建立气相色谱法测定乙腈装置减压共沸塔顶(T202顶)粗乙腈杂质含量的分析方法。采用DB-FFAP毛细管色谱柱、氢火焰检测器，带范围校正归一化法定量。通过实验选择最佳分析操作条件，成功分析出粗乙腈中微量丙烯腈、丙酮、唑、丙腈等杂质含量。解决了填充柱在分析此样品时，主要杂质丙烯腈与未知杂质色噁谱峰重叠的问题。测定的相对标准偏差均小于5.0%，各组分加标回收率在97%～102%之间，能满足分析要求。% A gas chromatography analysis method for determining impurity content in acetonitrile at the top of vacuum azeotropic tower was established through adopting capillary column DB-FFAP, flame ionization detector and correcting the area with normalization. The best analysis conditions were obtained through experiments, and impurity content in acetonitrile was successfully analyzed, such as trace acrylonitrile,acetone , oxazole , propionitrile and so on. The problem of overlapping chromatographic peaks in chromatography analysis with the packed column was solved. The relative standard deviation was less than 5.0%, the recovery rates of components were in the range of 97%~102%,so the method can satisfy the analysis requirement.
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