Processing kodak motion picture films, module 3 analytical procedures

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Figure 1 pH 11.4 High Control @ 25°C 11.460 11.455 11.450 UCLx 11.445 11.440 11.435 x 11.430 11.425 11.420 LCLx 11.415 0.020 0.015 0.010 0.005 0.000 UCLr r LCLr Individuals Ranges UCLx 11.4504 UCLr 0.0172 X bar 11.4363 r bar 0.0053 LCLx 11.4223 LCLr 0.0000 Units: pH Historical Limits: n = 19 Chart of Averages 1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31 33 35 37 39 Range Chart F002_0941HC 12 Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03
Potentiometric Titrations for Photoprocessing Solutions ULM-0003-01 INTRODUCTION Titrations involve the addition of accurately known volumes of standardized titrant to a solution containing the sample. The concentration of the analyte(s) being determined by titration can be calculated based on the volume of titrant used to reach the endpoint (also referred to as the equivalence point or break) of the titration. The titration endpoint can be determined manually or potentiometrically. In a manual titration the endpoint is determined by use of a visual indicator that changes color when the endpoint of the titration has been reached. In a potentiometric titration the endpoint is determined by use of a pair of electrodes or a combination electrode. The endpoint occurs where there is a maximal rate of change of potential at the endpoint of the titration. In the portion of the curve corresponding to this large change in potential, there is a point at which the curve changes its direction of curvature. This point is an inflection point or break in the curve and ideally it occurs at the equivalence point of the titration. However, in certain cases, there may be a bias in the analysis, and the break may be slightly displaced from the true equivalence point. The analysis of known samples may indicate that the bias is large enough to require a correction. The electrode pair for potentiometric titrations includes an indicator and reference electrode. The combination electrode contains the indicator and reference electrode configured in a single electrode. The electrodes for potentiometric titrations are chosen so that a change in potential of the titration solution, caused by titration of the analyte(s) of interest, is optimally detected. Potentiometric titrations are preferred to manual titrations, since they are more accurate and precise. They are also more easily adapted to automation, where automated titration systems can process larger volumes of samples with minimal analyst involvement. Use of this method requires handling of potentially hazardous chemicals. Material Safety Data Sheets should be consulted for each chemical before use. These can be obtained from the chemical's supplier. TYPES OF TITRATIONS Types of potentiometric titrations for the determination of analytes in photoprocessing solutions include acid-base (total alkalinity and total acidity), redox (HI/HY and cerate), precipitation (halides), and complexometric (free EDTA and Antical #5). The specific titrimetric method, including which electrode(s) to use, can be found in individual analytical methods for each photographic process. Since silver halide titrations are not explained in more detail in most methods, they will be discussed here. An Orion double junction electrode with an outer filling solution of potassium nitrate is used as the reference electrode for titrations of halides with silver nitrate. A silver electrode is used as the indicating electrode for halide titrations, because its potential is a function of the silver ion concentration in the titration solution. The potential between the electrodes is measured and recorded manually when a potentiometer or a pH meter is used; this is done automatically when an automatic titrator is used. These potential measurements are read on a millivolt scale. Difficulties may occur when more than one halide is present in a solution. One of the difficulties in titrations with silver nitrate is in knowing which particular halide caused the inflection point on the curve. Where iodide, bromide and chloride are present the first break should be that of the iodide, because it has the lowest solubility. However, if little or no iodide is present in the sample, the first break will be that of the bromide, followed by a break for chloride. See Figure 1, Typical Bromide Titration Curve. When little chloride is present, the bromide and chloride in the sample may co-precipitate. If so, one break may easily be confused with the other. This situation is avoided in several bromide methods by the addition of more chloride to the sample before titration, to pull the chloride break away from the bromide break. Figure 1 Typical Bromide Titration Curve mL titrant (0.0500 N AgNO 3 ) Chloride Break (Sodium Chloride Added) TITRANT PREPARATION AND STANDARDIZATION Titrant preparation and standardization methods can be found in Processing KODAK Motion Picture Films, Module 4, Reagent Preparation Procedures. Processing KODAK Motion Picture Films, Module 3, Analytical Procedures H24.03 1 pH Scale F002_0987AC Iodide Break Chloride Break (No Sodium Chloride Added) Bromide Break
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©Eastman Kodak Company, 1999 Proce
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ECP-2-1101 Ferrocyanide in Ferricya
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3 Analytical Procedures for Chemica
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Spectrophotometric Determination of
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Potentiometric Determination of Bro
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PROCEDURE B For Seasoned Tank and R
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APPARATUS All volumetric glassware
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APPARATUS All pipettes and volumetr
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Potentiometric Determination of Amm
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PROCEDURE A. Sample Treatment 1. Pi
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Titrimetric Determination of Buffer
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Buffering Capacity Determination of
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Titrimetric Determination of EASTMA
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VISUAL TITRATION STATISTICS Repeata
