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  • 02 KF Theory

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    liska ramdanawati
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    The document discusses Karl Fischer titration, a method for determining water content. It describes the KF reaction and summarizes two common titration methods: volumetric KF titration which uses an indicator electrode to detect the endpoint, and coulometric KF titration which generates iodine using a current and detects the endpoint potentiometrically. Key parameters for both methods are discussed, including endpoint criteria, drift as a secondary indicator, and suitable Metrohm instruments for KF titration.

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    The document discusses Karl Fischer titration, a method for determining water content. It describes the KF reaction and summarizes two common titration methods: volumetric KF titration which uses an indicator electrode to detect the endpoint, and coulometric KF titration which generates iodine using a current and detects the endpoint potentiometrically. Key parameters for both methods are discussed, including endpoint criteria, drift as a secondary indicator, and suitable Metrohm instruments for KF titration.

    Copyright:

    Attribution Non-Commercial (BY-NC)
    Download as PPT, PDF, TXT or read online from Scribd
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    Download as ppt, pdf, or txt
    81 views33 pages

    02 KF Theory

    Uploaded by

    liska ramdanawati
    The document discusses Karl Fischer titration, a method for determining water content. It describes the KF reaction and summarizes two common titration methods: volumetric KF titration which uses an indicator electrode to detect the endpoint, and coulometric KF titration which generates iodine using a current and detects the endpoint potentiometrically. Key parameters for both methods are discussed, including endpoint criteria, drift as a secondary indicator, and suitable Metrohm instruments for KF titration.

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    Download as PPT, PDF, TXT or read online from Scribd
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    of 33

    KF Titration

    Karl Fischer Titration

    Regina Schlink Metrohm Ltd, Herisau

    KF Titration
    Topics

    KF reaction Volumetric KF Titration Coulometric KF Titration Endpoint indication Drift as second endpoint indication Parameters KF Instruments

    KF Titration
    Topics

    KF reaction Volumetric KF titration Coulometric KF titration Endpoint indication Drift as second endpoint indication Parameters KF instruments

    KF Titration
    Method for water determination

    in technical products

    (oil, plastics and gases)


    in cosmetic products

    in pharmaceutical products
    in food industry
    4

    KF Titration
    The KF reaction
    I. CH3OH + SO2 + RN [RNH]SO3CH3 II. H2O + I2 + [RNH]SO3CH3 + 2RN [RNH]SO4CH3 + 2[RNH]I
    (RN = Base)

    KF Titration
    Basic ingredients of KF reagents Iodine I2

    Sulphur dioxide
    Buffer Solvent
    6

    SO2
    Imidazole

    Methanol

    KF Titration
    pH dependency
    log K

    pH

    Optimum: pH range between 5 and 7


    7

    KF Titration
    Topics

    KF reaction Volumetric KF titration Coulometric KF titration Endpoint indication Drift as second endpoint indication Parameters KF instruments

    KF Titration
    KF titration methods
    Volumetric KF titration Coulometric KF titration

    Working medium & titrant

    Iodine is generated in titration cell (anodic oxidation)


    9

    KF Titration
    Volumetric KF titration step by step

    Fill titration vessel with solvent Pretitration with KF reagent Add the sample Titrate with KF reagent

    10

    KF Titration
    Volumetric KF reagents
    One component reagents Titrant contains iodine, sulphur dioxide, buffer and methanol/ethanol Working medium contains only the methanol/ethanol Disadvantage: the titre decreases 5% per year in the closed bottle!
    Two component reagents Titrant contains iodine Solvent contains buffer and sulphur dioxide Advantages: pH optimum in the solvent / fast reaction / titre is very stable
    11

    KF Titration
    Topics

    KF reaction Volumetric KF titration Coulometric KF titration Endpoint indication Drift as second endpoint indication Parameters KF instruments

    12

    KF Titration
    Coulometric KF titration step by step
    -

    H+ II H

    current is our burette iodine is produced from a iodide containing solvent by anodic oxidation generating current is switched off as soon as a slight excess of free iodine is present free iodine is indicated by a double platinum electrode

    13

    KF Titration
    Coulometric KF titration

    Cell with diaphragm


    14

    Cell without diaphragm

    KF Titration
    How to fill coulometric cell with diaphragm?

