毛细管柱顶空-气相色谱法测定水中三卤甲烷和四氯化碳
目的 建立毛细管柱顶空-气相色谱测定三卤甲烷和四氯化碳共5种常见卤代烃的方法。方法 将样品放入顶空瓶中, 设置好顶空装置条件, 在自动顶空装置中加热平衡30 min, 经DB-624毛细管柱分离, 使用ECD作为检测器进行分析, 采用外标法定量, 气相色谱法测定水中三卤甲烷和四氯化碳含量。结果 本方法的分离效果良好, 三氯甲烷、四氯化碳、二氯一溴甲烷、二溴一氯甲烷和三溴甲烷的检出限分别为0.056、0.022、0.083、0.090、0.010 μg/L。在0.010~0.090 μg/L范围内线性关系良好, 相关系数范围为0.9990~0.9998, 加标回收率为91.6%~97.8%, 相对标准偏差(relative standard deviation, RSD)为1.19%~5.64%。结论 该方法具有良好的精密度和准确度, 能够满足日常实验室对卤代烃检测的要求。
Objective To establish a method for the determination of 5 common halogenated hydrocarbons including trihalomethanes and carbon tetrachloride. Methods The samples were put into the headspace bottle, after setting the device in the automatic headspace condition, the samples were heated and balanced for 30 min, separated by DB-624 capillary column, analyzed with ECD as the detector, and quantified by external standard method. The trihalomethanes and carbon tetrachloride in water were determined by gas chromatography. Results This method had good separation effects, the limits of detection of trichloromethane, carbon tetrachloride, bromodichloromethane, dibromo-monochloro-methane, and tribromomethane were 0.056, 0.022, 0.083, 0.090, and 0.010 μg/L, respectively. In the range of 0.010~0.090 μg/L, the correlation coefficients were in the range of 0.9990~0.9998. The spiked recoveries were 91.6%~97.8%, while the relative standard deviations (RSDs) were 1.19%~5.64%. Conclusion This method has good precision and accuracy, and can meet the requirements of halogenated hydrocarbon detection in daily laboratory.
标题:毛细管柱顶空-气相色谱法测定水中三卤甲烷和四氯化碳
英文标题:Determination of trihalomethanes and carbon tetrachloride in water by capillary column headspace-gas chromatography
作者:
杨大鹏 吉林省疾病预防控制中心
马杰 吉林省疾病预防控制中心
白梅 吉林省疾病预防控制中心
刘思洁 吉林省疾病预防控制中心
中文关键词:水,三卤甲烷,四氯化碳,顶空,气相色谱,检测,
英文关键词:water,trihalomethanes,carbon tetrachloride,headspace,gas chromatography,determination,
发表日期:2017-11-20
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