气相质谱法测定甲基氯硅烷中多氯联苯

Determination of Polychlorinated Biphenyls in Methyl Chlorosilane by Gas Chromatograph-Mass Spectrometer

通过采用氢氧化钾/甲醇溶液溶解和净化,再用正己烷萃取的前处理方式,采用气相质谱法对甲基氯硅烷产品中10种多氯联苯的含量进行分析。结果表明:10种多氯联苯的线性范围为10～500μg/L,相关系数R≥0.998,回收率为99.5%～111.0%,相对标准偏差RSD≤9.5%(n=9)。本方法前处理简便,灵敏度高,重现性好,适用于甲基氯硅烷产品中10种多氯联苯的同时分析。

In this paper, the contents of 10 polychlorinated biphenyls in methyl chlorosilane were analyzed by gaschromatograph -mass spectrometer （GC -MS） with the pretreatment method of being dissolved and purified in KOH/methanol solution and extracted by n-hexane. The results showed that the linear range of 10 polychlorinated biphenyls was10~500 滋g/L, the correlation coefficient（R） was no less than 0.998, the recovery rate was 99.5%~111.0%, the relativestandard deviation （RSD） was no more than 9.5%（n =9） . This method has advantages of simple pretreatment, highsensitivity and good reproducibility. It is suitable for the simultaneous analysis of 10 polychlorinated biphenyls in methylchlorosilane.