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
95 Percent Confidence Estimate (not including bias) The 95 percent confidence estimate (calculated using the customer standard deviation) around a single test result will include the sodium sulfite level 95 percent of the time. ECN-2 Sample Fresh 3 g/L Na2SO3 Seasoned Sample (mean = 1.66 g/L Na2SO3) ECP-2D Sample Fresh 3 g/L Na2SO3 Seasoned Sample (mean = 3.35 g/L Na2SO3 ) 95 Percent Confidence Estimate ± 0.090 g/L ± 0.090 g/L 95 Percent Confidence Estimate ± 0.098 g/L ± 0.260 g/L Bias Bias is a statistically significant deviation of the mean from the known sodium sulfite level at a 95 percent confidence level. It is determined for fresh samples only. Bias is not determined for seasoned samples, since the component concentration level cannot be determined independently of the test method. A statistically significant bias was found at all levels for the Process ECN-2 samples. A low bias of 4.1 percent, 2.4 percent, and 2.9 percent was found at the 1 g/L, 3 g/L, and 5 g/L levels, respectively. These bias were judged not to be practically significant. A low bias of 4.9 percent, 2.5 percent, and 3.6 percent was found at the 1 g/L, 3 g/L, and 5 g/L levels, respectively for the Process ECP-2D samples. These bias were judged not to be statistically or practically significant. Recovery Recovery is used instead of bias for seasoned samples, since the component concentration level cannot be determined independently of the test method. It is defined as the calculated mean for the seasoned sample with a standard addition of the component, divided by the calculated mean for the seasoned sample plus the actual amount of the standard addition. It is expressed as a percentage. The recovery of the standard addition was not statistically different from 100 percent. Apparatus All volumetric glassware should meet all “Class A” specifications, as defined by American Society for Testing and Materials (ASTM) Standards E 287, E 288, E 969, and E 1272 and all referenced documents. 10.0-, 15.0-, and 20.0-mL pipets 250-mL beakers Automatic titrator with stirrer, METROHM Potentiograph, Model E536 or equivalent ORION double-junction reference electrode 900200 or equivalent (10% KNO 3 outer filling solution) Platinum inlay electrode, BECKMAN #39373 or equivalent Reagents All chemicals are ACS Reagent Grade unless otherwise stated. 0.1 N Potassium Iodate, KIO 3 (standardized to 4 places) 0.6 M Potassium Iodide, KI 0.1 N Sodium Thiosulfate, Na2S2O3 (standardized to 4 places) 7 N Sulfuric Acid, H2SO4 Water, Type I Reagent – This method was developed, and the resulting statistical data were obtained using reagent water equivalent to purer than Type I Grade, as defined in ASTM Standard D 1193. Other grades of water, e.g., reverse osmosis (RO), demineralized, or distilled water, may give equivalent results, but the effects of water quality on method performance have not been studied. 2 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03
Procedure Treatment and Titration of the Sample 1. Pipet 20.0 mL of standardized 0.1 N potassium iodate into a 250-mL beaker containing 75 mL reagent water and a TEFLON-coated stirring bar. 2. While stirring, add 25 mL of 7.0 N sulfuric acid and 25 mL of 0.6 M potassium iodide. 3. While stirring, immediately pipet the sample size indicated below into the flask near the surface of the liquid. Rinse the sides of the beaker with reagent water. Process Sample Size ECN-2 20.0 mL ECP-2D 10.0 mL VNF-1/LC 2.00 mL RVNP 2.00 mL 4. Place the electrodes in the beaker. Note: The titrant delivery tip should be placed so that the titrant flows past the reference electrode before the platinum electrode. Calculations Na2SO3 , g/L = [(mL B x 1.33) – mL A] x (N Na2S2O3 ) x (eq. wt.) x (1000) (ml sample) x (1000) ECN-2 Na2SO3, g/L = [(mL B x 1.33) – mL A] x (N Na2S2O3 ) x (63.02) x (1000) (20) x (1000) ECP-2D Na2SO3 , g/L = [(mL B x 1.33) – mL A] x (N Na2S2O3) x (63.02) x (1000) (10) x (1000) VNF-1/RVNP Na2SO3 , g/L = [(mL B x 1.33) – mL A] x (N Na2S2O3 ) x (63.02) x (1000) (2) x (1000) Where: mL A = mL of Na2S2O3 consumed by sample mL B = mL of Na2S2O3 consumed by blank 1.33 = mL of 0.1 N potassium iodate used for sample mL of 0.1 N potassium iodate used for blank Titrate the solution potentiometrically with standardized 0.1 N sodium thiosulfate solution while stirring. Use the following parameters with a METROHM E536 Potentiograph: Rate: 15 min/100% volume Auto Control: OFF Mode: mV/pH Range: 500 mV Buret size: 20 mL Chart speed: 400 mm/100% volume 5. Determine the volume, in mL, of 0.1 N sodium thiosulfate added to reach the end point using concentric arcs (Method ULM-0003-01, Potentiometric Titrations for Photoprocessing Solutions, or subsequent revision). Record this as mL A 6. Repeat steps 1–5 pipetting 15.0 mL of standardized 0.1 N potassium iodate instead of 20.0 mL and substituting reagent water for the sample. This is the blank. Record this as mL B. Note: The blank only needs to be determined once when running a series of samples. Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3
