吹扫捕集/GC-MS联用法测定水中挥发性卤代烃的方法优化

Optimization Method for Determination of Volatile Halogenated Organic Compounds in Water by Purge and Trap/Gas Chromatography-Mass Spectrometry

采用吹扫捕集/气相色谱-质谱(GC-MS)法对水中13种挥发性卤代烃进行测定。通过调整吹扫温度和吹扫时间、解吸温度和解吸时间,分析吹扫捕集条件对吹扫捕集效率的影响,并确定最佳吹扫捕集条件。结果表明,在吹扫温度40℃、吹扫时间12 min、解吸温度240℃、解吸时间3 min的条件下,13种挥发性卤代烃的平均加标回收率为94.5%～106.7%,相对标准偏差为2.4%～5.5%,相关系数为0.999 1～0.999 9,最低检出限为0.03～0.28μg/L。与国家标准方法相比,该方法操作简单、检出限低,具有较好的线性关系、灵敏度高、重复性好等优点。

Purge and trap/gas chromatography mass spectrometry was used to determine 13 volatile halogenated organic compounds in water. By adjusting the purge and trap affected by purge temperature, purge time, desorption temperature and desorption time, the efficiency of purge and trap affected by purge and trap conditions was analyzed, and the best purge and trap conditions were determined. Under the optimized conditions, the detection limits were 0.03 ~0.28 ~g/L, the correlation coefficients of calibration curve were 0.999 1-0.999 9, the average recoveries were 94.5%-106.7%, and the relative standard deviations were 2.4%~5.5%. Compared with the national standard method, this method is easy to operate and of low detection limit. The linear relations were well, high sensitivity and good repeatability. The method can meet the requirements for the determination of volatile halogenated organiccompounds in surface water and drinking water.