饮用水中11种卤代烃的顶空气相色谱测定法

Determination of 11 Kinds of Halogenated Alkane Hydrocarbon in Drinking Water with Headspace Gas Chromatography

目的探讨生活饮用水中11种卤代烃的顶空气相色谱(HS-GC)测定方法。方法水中的微量卤代烃经顶空提取后,应用DB-5毛细管色谱柱,同时采用程序升温和程序升流方式进行GC分析(ECD检测器),以保留时间定性,外标法定量。结果二氯甲烷、三氯甲烷、1,1,1-三氯乙烷、1,2-二氯乙烷、四氯化碳、三氯乙烯、一溴二氯甲烷、1,1,2-三氯乙烷、二溴一氯甲烷、四氯乙烯、三溴甲烷的线性范围分别为0.8～4024.0、0.007～33.5、0.004～19.2、1.4～6821.0、0.002～10.0、0.005～25.6、0.002～12.1、0.1～717.8、0.005～23.5、0.002～8.1、0.02～87.7μg/L,最低检测浓度为0.01～4.1μg/L,水样加标回收率为89.7%～110.0%,RSD为2.8%～9.0%。结论该方法一次性完成饮用水中11种卤代烃的分离和测定,分析时间仅为10.7min,操作简便、灵敏。

Objective To establish a method to determine halogenated alkane hydrocarbon in drinking water with headspace gas chromatography. Methods Halogenated alkane hydrocarbon in the water were extracted by headspace technology, then analyzed with DB-5 capillary column, in the same time, they were determined with GC by controlling the temperature and the speed of nitrogen. The retention time of the peaks was used for qualitative analysis, while external standard method was used for quantitative analysis. Results The linear ranges for dichloromethane, trichloromethane, 1, 1, 1-trichloroethane, 1, 2-dichloroethane, carbon tetrachloride, trichloroethylene, bromodichloromomethane, 1, 1, 2-trichloroethane, dibromochloromethane, tetrachloroethylene, tribromomethane were 0.8-4 024.0, 0.007-33.5, 0.004-19.2, 1.4-6 821.0, 0.002-10.0, 0.005-25.6, 0.002-12.1, 0.1-717.8, 0.005-23.5, 0.002-8.1 and 0.02-87.7 μg/L. The lowest determination limit were 0.01- 4.1 μg/L, the rate of recovery were 89.7%-110.0% and RSDs were 2.8%-9.0%. Conclusion This method can efficiently separate and accurately determine 11 kinds of halogenated alkane hydrocarbon in drinking water. It is simple, rapid and sensitive.