气相色谱法分析工业丙烯腈中的杂质

Analyzing impurities in industrial acrylonitrile by gas chromatographic method

以氮气为载气,选用酸改性聚乙二醇(FFAP)毛细管色谱柱对工业丙烯腈中杂质进行了定性分析,并采用校正面积归一化法进行了定量分析。结果表明:采用该方法并根据有效碳数理论,以丙烯腈替代丙腈、顺式(或反式)-丁烯腈替代甲基丙烯腈,测定丙烯腈标样中杂质的回收率为90.1%~106.8%,相对标准偏差为0.8%~7.5%,检测限低于6.6μg/g;对丙烯腈产品中杂质分别采用校正面积归一化法及内标法定量时,同一组分的3次测量结果的重复性良好,2种计算结果无显著差异。

The impurities in acrylonitrile were qualitatively analyzed by using acid-modified polyethylene glycol(FFAP)capillary column with nitrogen as the carrier gas,and the corrected area normalization method was taken as the quantitation method.The results showed that according to the effective carbon number theory,acrylonitrile was suitable to replace propionitrile and cis-(or trans-)butenonitrile was suitable to replace methacrylonitrile.The recovery of impurities in acrylonitrile was 90.1%-106.8%,the relative standard deviation(RSD)was 0.8%-7.5%,and the limit of detection was less than 6.6μg/g.Both corrected area normalization method and internal standard method were applicated to quantitate the impurities in acrylonitrile products,the three measurement results of the same component showed excellent repeatability,and there were no significant difference between the two calculation results.