顶空气相色谱法同时测定生活饮用水中17种挥发性卤代烃

Simultaneous determination of 17 kinds of volatile halogenated hydrocarbons in drinking water by headspace gas chromatography

建立了顶空气相色谱法同时测定生活饮用水中17种挥发性卤代烃的分析方法。样品采用自动顶空进样技术,经DB–5毛细管色谱柱(30 m×0.32 mm,0.25μm)分离后,用电子捕获检测器检测。优化样品保存条件为加入0.5 g抗坏血酸,冷藏避光保存。优化顶空条件:平衡温度为70℃,平衡时间为30 min,NaCl添加量为2.5 g。使用4-溴氟苯作为质控物质,保证测定结果的准确性。17种挥发性卤代烃的标准曲线相关系数均不小于0.998,方法检出限为0.003~2μg/L,平均回收率为85.7%~105.7%,测定结果的相对标准偏差为1.0%~5.6%(n=6)。该方法快速、灵敏度高、重现性好,适用于生活饮用水中17种挥发性卤代烃的同时测定。

A method was established for the simultaneous determination of 17 volatile halogenated hydrocarbons in drinking water by headspace gas chromatography.The samples were injected by automatic headspace sampling technology,separated by DB-5 capillary column(30 m×0.32 mm,0.25μm),and analyzed by ECD detector.Optimize sample storage conditions were added 0.5 g ascorbic acid,refrigerated and protected from light.Optimize headspace conditions were equilibrium temperature of 70℃,equilibrium time of 30 min,NaCl addition of 2.5 g.4-bromofluorobenzene was used as quality control material to ensure the accuracy of determination.The standard curve correlation coefficients of 17 volatile halogenated hydrocarbons were all not less than 0.998.The detection limits of the method were within 0.003-2μg/L,the average recovery rates were within 85.7%-105.7%,and the relative standard deviations of determination results were within 1.0%-5.6%(n=6).This method is rapid,sensitive and repeatable,which is suitable for the simultaneous determination of 17 volatile halogenated hydrocarbons in drinking water.