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    Home > Chemicals Industry > Chemical Technology > Cyclohexanol for industrial use (2)

    Cyclohexanol for industrial use (2)

    • Last Update: 2021-09-25
    • Source: Internet
    • Author: User
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    5 Test method

    5.


    Industrial cyclohexanol is a flammable product, so pay attention to safety during analysis


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    Unless otherwise specified, only reagents confirmed to be analytically pure and grade 3 water specified in GB/T6682-2008 are used in the analysis


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    Using gas chromatography, under selected working conditions, the sample is vaporized and passed through the chromatographic column, so that the components are separated, detected by a hydrogen flame ionization detector, corrected for water content, and calculated by area normalization method.


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    3.
    4 Chromatographic analysis conditions

    The recommended chromatographic columns and typical chromatographic analysis conditions are shown in Table 2
    .
    The typical chromatogram of the capillary column is shown in Appendix A, Figure A.
    1, and the relative retention value of each component is shown in Appendix A, Table A.
    1
    .
    Other chromatographic columns and chromatographic operating conditions that can achieve the same degree of separation can be used
    .

    Table 2 Recommended chromatographic columns and typical chromatographic analysis conditions

    5.
    3.
    5 Analysis steps

    Adjust the instrument according to the chromatographic operating conditions.
    After the baseline is stable, use a micro-syringe to inject the sample, measure the area of ​​each peak, and calibrate the water content and calculate according to the area normalization method
    .

    5.
    3.
    6 Result calculation

    The mass fraction w i of each tested component , the value is expressed in %, respectively calculated according to formula (1):

    Where:

    A i —the peak area of ​​the measured component i;

    w Water —The value of the mass fraction of water measured according to 5.
    5;

    ∑A i — the sum of the corrected peak areas of each component
    .

    Take the arithmetic average of the two parallel determination results as the determination result
    .
    The absolute difference between the two parallel determination results of cyclohexanol content is not more than 0.
    2%; when the mass fraction of impurities is ≥0.
    5%, the absolute difference between the two parallel determination results is not more than 5% of the arithmetic mean; the mass fraction of impurities is < At 0.
    5%, the absolute difference between the two parallel determination results is not more than 10% of the arithmetic mean
    .

    5.
    4 Determination of chromaticity

    According to the provisions of GB/T3143-1982
    .

    5.
    5 Determination of water content

    According to the provisions of GB/T6283-2008 or GB/T2366-2008
    .
    The test method specified in GB/T6283-2008 is the arbitration law
    .
    When measuring samples containing cyclohexanone impurities according to the method specified in GB/T6283-2008 , Karl Fischer reagent uses special reagents for aldehydes and ketones
    .

    Take the arithmetic average of the two parallel determination results as the determination result.
    When the determination is performed according to the provisions of GB/T6283-2008, the absolute difference between the two parallel determination results shall not be greater than 25% of the arithmetic average; according to GB/T2366-2008 When the determination is carried out according to the regulations, the absolute difference between the two parallel determination results shall not be greater than 35% of the arithmetic mean
    .

     

     

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