- Page 69 and 70: Spectrophotometric Determination of
- Page 71 and 72: APPARATUS Double Beam Spectrophotom
- Page 73 and 74: APPENDIX II This appendix contains
- Page 75 and 76: Spectrophotometric Determination of
- Page 77 and 78: Calculations a. Range: 0.5-2.5 g/L
- Page 79 and 80: APPENDIX 2 Typical Absorptivity mL
- Page 81 and 82: Spectrophotometric Determination of
- Page 83 and 84: APPARATUS All volumetric glassware
- Page 85 and 86: Procedure Preparation of 10 g/L Iro
- Page 87 and 88: Determination of Total Iron in East
- Page 89 and 90: Determination of Total Iron in East
- Page 91 and 92: Determination of Total Iron in EAST
- Page 93 and 94: 12. Press ‘ZERO’. The instrumen
- Page 95 and 96: Spectrophotometric Determination of
- Page 97 and 98: PROCEDURE A. Spectrophotometer Zero
- Page 99 and 100: Absorptivity of Iron-Thiocyanate Co
- Page 101 and 102: Potentiometric Determination of Unc
- Page 103 and 104: Potentiometric Determination of Kod
- Page 105 and 106: Titrimetric Determination of Persul
- Page 107 and 108: APPARATUS Conical Flask with stoppe
- Page 109 and 110: Potentiometric Determination of Sil
- Page 111 and 112: APPARATUS METROHM 536 Titrator or e
- Page 113 and 114: Potentiometric Determination of Sod
- Page 115 and 116: PROCEDURE Treatment of the Sample 1
- Page 117 and 118: Iodometric Determination of Sodium
- Page 119: Determination of Sodium Sulfite in
- Page 123 and 124: Iodometric Determination of Sulfite
- Page 125 and 126: Potentiometric Determination of Tot
- Page 127 and 128: Automated Titration An example of a
- Page 129 and 130: Buffering Capacity Determination of
- Page 131 and 132: Buffering Capacity Determination of
- Page 133 and 134: Titrimetric Determination of EASTMA
- Page 135 and 136: VISUAL TITRATION STATISTICS Repeata
- 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
Procedure<br />
Treatment and Titration of the Sample<br />
1. Pipet 20.0 mL of standardized 0.1 N potassium iodate<br />
into a 250-mL beaker containing 75 mL reagent water<br />
and a TEFLON-coated stirring bar.<br />
2. While stirring, add 25 mL of 7.0 N sulfuric acid and<br />
25 mL of 0.6 M potassium iodide.<br />
3. While stirring, immediately pipet the sample size<br />
indicated below into the flask near the surface of the<br />
liquid. Rinse the sides of the beaker with reagent<br />
water.<br />
Process Sample Size<br />
ECN-2 20.0 mL<br />
ECP-2D 10.0 mL<br />
VNF-1/LC 2.00 mL<br />
RVNP 2.00 mL<br />
4. Place the electrodes in the beaker.<br />
Note: The titrant delivery tip should be placed so that<br />
the titrant flows past the reference electrode before the<br />
platinum electrode.<br />
Calculations<br />
Na2SO3 , g/L = [(mL B x 1.33) – mL A] x (N Na2S2O3 ) x (eq. wt.) x (1000)<br />
(ml sample) x (1000)<br />
ECN-2<br />
Na2SO3, g/L = [(mL B x 1.33) – mL A] x (N Na2S2O3 ) x (63.02) x (1000)<br />
(20) x (1000)<br />
ECP-2D<br />
Na2SO3 , g/L = [(mL B x 1.33) – mL A] x (N Na2S2O3) x (63.02) x (1000)<br />
(10) x (1000)<br />
VNF-1/RVNP<br />
Na2SO3 , g/L = [(mL B x 1.33) – mL A] x (N Na2S2O3 ) x (63.02) x (1000)<br />
(2) x (1000)<br />
Where:<br />
mL A = mL of Na2S2O3 consumed by sample<br />
mL B = mL of Na2S2O3 consumed by blank<br />
1.33 =<br />
mL of 0.1 N potassium iodate used for sample<br />
mL of 0.1 N potassium iodate used for blank<br />
Titrate the solution potentiometrically with<br />
standardized 0.1 N sodium thiosulfate solution while<br />
stirring. Use the following parameters with a<br />
METROHM E536 Potentiograph:<br />
Rate: 15 min/100% volume<br />
Auto Control: OFF<br />
Mode: mV/pH<br />
Range: 500 mV<br />
Buret size: 20 mL<br />
Chart speed: 400 mm/100% volume<br />
5. Determine the volume, in mL, of 0.1 N sodium<br />
thiosulfate added to reach the end point using<br />
concentric arcs (Method ULM-0003-01,<br />
Potentiometric Titrations for Photoprocessing<br />
Solutions, or subsequent revision). Record this as<br />
mL A<br />
6. Repeat steps 1–5 pipetting 15.0 mL of standardized<br />
0.1 N potassium iodate instead of 20.0 mL and<br />
substituting reagent water for the sample. This is the<br />
blank. Record this as mL B.<br />
Note: The blank only needs to be determined once<br />
when running a series of samples.<br />
<strong>Processing</strong> KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 3
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