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    Home > Chemicals Industry > Chemical Technology > Determination of Alkyl Mercury in Solid Waste Leachate Purge and Trap/Gas Chromatography-Cold Atomic Fluorescence Method (1)

    Determination of Alkyl Mercury in Solid Waste Leachate Purge and Trap/Gas Chromatography-Cold Atomic Fluorescence Method (1)

    • Last Update: 2022-03-12
    • Source: Internet
    • Author: User
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    1.
    Scope of application

    This method is applicable to solid waste leachate methylmercury and ethylmercury assay containing the wall
    .

    When the sampling volume of the extract is 45 mL, the detection limits of methyl mercury and ethyl mercury are 0.
    01 ng/L and 0.
    02 ng/L, respectively

    .

    Second, the principle of the method

    The extract was distilled with a distillation apparatus, and the distillate was derivatized with sodium tetrapropyl boride and measured by an alkyl mercury analyzer
    .
    Qualitatively by retention time and quantified by external standard method

    .

    3.
    Reagents and materials

    Unless otherwise specified, analytical reagents conforming to national standards are used for analysis, and the experimental water is newly prepared ultrapure water or distilled water
    .

    (1) Hydrochloric acid : pure superior grade
    .

    (2) Copper sulfate : analytically pure
    .

    (3) Acetic acid : pure superior grade
    .

    (4) Sodium acetate : excellent grade pure
    .

    (5) Sodium tetrapropyl boride: analytically pure
    .

    Dissolve 1.
    0 g of sodium tetrapropyl boride in 100 mL of KOH solution with a mass fraction of 2% at 0°C, shake well, and dispense into 4 mL brown glass bottles, and then immediately place them in a refrigerator at -18°C for storage and use Temporarily thaw before

    .

    (6) Standard solution: standard solution of methylmercury and ethylmercury, ρ=1.
    00mg/L, and the solvent is pure water

    .

    (7) Concentrated sulfuric acid: pure superior grade
    .

    (8) Concentrated nitric acid: pure superior grade
    .

    (9) Extractant: Add a mixture of concentrated sulfuric acid and concentrated nitric acid with a mass ratio of 2:1 to ultrapure water (about 2 drops of 1L water) to make the pH 3.
    20±0.
    05

    .

    Four, instruments and equipment

    (1) Alkyl mercury analyzer: It consists of a purge and trap system, a gas chromatograph, a thermal cracking system, and a cold atomic fluorescence spectrometer
    .

    (2) Distillation instrument: fraction collection device with ice bath
    .

    (3) Flip the oscillator
    .

    Five, pre-treatment

    (1) Preparation of leaching solution

    "Semi-Volatile Organic Compound Analysis Technology-Preparation of Sulfuric Acid and Nitric Acid from Leachate"

    (2) Steaming letter

    Accurately measure 45mL pure water (or sample, need to add 0.
    4% HC1) in a distillation flask, add 100mL saturated CuSO
    4 solution, add 4.
    4mL ultrapure water and 0.
    6mL acetic acid/sodium acetate buffer solution with pH 6.
    0 to the receiving flask ( 2mol/L), distill at 125°C for 3.
    5~4h, distill out about 80% of the distillate (35~36mL), the distillate receiving flask should be placed in a water tank with an ice bath

    .

    (3) Derivative

    Pour all the distillate into a 42 mL sample bottle, then add 50 μm of sodium tetrapropyl boride for derivatization, and analyze it on the machine after 20 minutes
    .

    Related links: Semi-volatile organic compounds analysis technology-leaching solution preparation sulfuric acid and nitric acid method

     

     

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