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Kodak ECN-0002/1 User's Manual

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1. es sulfite were judged not to be practically significant Processing KODAK Motion Picture Films Module 3 Analytical Procedures Recovery Recovery is used instead of bias 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 table below show whether or not a recovery is statistically or practically significant from 100 percent VISUAL RECOVERY Process ECN 2 Analyte Recovery Value Statistically Significant Practically Significant Hypo Index 1 mL 73 3 Yes No Thiosulfate S2037 80 4 Yes No Sodium Sulfite NagSO3 53 4 Yes No Customer Standard Deviation 1s amp 95 Percent Confidence Estimate not including bias The customer standard deviation 1s 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
2. timer for 2 minutes of stirring 2 Titration of Sample a Into a 400 mL beaker with a magnetic stir bar pipette 40 0 mL of standardized 0 1 N potassium iodate while the timer from step 1 d is running b While stirring add 10 mL of 2 0 N acetic acid to the 400 mL beaker continue stirring through step 2e c When the timer goes off add 25 mL of 0 6 M KI to the 400 mL beaker d Immediately after the 0 6 M KI has been added add the solution in the 250 mL beaker from step 1 Sample Pretreatment to the 400 mL beaker e Rinse the 250 mL beaker three times with reagent water and add the rinses to the 400 mL beaker f Titrate the contents of the 400 mL beaker with standardized 0 1 N sodium thiosulfate on an E536 Metrohm Potentiograph or equivalent titrator If using a Metrohm E536 titrate the solution from step 2e using the parameters found in step 5 of the Hypo Index HI or Total Reductants procedure g Determine the volume of 0 1 N sodium thiosulfate at the end point using concentric arcs see Universal Method ULM 0003 01 Potentiometric Titrations for Photoprocessing Solutions or any subsequent revision Runa blank following all the steps in 1 and 2 above except omit the addition of sample in step 1b 0 1 N potassium iodate solution into a 250 mL conical flask containing a magnetic stir bar Add 10 mL of 2 0 N acetic acid solution from a tip up or equivalent pipette Stir the solutio
3. 53 mL of 0 1000 N lp consumed by 1 0 mL sample millilitres of titrant at the end point of the blank visual titration Procedure A millilitres of titrant at the end point of the sample visual titration Procedure A normality of the titrant meq mL nominal value for the normality of the titrant in meq mL B Thiosulfate S2037 mL 12 N Is eq wt S2037 1000 g L S2037 Where mL l gt N ly eq wt S2037 1000 mL Sample size 1000 millilitres of iodine titrant measured at the visual end point normality of the titrant meq mL equivalent weight of thiosulfate expressed in mg meq 112 13 factors to convert mg mL to g L C Sodium Sulfite Na S03 g L Na2S03 Where HI N lp mL Ip N Ip eq wt S2037 mL Sample 1000 HI N 12 3 mL 12 N 12 eq wt S2037 1000 mL Sample size 1000 mL of 0 1000 N I2 consumed by 1 0 mL sample nominal 0 1000 normality of iodine used in the Hypo Index calculation meq mL conversion of Hypo Index to a 3 0 mL sample size millilitres of iodine titrant measured at the visual end point Procedure B normality of the iodine titrant meq mL used in Procedure B visual end point equivalent weight of thiosulfate expressed in mg meq 112 13 sample size used in Procedure B visual end point conversion factors for milligrams to grams and milliliters to liters 10 Processing KODAK Motion Picture Films Mo
