提出了静态顶空-气相色谱法测定养殖用水中11种氯苯类化合物的方法。取10 mL含200 g·L-1氯化钠的水样在20 mL顶空瓶中于70 ℃振摇30 min进行顶空进样的条件优化。选用DB-35MS毛细管气相色谱柱(30 m×0.25 mm,0.25 μm)分离,电子捕获检测器检测,外标法或标准加入法定量。在优化条件下,二氯苯、三氯苯、四氯苯的线性范围分别为0.16~8 μg·L-1,0.017 6~0.88 μg·L-1,0.004~0.2 μg·L-1,五氯苯和六氯苯的线性范围均为0.001~0.05 μg·L-1。11种氯苯类化合物检出限(3S/N)为0.0002~0.04 μg·L-1,应用此方法对养殖用水进行测定,回收率在86.0%~106%之间,测定值的相对标准偏差(n=5)在2.1%~5.8%之间。

GC was applied to the determination of 11 chlorobenzenes in aquaculture water with static headspace. The optimum experimental conditions found were to put 10 mL water sample containing 200 g·L-1 sodium chloride in a 20 mL vial and stir at 70 ℃ for 30 mins. 11 chlorobenzenes were separated completely by DB-35 MS capillary column (30 m×0.25 mm, 0.25 μm), detected by electron capture detector and then quantify through external standard method or standard addition method. The linearity of the method ranged from 0.16 to 8.0 μg·L-1 for dichlorobenzene isomers, 0.017 6-0.88 μg·L-1 for trichlorobenzene isomers, 0.004-0.2 μg·L-1 for tetrachlorobenzene isomers and from 0.001 to 0.05 μg·L-1 for pentachlorobenzene and hexachlorobenzene. The limits of detection ranged from 0.0002 to 0.04 μg·L-1. The proposed method was used in the analysis of aquaculture water samples, giving values of recovery and RSD′s (n=5)in the ranges of 86.0%-106% and 2.1%-5.8% respectively.