顶空气相色谱法测定饮用水中11种氯苯类化合物及六氯丁二烯

奚晔; 郑嵘; 詹铭

doi:10.19428/j.cnki.sjpm.2017.01.011

顶空气相色谱法测定饮用水中11种氯苯类化合物及六氯丁二烯

Measuring eleven kinds of chlorobenzenes and hexachlorobutadiene in drinking water by HS-GC

摘要

摘要:
目的建立顶空(HS)气相色谱(GC)法测定生活饮用水中11种氯苯类化合物及六氯丁二烯的方法。
方法取水样10 mL放入预先加入2.5 g氯化钠的20 mL顶空瓶中，在80℃平衡15 min后顶空进样，选用Rtx-1701(30.00 m×0.25 mm×0.25 μm)分离，电子捕获检测器测定。
结果二氯苯、三氯苯、四氯苯、五氯苯、六氯苯和六氯丁二烯方法线性范围分别为1.00~32.00 μg/L、0.20~6.40 μg/L、0.05~1.60 μg/L、0.02~0.64 μg/L、0.02~0.64 μg/L和0.01~0.32 μg/L。若取10 mL水样，则最低检测质量浓度为0.001 62~0.262 00 μg/L。出厂水实际水样加标回收率为80%~119%，相对标准偏差为2.24%~4.99%。
结论该方法具有操作简单、快捷、灵敏度高、不使用有机溶剂等特点，适用于同时测定生活饮用水中氯苯类化合物和六氯丁二烯。

Abstract:
ObjectiveTo apply the HS-GC method to measure eleven kinds of chlorobenzenes and hexachlorobutadiene in drinking water.
MethodsWe put 10mL water sample into a 20 mL vial containing 2.5 g sodium chloride. The vial was stirred at 80℃ for 15 mins prior to headspace sampling. Eleven kinds of chlorobenzenes were separated completely by Rtx-1 701 capillary column(30.00 m×0.25 mm×0.25 μm), detected by electron capture detectors.
ResultsThe linearity of the method ranged from 1.00-32.00 μg/L, 0.20-6.40 μg/L, 0.05-1.60 μg/L, 0.02-0.64 μg/L, 0.02-0.64 μg/L and 0.01-0.32 μg/L for dichlorobenzene isomers, trichlorobenzene isomers, tetrachlorobenzene isomers, pentachlorobenzene, hexachlorobenzene and hexachlorobutadiene. In case of a 10 mL water sample, the lowest detected range of mass concentration was 0.001 62-0.262 00 μg/L. The additional standard recovery rate of finished water samples was in the range of 80%-119% with the relative standard deviation (RSD) in the range of 2.24%-4.99%.
ConclusionThis method is simple, fast, sensitive and needs no organic solvents. It is suitable for measuring both chlorobenzene compounds and hexachlorobutadiene in drinking water simultaneously.

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