4. S Confidence Estimate Process ECN 2 Fixer mL 0 1 N l3 mL 0 1 N Ip p mL 0 1 N l5 Fresh at Aim 10 02 5 0 086 0 24 PS 15 80 5 0 073 0 20 Seasoned with Standard Addition IRE gt gt b pul 0 33 THIOSULFATE Repeatability 95 Percent a a Fixer Er N Standard Deviation 1S Confidence Estimate a g L S2037 g L S2037 Fresh at Aim 81 18 5 0 67 1 9 Seasoned As Received 125 67 5 0 47 1 3 Seasoned with Standard Addition 153 795 oS 0 60 EN SULFITE Repeatability 95 Percent aes ENS Fixer ee N Standard Deviation 1S Confidence Estimate gi Nass g L NajSO3 g L NaySO3 Fresh at Aim 17 55 5 0 69 1 9 Seasoned As Received 28 92 5 0 65 t 1 8 Seasoned with Standard Addition SO 2 Ave 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 is not determined for seasoned samples since the component concentration level was not determined independently of the test method A Statistically significant bias for thiosulfate of 1 09 percent was found for a fresh tank Process ECN 2 Fixer sample The biases for Hypo Index and Sodium Sulfite were not statistically significant However the bias for thiosulfate was judged not to be practically significant 2 Processing KODAK Motion Picture Films M
5. Titrimetric Determination of Hypo Index Thiosulfate and Sulfite in EASTMAN Color Films Process ECN 2 Fixer ECN 0002 1 Process ECN 2 ECP 2D VNF 1 LC RVNP Formulas F 34a F 34aR INTRODUCTION This method describes the titrimetric determination of hypo index total reductants thiosulfate and sulfite in EASTMAN Color Films Process ECN 2 fixers It is recommended that these determinations be carried out by a potentiometric titrimetric approach using an auto titrator However for those unable to use instrumentation the manual titrimetric technique using the visual starch indicator is included For the potentiometric measurement a Metrohm Potentiograph Model E536 or equivalent should be used The potentiometric titration requires a platinum indicator electrode and a double junction reference electrode The Hypo Index HI or total reductants of a fixer is defined as the millilitres of 0 1 N iodine consumed by the thiosulfate and sulfite combined reaction 1 amp 2 ina specified volume of fixer The fixer is added to an excess of iodine liberated from the reaction of potassium iodate and potassium iodide under acidic conditions reaction 3 The unreacted iodine is titrated either potentiometrically or visually with standardized sodium thiosulfate from the appropriate capacity burette The difference between the blank titration and the sample titration represents the milliequivalents of
6. ator to the conical flask b Titrate with standardized 0 1 N iodine solution to the first distinct blue color that persists for 15 seconds C Sulfite 1 Sulfite is a calculated value and requires no additional measurement Processing KODAK Motion Picture Films Module 3 Analytical Procedures H24 03 7 CALCULATIONS For Potentiometric Titration A Hypo Index HI or Total Reductants mL Blank A mL Sample A N Na2S203 HI 1 mL 0 1000 N Na2S203 Where HI 1 mL mL of 0 1000 N Ip consumed by 1 0 mL sample mL Blank A millilitres of titrant at the end point of the blank titration of potentiometric Procedure A mL Sample A millilitres of titrant at the end point of the sample titration of potentiometric Procedure A N Na2S203 normality of the titrant meq mL 0 1000 nominal value for the normality of the titrant in meq mL B Thiosulfate S503 mL Blank B mL Sample B N Na2S203 112 13 1000 g L S2037 oe sample size 1000 Where mL Blank B millilitres of titrant at the end point of the blank titration of potentiometric Procedure B mL Sample B millilitres of titrant at the end point of the sample titration of potentiometric Procedure B N NazS203 normality of the titrant meq mL 112 13 equivalent weight of thiosulfate expressed in mg meq 1000 conversion factor of milligrams to grams 1000 conversion factor of millilitres to litres sample size sam
7. dule 3 Analytical Procedures H24 03
8. e 400 mL beaker 4 With continued stirring immediately pipette 1 0 mL of sample near the surface of the liquid Rinse the sides of the beaker with reagent water 5 Titrate with standardized 0 1 N sodium thiosulfate on an E536 Metrohm Potentiograph or equivalent titrator If using an E536 titrate the solution from step 4 using the following parameters Rate 10 min 100 vol Auto Control OFF Mode mV pH Range 500 mV Burette Size 50 mL Indicator Electrode Platinum inlay or platinum wire i e Beckman Model 39273 Reference Electrode Double junction reference i e Orion Model 90 02 6 Determine the volume of 0 1 N sodium thiosulfate at the end point using concentric arcs see Universal Method ULM 0003 01 Potentiometric Titrations for