    Catholyte 5 mL Reduction: 2 H+ +2 e- = H2
    change catholyte weekly!

    Anolyte: about 100 mL 2 I - = I2 + 2 e -

    15

    KF Titration
    Comparison with and without diaphragm
    Without diaphragm
    Recommendable for most applications, sample should have a good solubility in alcohol

    With diaphragm
    Reagents with low conductivity (the addition of chloroform or xylene > 10%), with ketone reagents absolute water content < 50 ppm

    Generator I: 400 mA

    Generator I: auto

    16

    KF Titration
    Coulometric KF reagents

    Capacity of more than 1000 mg of water (100 mL KF reagent) Anodic and cathodic reagents Combined reagents Special reagents for ketones

    17

    KF Titration
    Which is the right method for my application?

    Volumetric titration range of application 0.1 % - 100 % depends on sample size Coulometric range of application 0.001 % - 1 % (10 g - 200 mg absolute water content), mainly liquids and gases

    18

    KF Titration
    Topics

    KF reaction Volumetric KF titration Coulometric KF titration Endpoint indication Drift as second endpoint indication Parameters KF instruments

    19

    KF Titration
    Endpoint indication
    Bivoltametry Ipol = 50 uA Constant current applied to double Pt electrode

    During titration: Excess H2O High voltage between Pt wires At end of titration: Small excess of free iodine Voltage decreases sharply
    20

    KF Titration
    Endpoint indication

    21

    KF Titration
    Topics

    KF reaction Volumetric KF titration Coulometric KF titration Endpoint indication Drift as second endpoint indication Parameters KF instruments

    22

    KF Titration
    permanent consumption of KF reagent

    Drift
    Aim: Optimal: constant and low drift Volumetry <10 L/min Coulometry 2...10 g/min

    Influence on the results drift correction


    23

    KF Titration
    Drift
    -

    Start drift acceptable drift value for start of determination (cond. OK) Stop criteria drift absolute or relative drift value Absolute drift the entered value is the stop drift Relative drift the stop drift is calculated from the measured drift value (start) and the entered value

    24

    KF Titration
    Topics

    KF reaction Volumetric KF titration Coulometric KF titration Endpoint indication Drift as second endpoint indication Parameters KF instruments

    25

    KF Titration
    Titration parameter
    Volumetry
    EP at U Dynamics Stop criteria Stop drift Delay time 250 mV 100 mV drift/time 20 uL/min 10 s

    Coulometry
    EP at U Dynamics Stop criteria Stop drift Rel. Drift Start drift 50 mV 70 mV drift/rel drift 5 ug/min 5 ug/min 20 ug/min 10 uA

    I(pol):

    50 uA

    I(pol) :

    26

    KF Titration
    Topics

    KF reaction Volumetric KF titration Coulometric KF titration Endpoint indication Drift as second endpoint indication Parameters KF instruments

    27

    KF Titration
    Volumetric KF Titration

    Titrinos:
    787 KF Titrino 795 KFP Titrino

    Titrandos:

    841 Titrando PC Control / tiamo Touch Control

    28

    KF Titration
    Volumetric KF Titration
    Modi KFT
    841 Titrando

    SET Meas

    X X

    29

    KF Titration
    Only a version with dosing units ?

    Advantages: The dosing unit can be totally emptied that means:


    No crystallisation in cock and tubings Rinsing the buret several times after changing the titrant is no longer necessary

    30

    KF Titration
    Coulometric KF titration

    756 Coulometer
    with internal printer

    831 Coulometer

    31

    KF Titration
    Principle of the oven technique

    Coulometric cell

    Vial placed in the oven

    32

    KF Titration
    832 Thermoprep 774 Oven Sample Processor

    33

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