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Back-Extraction of the Developing A
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Potentiometric Determination of Fer
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Recovery Recovery is used instead o
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CALCULATIONS For Na3Fe(CN) 6 g/L Na
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Cerimetric Determination of Sodium
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Bias Bias is a statistically signif
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APPARATUS Pipet (40-mL) Graduated C
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B. Analysis of Standards 1. Run eac
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Determination of Ferrous Iron in EA
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PROCEDURE Blank 1. Set a double-bea
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APPENDIX B This appendix contains t
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Titrimetric Determination of Hypo I
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B. Thiosulfate Determination 1. Sam
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Example Potentiometric Calculations
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APPARATUS Double Beam Spectrophotom
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APPENDIX II This appendix contains
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Calculations a. Range: 0.5-2.5 g/L
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APPENDIX 2 Typical Absorptivity mL
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Procedure Preparation of 10 g/L Iro
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Determination of Total Iron in East
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Determination of Total Iron in East
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Determination of Total Iron in EAST
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12. Press ‘ZERO’. The instrumen
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PROCEDURE A. Spectrophotometer Zero
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Absorptivity of Iron-Thiocyanate Co
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Potentiometric Determination of Unc
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Potentiometric Determination of Kod
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Titrimetric Determination of Persul
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APPARATUS Conical Flask with stoppe
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Potentiometric Determination of Sil
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APPARATUS METROHM 536 Titrator or e
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Potentiometric Determination of Sod
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PROCEDURE Treatment of the Sample 1
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Iodometric Determination of Sodium
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Determination of Sodium Sulfite in
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Procedure Treatment and Titration o
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Iodometric Determination of Sulfite
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Potentiometric Determination of Tot
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Automated Titration An example of a
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Titrimetric Determination of EASTMA
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VISUAL TITRATION STATISTICS Repeata
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Titration of the Developing Agent w
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Cerimetric Determination of CD-2 Co
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Cerimetric Determination of KODAK C
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Back-Extraction of CD-2 1. Add 50 m
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CALCULATIONS For Na3Fe(CN) 6 g/L Na
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Bias Bias is a statistically signif
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Hydroquinone in Sound Track Develop
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B. Thiosulfate Determination 1. Sam
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Examples: Titration mL 0.1 N Na 2S
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Potentiometric Determination of Pot
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PROCEDURE A. Preparation of Sample
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Titrimetric Determination of Persul
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APPARATUS Conical Flask with stoppe
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Determination of the pH of the East
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Determination of the pH of Processe
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Potentiometric Determination of Sil
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Determination of Sodium Metabisulfi
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II. Visual Endpoint Titrations A. R
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Viscosity Determination of Sound-Tr
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Titrimetric Determination Of Benzyl
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PROCEDURE B For Seasoned Tank Note:
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CALCULATIONS mL AgNO 3 that would b
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Titrimetric Determination of Buffer
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Titrimetric Determination of Citraz
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Potentiometric Determination of Eth
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Titrimetric Determination of Ferric
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Iodometric Determination of Ferricy
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Iodometric Determination of Formali
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Potentiometric Determination of Iod
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Potentiometric Determination of Pot
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Titration Note: For preparation of
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