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    258 views3 pages

    Karl Fischer Water Determination

    Uploaded by

    Emad Ali

    Copyright:

    © All Rights Reserved
    Download as DOC, PDF, TXT or read online from Scribd
    Flag for inappropriate content
    Download as doc, pdf, or txt
    of 3

    Karl Fischer Water Determination

    Introduction:

    Determination of the moisture content in sample substance of the most varied kinds is an important
    routine operation in many analytical laboratories, this is done by applying either a constant DC voltage
    or a constant DC current to double platinum electrode immersed in the titration mixture, and during the
    titration the current or the voltage is measured. The titrating reagents used are variations on the original
    Karl Fischer reagent of which the common feature is that they all contain the basic ingredients of
    iodine and sulphur dioxide, the background solvents may be methanol, isopropanol, pyridine,….

    Principle:

    Karl Fischer reagent consist of C5H5N + I2 + SO2 , in the presence of water, sulphur dioxide oxidized
    by the Iodine to produce sulphuric acid according to the following equation :

    SO2 + I2 + 2H2O 2HI + H2SO4

    C5H5N + I2 + SO2 + H2O C5H5 NH+I- + C5H5N + SO3-

    C5H5N + SO3- + CH3OH C5H5N.HSO4CH3

    So total equation is: I2 + SO2 + 3C5H5N + CH3OH + H2O 2C5H5N.HI + C5H5N.HSO4CH3

    The acid reaction products are buffered by the background solution, when no more water remain in the
    reaction mixture, the excess of free Iodine acts as electrode depolarizer, resulting in a sharp voltage or
    current jump , thus indicating the titration end point

    Reagent:

    Karl Fischer reagent C5H5N + I2 + SO2

    Solvent:

    Methanol CH3OH (for general used), Pyridine C5H5N, Chloroform or Trichloroethylene are used
    when the sample contain substance insoluble in methanol (these chlorinated hydrocarbons high
    electrical resistance, so they used in mixtures with methanol)

    Apparatus:

    Karl Fischer Automat, Karl Fischer processor, KF Titrino, EP/KF processor, Double Platinum
    electrode, reaction vessel

    Methods:

    Determination of Karl Fischer factor:

    It is the item for power of Karl Fischer which means number of ml Karl Fischer equivalent with
    constant weight of water, It can be determined by add about 20 ml of methanol free of water (if contain
    water titrate with Karl Fischer reagent till end point) then we add constant weight of water by micro
    syringe or by add constant weight of sodium tartrate C4H4Na2O6.2H2O which contain certain amount of
    water, and titrate against Karl Fischer reagent till the EP:

    Factor = mg of water / ml of Karl Fischer

    Sample size x factor


    Factor =
    Volume of KFR

    Standard used Sample size Factor


    Water g 1000
    Water µl 1
    methanol ml Content of methanol (g/ml)
    methanol µl 0.001 x content of methanol
    Sodium tartrate.2H2O g 156.6
    Sodium tartrate.2H2O mg 0.1566

    Determination of moisture on sample:

    Liquid Sample:
    It is measure out into titration vessel by syringe or rarely with pipette, the vessel contain solvent
    (solvent for sample) free of water, and start titration with Karl Fischer reagent till the EP

    Solid Sample:
    It should be powder as finely as possible, and then introduced into the titration vessel with a weighing
    spoon (differential weighing)

    Greases and Oil Sample:


    Are also introduced into the titration vessel by means of a syringe free from injection needle and the
    quantity of the sample is found by differential weighing

    Sample with Blank:


    Can be used blank with sample, if it is determined with an excessive solvent volume, the result can be
    converted to the amount used subsequently with the aid of the factor

    Result:

    Volume of KFR x titer (KF factor) x factor


    Water content =
    Sample size x Divisor
    Unit of Result Sample Size Factor Divisor
    % g 0.1 1
    % mg 100 1
    % ml 0.1 Density
    ppm g 1000 1
    ppm ml 1000 Density
    ppm µl 1 Density
    mg/ml g 1 Density
    mg/ml ml 1 1
    mg 1 1 1
    ml 1 1 1000

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