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    Home > Chemicals Industry > Chemical Technology > Pentaerythritol for industrial use (3)

    Pentaerythritol for industrial use (3)

    • Last Update: 2021-11-18
    • Source: Internet
    • Author: User
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    The pentaerythritol and impurity components in the sample react with the silylation reagent to generate the corresponding silylated derivatives


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    The chromatographic column and chromatographic operating conditions recommended by this standard are shown in Table 2


    The chromatographic column should be aged before first use
    .
    In the case of a carrier gas (N 2 ) flow rate of 10 mmL/min, the initial column temperature is kept at 120°C for 2 hours
    .
    Then the temperature was raised to 260°C for 2h, and then to 290°C for 12h
    .

    Table 2 Recommended chromatographic column and chromatographic operating conditions

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    5 Analysis steps

    Debug the instrument according to the chromatographic operating conditions listed in Table 2 to make the instrument stable
    .

    Weigh 5.
    1 mg (5-6) mg of the prepared sample, place it in a 2mL sample bottle, add 0.
    1mL N,N-dimethylformamide, 0.
    05mL N,O-(trimethylsilyl ) Trifluoroacetamide, cover the bottle stopper and shake well, and heat it in an oven at (70-80)°C for 10 minutes to obtain the prepared silanized derivative
    .

    Use a 10uL glass syringe to draw 1uL for analysis or use an autosampler to inject
    .
    Quantify by area naturalization method
    .

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    6 Result calculation

    The mass fraction w 2 of pentaerythritol , the value is expressed in %, calculated according to formula (2):

    Where:

    A—the area of ​​the chromatographic peak of pentaerythritol silylated derivative;

    A i —the area of ​​the chromatographic peak of a silanized derivative of a component;

    w 5 —5.
    5 The mass fraction of the measured loss on drying, and the value is expressed in %
    .

    Take the arithmetic average of the two parallel determination results as the determination result
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    The absolute difference between the two parallel determination results is not more than 0.
    20%
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    Related Links: Pentaerythritol for Industrial Use (2)

     

     

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