无分流/顶空自动进样气相色谱法测定挥发性卤代烃

Determination of Volatile Halogenated Hydrocarbon by Splitless GC and Automatic Top-balance Inject

采用大口径毛细管柱无分流/静态顶空自动进样法测定水中挥发性卤代烃。使用顶空自动进样器,在无分流毛细管柱/电子捕获检测器的仪器条件下,分析地表水和自来水中的三氯甲烷、四氯化碳、三氯乙烯、四氯乙烯、三溴甲烷。对色谱条件和顶空自动进样器条件进行了合理选择。该方法与传统恒温加热手动进样法相比,重复性好,精密度高,相对标准偏差为2.6%-6.3%,回收率在91%-110%之间。由于采用无分流进样方式,因此大大降低了检出限,各分析对象检出限为三氯甲烷0.005μg.L^-1,四氯化碳0.003μg.L^-1,三氯乙烯0.09μg.L^-1,四氯乙烯0.02μg.L^-1,三溴甲烷0.15μg.L^-1。方法无需前处理,操作快捷,对人体伤害少。

The method for determination of volatile halogenated hydrocarbon in the water by splitless GC was studied. The way of automatic top-balance inject was adapted and used the splitless GC with ECD, nitrotri- chloromethane, carbon tetra-chloride, trichloroethylene, tetrachloroethylene, tribromomethane in the drink water and the tap water were determined. The condition of the splitless GC and automatic top-balance inject was selected. Compared with the top-balance inject with hand, this method had the good repetition and precision. Relative standard deviations was 2.6% --6.3%, recoveries was 91% -- 110%. Becase of the application of splitless GC, the detection limits had come donna： nitrotri-chloromethane 0. 005 μg·L^-1, carbon tetra-chloride 0. 003μg·L^-1, trichloroethylene 0.09μg·L^-1, tetrachloroethylene 0.02 μg·L^-1, tribromomethane 0.15μg·L^-1.