Photoprocessing Solutions or subsequent revision 7 Runa blank do steps 1 6 but omit the addition of the sample in step 4 6 Processing KODAK Motion Picture Films Module 3 Analytical Procedures H24 03 B Thiosulfate Determination For Visual Titration 1 Sample Pretreatment A Hypo Index HI or Total Reductants Treatment and Titration of Sample 1 Pipette wipe before leveling 40 0 mL of standardized a To a250 mL beaker with a magnetic stir bar add 75 mL of reagent water b Pipette 2 0 mL of sample into the 250 mL beaker c Add5 mL of 6 formaldehyde pH 3 9 to the beaker d Start stirring the contents of the 250 mL beaker set and start a
9. iodine consumed by the sample Dividing the milliequivalents of iodine by 0 1 meq mL yields the HI of the sample Hypo index is reported in the terms of HI 1 mL which is the millilitres of 0 1000 N I consumed by 1 0 mL of sample 2 S2037 l gt 21 S4067 reaction 1 HSO3 lo H2O gt SO 21 3H reaction 2 103 51 6H gt 3lp 3H2O reaction 3 NapSO3 HCHO H2O gt CH3 OH SO3Na NaOH reaction 4 The thiosulfate is determined potentiometrically by adding 6 percent formaldehyde to a second sample aliquot in reagent water Under these conditions the sulfite in the sample forms a formaldehyde bisulfite complex reaction 4 This sample is then added to an excess of acidified iodine The unreacted iodine is titrated either potentiometrically with standardized sodium thiosulfate from a 50 mL capacity burette The difference between the blank titration and the sample titration represents the milliequivalents of iodine consumed by the thiosulfate in the sample The thiosulfate is expressed as g L thiosulfate ion S2037 The thiosulfate is determined by the visual titration by adjusting the pH of a sample aliquot to 8 5 At this pH the sulfite rapidly forms the stable sulfite formaldehyde adduct Upon acidification which prevents the adduct from reacting with iodine the thiosulfate from the sample is titrated with standardized iodine reagent to a starch end point The sulfite content is calculated by subtracting
10. n with a magnetic stirrer and add 25 mL of 0 6 M potassium iodide solution from a tip up pipette Immediately pipette wipe 1 0 mL of the fixer sample into the 250 mL flask while the solution is stirring hold the tip of the pipette against the wall of the flask and as close to the surface of the stirring solution as possible while the sample is draining but do not immerse the tip of the pipette in the stirring solution Titrate with standardized 0 1 N sodium thiosulfate solution to a light yellow color Add 5 mL of the starch indicator from a tip up pipette and continue the titration until the blue color just disappears for 15 seconds Runa blank do steps 1 6 but omit the addition of the sample in step 4 B Thiosulfate Hypo 1 Treatment of the Sample a Pipette 2 0 mL of the fixer sample into a 250 mL conical flask containing a magnetic stir bar b Add 5 mL of formalin from a tip up pipette c Add 3 or 4 drops of phenolphthalein indicator to the flask e Ifthe solution is pink titrate with 1 0 N sulfuric acid to colorless e Ifthe solution is colorless titrate with 1 0 N sodium hydroxide to the first light pink color d Let the solution stand for 2 minutes e Add 10 mL of 2 0 N acetic acid from a tip up pipette 2 Titration with Iodine C Sulfite 1 Sulfite is a calculated value and requires no additional measurement a Add from a tip up pipette 5 mL of the starch indic
11. odule 3 Analytical Procedures H24 03 Recovery Recovery is used instead of bias 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 table below shows whether or not a recovery is statistically or practically different from 100 percent POTENTIOMETRIC RECOVERY Process ECN 2 Analyte Recovery Value Statistically Significant Practically Significant Hypo Index 1 mL 76 Yes No Thiosulfate S2037 74 Yes No Sodium Sulfite NazSO3 80 4 No No Reliability Customer Standard Deviation 1s amp 95 Percent Confidence Estimate not including bias The customer standard deviation 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 HYPO INDEX Reproducibility 95 Percent parte Sie aig 5 ni N Standard Deviation 1S C
