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    Home > Chemicals Industry > Chemical Technology > Determination of cyanide ion in solid waste by ion chromatography (2)

    Determination of cyanide ion in solid waste by ion chromatography (2)

    • Last Update: 2022-02-26
    • Source: Internet
    • Author: User
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    Six, analysis and testing

    (1) Instrument conditions

    Eluent: 100mmol/L sodium hydroxide solution-250mmol/L sodium acetate solution


    Flow rate of eluent: 1.


    Analytical column: Metrosep A SUPP1 from Metrohm


    Detector: Ampere detector, Au working electrode (oxidation potential is 0.


    Injection volume: 50uL


    (2) Drawing of standard curve

    Take 5 100mL volumetric flasks, add cyanide ion standard solution 1.


    (3) Determination of samples

    In accordance with the same chromatographic conditions and steps as the standard curve, the distillate of the sample is injected into the ion chromatograph to determine the mass concentration of cyanide ion, and the retention time is qualitatively and the instrument response value is quantified


    (4) Blank test

    According to the same chromatographic conditions and steps of the sample determination, the blank sample is injected into the ion chromatograph to determine the cyanide ion mass concentration, and the retention time is qualitatively and the instrument response value is quantified


    Seven, calculation and presentation of results

    (1) Determination of solid waste leachate

    1.


    The cyanide ion mass concentration p(ug/L) in the sample leaching solution is calculated according to formula (1):


    In the formula, c——the peak area of ​​cyanide ion in the sample;

    c 0 ——The peak area of ​​cyanide ion in the blank sample;

    a——Intercept of the standard curve;

    b——The slope of the standard curve;

    f——The dilution factor of the sample


    2.


    When the measurement result is less than 1ug/L, the result retains two decimal places; when the measurement result is greater than or equal to 1ug/L, the result retains three significant digits


    (2) Total solid waste determination

    1.


    The cyanide ion content w (ug/kg) in the sample is calculated according to formula (2):


    In the formula, c——the peak area of ​​cyanide ion in the sample;

    c 0 ——The peak area of ​​cyanide ion in the blank sample;

    a——The intercept of the calibration curve;

    b——The slope of the calibration curve;

    m——weigh the mass of the sample, g;

    w dm ——mass fraction of dry matter in the sample, %;

    V——Volume of distillate, mL;

    f——The dilution factor of the sample


    2.
    Result presentation

    When the measurement result is less than 1mg/kg, the result shall retain two decimal places; when the measurement result is greater than or equal to 1mg/kg, the result shall retain three significant digits
    .

    8.
    Quality Assurance and Quality Control

    (1) The cyanide ion content of the blank test should be less than the detection limit of the method
    .

    (2) At least 10% parallel samples should be made for each batch of samples, and the relative deviation of cyanide ion content should be less than 20%
    .

    (3) At least 10% standard addition should be made for each batch of samples, and the standard addition recovery rate of cyanide ion should be controlled between 70% and 120%
    .

    (4) The preparation of the standard series should be at least 5 points, and the correlation coefficient of the standard curve should not be less than 0.
    999; at least one intermediate calibration point should be made for each batch of samples, and the relative deviation of the measured value from the corresponding point of the standard curve should not exceed 5%
    .

    Nine, matters needing attention

    Hydrogen cyanide is volatile, so in the process of sample determination, every step must be operated quickly and operated in a fume hood, and the bottle cap should be tightly closed at any time
    .

    Related Links: Determination of Cyanide Ion in Solid Waste by Ion Chromatography (1)

     

     

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