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    Home > Chemicals Industry > Chemical Technology > Determination of trace carbon monoxide, carbon dioxide and acetylene in ethylene and propylene for industrial use. Gas chromatography (2)

    Determination of trace carbon monoxide, carbon dioxide and acetylene in ethylene and propylene for industrial use. Gas chromatography (2)

    • Last Update: 2022-01-18
    • Source: Internet
    • Author: User
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    5 Instruments

    5.
    1 Gas chromatograph: equipped with 10-port valve sampling device (quantity tube volume 1mL~3mL) and backflushing device, split sampling system and hydrogen flame ionization detector (FID), and can operate according to the conditions of Table 1 or Table 3.
    Any dual gas path gas chromatograph

    .
    To determine
    carbon monoxide , carbon dioxide also needs to be equipped with a nickel reformer catalytic hydrogenation device
    .
    The peak height of the cattle produced by the instrument for the minimum detection concentration of impurities specified in this standard should be at least twice the noise

    .
    The ten-way valve connection and back-flushing device of the instrument are shown in Figure 1 and Figure 2

    .
    Other sampling and backflushing devices that meet the separation and quantification effects of this standard can also be used

    .

    Note: It is not necessary to connect a nickel reformer to determine acetylene
    .

    Figure 1 Connection diagram of ten-way valve in sampling and backflushing state

    Note: It is not necessary to connect a nickel reformer to determine acetylene
    .

    Figure 2 Connection diagram of the ten-port valve in the sampling state

    5.
    2 Chromatographic column: The chromatographic column recommended by this standard for the determination of
    carbon monoxide and carbon dioxide and typical operating conditions are shown in Table 1.
    Typical chromatograms are shown in Figures 3 and 4; the chromatographic columns recommended by this standard for the determination of acetylene and typical operating conditions are shown in Table 3.
    Typical chromatograms Figures are shown in Figure 5 and Figure 6

    .
    Other chromatographic columns and analysis conditions that can give the same separation and quantification effect can also be used

    .

    5.
    3 Nickel reformer: The nickel reformer
    is a device that converts carbon monoxide and
    carbon dioxide into methane by catalytic hydrogenation, and consists of a nickel catalytic hydrogenation column and a heating device
    .
    The recommended operating conditions of the nickel catalytic hydrogenation column are shown in Table 2 (the operating conditions of the packed column and the capillary column are the same)

    .

    The nickel catalytic hydrogenation column is prepared as follows: Weigh 200g of nickel nitrate and dissolve it in 90mL of distilled water, add 80g of 6201 chromatographic support or other suitable support, boil (5-10) min, cool, filter, and place the support in an evaporating dish Dry it at 105°C, then place it on an electric stove to slowly heat (should be in a fume hood) until the red-brown nitrogen dioxide is exhausted.
    After burning at 450°C under nitrogen for 7 hours, cool down to obtain nickel oxide.
    Catalyst

    .
    Put it into a clean, dry stainless steel column tube, and pass hydrogen (flow rate about 50mL/min) at 350℃~380℃ for 4h to reduce it to nickel catalyst for use

    .
    The prepared nickel catalytic hydrogenation column should be sealed and stored to prevent the activity of the catalyst from being reduced after contact with air and water

    .

    Note: Standard samples should be used to check the reactivity of the nickel catalytic hydrogenation column on a regular basis
    .

    5.
    4 Recording device: electronic integrator or chromatographic data processing device

    .

    Table 1 Chromatographic columns and typical operating conditions for the determination of carbon monoxide and carbon dioxide

    Table 2 Operating conditions of nickel catalytic hydrogenation column

    Figure 3 Typical chromatograms of ethylene and propylene standard samples on TDX-01 packed column

    Figure 4 Typical chromatogram of ethylene and propylene standard sample on Carbonbond capillary column

    Table 3 Chromatographic column for acetylene analysis and typical operating conditions



    Figure 5 Typical chromatograms of ethylene and propylene standard samples on TDX-01 packed column

    Figure 6 Typical chromatograms of ethylene and propylene standard samples on Carbonbond capillary column

     

     

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