 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: Titrimetric Determination of Ferric
- 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
- Page 241 and 242: APPENDIX B Effect of Temperature in
- Page 243 and 244: Potentiometric Determination of Sil
- Page 245 and 246: Potentiometric Determination of Sod
- Page 247 and 248: Iodometric Determination of Total S
- Page 249 and 250: Titrimetric Determination of Total
- Page 251 and 252: Table 2 Contribution of Constituent
- Page 253 and 254: Determination of Sulfite in KODAK R
- Page 255 and 256: CALCULATIONS Na2SO3 , g/L = (mL B -
- Page 257 and 258: Colorimetric Determination of Thioc
- Page 259 and 260: APPENDIX A Calibration of Spectroph
- Page 261 and 262: Analysis Order for Photographic Pro
- Page 263 and 264: Procedure for Electroplating a Silv
- Page 265 and 266: The Selection, Care, and Use of Vol
- Page 267 and 268: In observing the lowest point on th
Ferricyanide Determination<br />
1. Add from a tip-up pipes 5 mL of 7.0 N sulfuric acid to<br />
the precipitate remaining after Step 10 of the<br />
Separation from Persulfate section above.<br />
2. Add 6 g of potassium iodide crystals.<br />
3. Stopper the tube and shake it until the precipitate is<br />
completely dispersed.<br />
4. Quantitatively transfer the mixture into a 250-mL<br />
conical flask, using distilled water from a wash bottle<br />
5. Rinse the stopper and sides of the centrifuge tube with<br />
distilled water and add the rinses to the flask.<br />
6. Add distilled water to the 250-mL conical flask to<br />
attain an approximate volume of 125 mL.<br />
7. Titrate with standardized 0.1 N sodium thiosulfate to a<br />
light yellow color.<br />
8. Add 5 mL of starch indicator and continue the titration<br />
until the blue color just disappears. Any precipitate<br />
present does not interfere.<br />
Calculations<br />
Na 3Fe(CN) 6, g/L =<br />
(N Na 2S 2O 3)(mL Na 2S 2O 3)[eq wt Na 3Fe(CN) 6](1000) =<br />
(mL sample)(l000)<br />
(N Na 2 S 2 O 3 )(mL Na 2 S 2 O 3 )[280.6](1000)<br />
(5.00)(l000)<br />
56.12(N Na 2 S 2 0 3 )(mL Na 2 S 2 O 3 )<br />
Persulfate Determination<br />
1. Pipet (wipe the pipet before leveling) 4.00 mL of<br />
0.10 N ferrous ammonium sulfate into the 250-mL<br />
conical flask containing the decanted liquid from<br />
Step 10 of the Separation from Persulfate section.<br />
2. Swirl the flask and allow it to stand for one minute.<br />
3. Add 10 mL of 7.0 N sulfuric acid from a tip-up pipet.<br />
4. Add four drops of Ferroin indicator to the flask.<br />
5. Titrate with standardized 0.01 N sulfato cerate to the<br />
first blue color that persists for 15 seconds. The<br />
volume of sulfato cerate required is “B” in the<br />
calculations below.<br />
Note: If the volume of titrant required for the decanted<br />
liquid is 5 mL or less, repeat the Separation from<br />
Persulfate section and this section, pipetting 10.0 mL<br />
of 0.10 N ferrous ammonium sulfate.<br />
=<br />
6. Once daily, determine the strength of the ferrous<br />
ammonium sulfate using approximately 20 mL of<br />
distilled water in place of the decanted liquid. Repeat<br />
Steps 1 through 5 of this section as you did with the<br />
decanted liquid. The volume of sulfato cerate required<br />
is “A” in the calculations below.<br />
Calculations<br />
Potassium Persulfate<br />
K 2 S 2 O 8 , g/L =<br />
(N sulfato cerate)(A - B)(eq wt K 2 S 2 O 8 )(1000)<br />
Ammonium Persulfate<br />
(NH 4 ) 2 S 2 O 8 , g/L =<br />
(mL sample)(l000)<br />
(N sulfato cerate)(A - B)(135)(1000) =<br />
(5.00)(l000)<br />
27(N sulfato cerate)(A - B)<br />
(N sulfato cerate)(A - B)[eq wt (NH 4 ) 2 S 2 O 8 ](1000)<br />
(mL sample)(l000)<br />
(N sulfato cerate)(A - B)(114)(1000) =<br />
(5.00)(l000)<br />
22.8(N sulfato cerate)(A - B)<br />
2 <strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03<br />
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