12. onfidence Estimate we mL 0 1 N Ip mL 0 1 N l5 Fresh at Aim 12 88 16 0 25 0 54 Seasoned As fs Received 12 73 16 0 13 0 27 Seasoned with Standard Addition 13 83 e oe 503 THIOSULFATE Reproducibility 95 Percent ipa sre er T Else N Standard Deviation 1S Confidence Estimate ie g L S2037 g L S2037 Fresh at Aim 108 14 16 0 94 2 00 Seasoned As Received 114 86 16 0 73 1 56 Seasoned with Standard Addition ae re 0 7 ENRI SULFITE Na S03 Reproducibility 95 Percent N T Neco N Standard Deviation 1S Confidence Estimate git NA293 g L NajSO3 g L NajSO3 Fresh at Aim 20 79 15 0 59 1 26 Seasoned As Received 15 70 16 0 68 1 45 Seasoned with Standard Addition Pe We 0 76 eee Processing KODAK Motion Picture Films Module 3 Analytical Procedures VISUAL TITRATION STATISTICS Repeatability Standard Deviation 1s and 95 Percent Confidence Estimate 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 HYPO INDEX 3 0 mL Repeatability Standard 95 Percent aH a rex i he N Deviation 1S Confidence Estimate EON i2 mL 0 1 N Ip mL 0 1 N Ip Fresh a
13. ple size used in potentiometric Procedure B 2 0 mL C Sodium Sulfite NagSO3 mL Blank A mL Sample A DmLA mL Blank B mL Sample B DmLB D mL A 2 0 D mL B N NagS203 63 02 1000 g L NapSO3 sample size 1000 Where N NasS203 normality of the titrant 2 0 conversion of hypo index to 2 0 mL sample size 63 02 equivalent weight of sodium sulfite in mg meq 1000 conversion factor of milligrams to grams sample size sample size used in potentiometric Procedure B 2 0 mL 1000 conversion factor of millilitres to litres 8 Processing KODAK Motion Picture Films Module 3 Analytical Procedures H24 03 Example Potentiometric Calculations Titration mL 0 1 N NagSoO3 Titrant BlankA 40 50 SampleA 21 85 BlankB 40 55 Sample B 19 80 Hypo Index HI or Total Reductants 40 50 21 85 0 0989 0 1000 HI 1 mL 18 4mL0 1000N Ip Thiosulfate S2037 40 55 19 80 0 0989 112 13 1000 g L SO Pe 2 0 1000 57 5g L Sodium Sulfite NazSO 3 40 50 21 85 2 0 40 55 19 80 0 0989 63 02 1000 g L NapSO ae 2 0 1000 51 4g L Processing KODAK Motion Picture Films Module 3 Analytical Procedures H24 03 For Visual Titration A Hypo Index HI or Total Reductants HI 1 mL mL Blank A mL Sample A N Na2S203 Where HI 1 mL mL Blank A mL Sample A N Na2S203 0 1000 0 1000 N Na2S20
14. r equivalent Double junction i e Orion Reference electrode 900200 or equivalent 10 KNO outer filling solution For Visual Titration e Burette Class A 50 mL capacity Teflon stopcock e Magnetic Stirrer REAGENTS Use ACS Reagent Grade reagents unless otherwise specified e Potassium Iodate KIO 0 1 N standardized to four decimal places e Acetic Acid CH COOH 2 0 N Potassium Iodide KI 0 6 M e Sodium Thiosulfate NayS 03 0 1 N standardized to four decimal places Formaldehyde 6 pH 3 9 e Starch Indicator Phenolphthalein Indicator e Sodium Hydroxide NaOH 1 0 N Sulfuric Acid HSO 1 0 N Iodine I 0 1 N standardized to four decimal places e Water Type I Reagent This method was developed and the resulting statistical data were obtained using reagent water equivalent to or 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 PROCEDURE For Potentiometric Titration A eS Index HI or Total Reductants To a400 mL beaker with a magnetic stir bar add 100 mL reagent water 2 Pipette 40 0 mL use a 20 mL pipette twice of standardized 0 1 N potassium iodate into the 400 mL beaker 3 While stirring add 10 mL of 2 0 N acetic acid and 25 mL of 0 6 M potassium iodide KI to th
15. repared at 109 212 g L thiosulfate ion and 21 335 g L sodium sulfite b an EASTMAN Color Films Process ECN 2 seasoned tank fixer sample analyzed as received in the same manner as the fresh fixer c the same as in number b above EASTMAN Color Films Process ECN 2 seasoned tank fixer sample reanalyzed in the same manner as the fresh fixer after standard additions of thiosulfate and sulfite were made The seasoned sample of EASTMAN Color Films Process ECN 2 fixer analyzed to be 115 17 g L thiosulfate ion and 15 69 g L sodium sulfite Standard Processing KODAK Motion Picture Films Module 3 Analytical Procedures H24 03 additions of 34 57 g L thiosulfate ion and 5 444 g L sodium sulfite were made to that seasoned sample POTENTIOMETRIC TITRATION STATISTICS Repeatability Standard Deviation 1s amp 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 will include the mean value 95 percent of the time HYPO INDEX 1 mL Repeatability 95 Percent Samples Mean Level PARE j OF N Standard Deviation 1
