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Analytic method of acrylonitrile material

An analysis method and technology of acrylonitrile, which is applied in the field of analysis of acrylonitrile materials, can solve the problems of low content, qualitative and quantitative analysis, etc., and achieve high sensitivity detection and accurate quantification, good quantitative accuracy and repeatability, and good technology effect of effect

Active Publication Date: 2014-07-02
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the trace organic impurities in high-purity acrylonitrile cannot be qualitatively and quantitatively analyzed by the existing acrylonitrile analysis method because the content is too low (<1mk / kg), and a new acrylonitrile is provided. Analytical method for nitrile materials

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  • Analytic method of acrylonitrile material
  • Analytic method of acrylonitrile material
  • Analytic method of acrylonitrile material

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Embodiment 1

[0022] Adopt gas chromatography-mass spectrometry analysis method of the present invention, take toluene as internal standard substance, to containing acetaldehyde, acetone, acrolein, benzene, methacrylonitrile, methyl methacrylate, acetonitrile, oxazole, propionitrile, cis - Acrylonitrile standard samples of ten trace organic impurities were analyzed. The standard sample is injected from the split inlet of the gas chromatography, and the components are separated by the capillary column, and then enter the mass spectrometry system through the transfer line, and are detected by the quadrupole mass spectrometer detector and the selected ion detection mode, and the internal standard method is used for quantification. Typical analysis conditions are shown in Table 1. Standard 1 # Relative mass correction factor for determination of each impurity, standard 2 # analyzed as the sample to be tested. The selected ion detection diagram of the standard sample is shown in figure 1 , S...

Embodiment 2

[0029] The gas chromatography-mass spectrometry analysis method of the present invention is used to analyze the actual samples before and after refining the acrylonitrile with toluene as an internal standard. The sample is injected by the split inlet of gas chromatography, and each component is separated by capillary chromatographic column, and then enters the mass spectrometry system through the transmission line, and is detected by the quadrupole mass spectrometer detector and the selected ion detection mode, and the internal standard method is used for quantification. Typical analysis conditions are shown in Table 1, and the selected ion detection diagrams of acrylonitrile samples before and after purification are shown in figure 2 , and the analysis results are shown in Table 3.

[0030] Table 3 Analytical results of the actual sample of acrylonitrile before and after refining mk / kg (w / w)

[0031] components

[0032] As can be seen from the measurement results ...

Embodiment 3

[0034]Using the gas chromatography-mass spectrometry analysis method of the present invention, an actual sample of high-purity acrylonitrile is analyzed with toluene as an internal standard. The sample is injected by the split inlet of gas chromatography, and each component is separated by capillary chromatographic column, and then enters the mass spectrometry system through the transmission line, and is detected by the quadrupole mass spectrometer detector and the selected ion detection mode, and the internal standard method is used for quantification. Typical analysis conditions are shown in Table 1. The comparison of this method with the gas chromatography-mass spectrometry / full scan (Scan) method and the standard method GB / T7717.12-2008 measurement results is shown in Table 4, and the chromatogram is shown in image 3 . The gas chromatography-mass spectrometry / full scan (Scan) method mass range is 15-200, and the rest of the analysis conditions are the same as in Table 1....

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Abstract

The invention relates to an analytic method of an acrylonitrile material to mainly solve a problem that microscale organic impurities in highly pure acrylonitrile cannot be qualitatively or quantitatively analyzed through present acrylonitrile analysis methods because contents of the organic impurities are too low (less than 1mg / kg). The analytic method, which adopts a gas chromatography-mass spectrometry / selection ion detection technology and an internal standard method to make the microscale organic impurities in the acrylonitrile be accurately qualitative and quantitative, so the method well solves the problem through above technical scheme, and can be used for the determination of the microscale organic impurities in the highly pure acrylonitrile.

Description

technical field [0001] The invention relates to an analysis method for acrylonitrile materials, in particular to a gas chromatography-mass spectrometry analysis method for trace organic impurities in high-purity acrylonitrile. Background technique [0002] Carbon fiber is a fibrous carbon material that has a wide range of applications in the automotive industry, aviation, aerospace and sports equipment. In recent years, the development of carbon fiber and composite materials is very rapid, and polyacrylonitrile-based carbon fiber has become one of the hot spots in the research and development of new materials. [0003] In order to ensure the good performance and product quality of carbon fiber, the carbon fiber production process has put forward strict quality requirements for its precursor and polymer grade acrylonitrile. The purity of acrylonitrile should reach more than 99.99% (mass fraction), and the acrolein in acrylonitrile And other trace organic impurities should al...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 张育红高枝荣王川
Owner CHINA PETROLEUM & CHEM CORP
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