16. t Aim 29 42 5 0 089 0 25 Seasoned As Received 47 29 5 0 060 0 17 Seasoned with 3 Standard Addition 5 89 3 0 084 20 23 THIOSULFATE S2037 Repeatability Standard 95 Percent pat ed oa pia ea N Deviation 1S Confidence Estimate a g L S2037 g L S2037 Fresh at Aim 81 37 5 0 10 0 28 Seasoned As Received 125 29 5 0 24 0 67 Seasoned with pa Standard Addition 19949 I9 0 13 O98 SULFITE Na2SO3 Repeatability Standard 95 Percent mr sae Hea anes N Deviation 1S Confidence Estimate gi Na2903 g L NajSO3 g L NajSO3 Fresh at Aim 16 08 5 0 18 0 50 Seasoned As ef Received 28 93 5 0 24 0 67 Seasoned with x Standard Addition een le oe p 86 Bias Bias is a statistically significant deviation of the mean from Bi i ias ias the known mig level at a 95 percent confidence level It is Analyte Measurement Unit of Analyte determined for fresh samples only Bias is not determined for seasoned samples since the component concentration vids pete 0 82 271 level was not determined independently of the test method mi0 2 Statistically significant biases were found for hypo index Thiosulfate 0 696 0 85 i L S2037 pis thiosulfate and sodium sulfite see the table below for a g L S203 fresh tank Process ECN 2 Fixer sample However the Sodium Sulfite ee a individual biases for hypo index thiosulfate or sodium NaSO3 i
17. the milliequivalents of iodine consumed by the thiosulfate from the milliequivalents of iodine consumed by the thiosulfate and sulfite The sulfite is reported as sodium sulfite Use of 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 PRECISION AND BIAS Repeatability To obtain the repeatability data a single skilled analyst performed five 5 replicates on each of the following solutions this procedure was done by both potentiometric and visual end point detection a A fresh EASTMAN Color Films Process ECN 2 Fixer prepared with all components at their respective aim concentrations in a working tank b A seasoned EASTMAN Color Films Process ECN 2 Fixer analyzed as received at 125 67 g L thiosulfate ion and 28 92 g L sodium sulfite c The same seasoned solution as in number b above reanalyzed after making standard additions of 37 850 g L thiosulfate ion and 8 415 g L sodium sulfite Reproducibility Three EASTMAN Color Films Process ECN 2 Fixer samples were analyzed by four analysts each using different titration stations on two different days Each analyst analyzed each sample by both the potentiometric and the visual end point technique Duplicate analyses were performed on each sample on each of the two days These samples were a a fresh tank solution p
18. the time HYPO INDEX 1 0 mL Reproducibility 95 Percent Seer E aie F NE N Standard Deviation 1S Confidence Estimate ee mL 0 1 N Ip mL 0 1 N Ip Fresh at Aim 12 97 16 0 18 0 39 Seasoned As Received 12 70 16 0 15 0 31 Seasoned with Standard Addition sce eee met ae THIOSULFATE S303 Reproducibility 95 Percent R Huy Gees N Standard Deviation 1S Confidence Estimate ae g L S2037 g L S2037 Fresh at Aim 107 95 16 0 93 1 99 Seasoned As Received 114 95 16 0 97 2 06 Seasoned with Standard Addition eee ele LOZ eee SULFITE NajSO3 Reproducibility 95 Percent PENS a NESC N Standard Deviation 1S Confidence Estimate gi NA293 g L NajSO3 g L NaySO3 Fresh at Aim 21 17 16 1 18 2 52 Seasoned As Received 15 46 16 1 14 2 43 Seasoned with Standard Addition eee ite pee aes Processing KODAK Motion Picture Films Module 3 Analytical Procedures 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 and E 969 unless otherwise stated For Potentiometric Titration e Metrohm Potentiograph Model E536 or equivalent titrator Metrohm Model 665 Dosimat with a 50 mL burette size no substitution Electrodes Platinum inlay i e Beckman Indicator electrode Model 39273 o

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