金属浴气相色谱法测定水中三氯甲烷和四氯化碳
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摘要
目的建立水中三氯甲烷、四氯化碳的金属浴自动顶空气相色谱法,应用该方法检测铁路饮用水、工业废水中三氯甲烷、四氯化碳含量。方法选用弱极性HP-5高弹石英毛细管柱,安捷伦金属浴自动顶空仪,电子捕获检测器检测,外标法定量。结果三氯甲烷在20~200μg/L浓度范围内具有良好的线性关系,相关系数r=0.999 9,加标回收率为91.3%~99.1%,RSD为3.3%~5.2%,检出限为0.1μg/L。四氯化碳在1~10μg/L浓度范围内具有良好的线性关系,相关系数r=0.999 5,加标回收率为91.1%~99.0%,RSD为4.8%~9.5%,检出限为0.01μg/L。本方法能够减少样品采样量,避免每次30μl手动直接进样的误差,降低由于水浴加热的不稳定导致的各个顶空瓶的饱和蒸气压差异较大。结论该方法具有灵敏、准确、高效等优点,适合分析大批量水样中三氯甲烷、四氯化碳的含量。
Objective To establish an metal bath automatic headspace gas chromatography method for the determination of trichloromethane and carbon tetrachloride in water, and detect the content of trichloromethane and carbon tetrachloride in railway drinking water and industrial waste water by this method. Methods Weak polarity HP-5 high elasticity quartz capillary column, agilent metal bath automatic headspace instrument, electron capture detector and external standard method were used. Results Trichloroform had a good linear relationship in the concentration range of 20-200 μg/L, the correlation coefficient was r=0.999 9 and the recoveries rate was 91.3%-99.1%, and the RSD was 3.3%-5.2%. The detection limit was0.1 μg/L. The detection limit for carbon tetrachloride had a good linear relationship in the concentration range of 1-10 μg/L, the correlation coefficient was r=0.999 5 and the recoveries rate was 91.1%-99.0%,and the RSD was 4.8%-9.5%. The detection limit of this method was 0.01 μg/L. This method can reduce the sample sampling amount, avoid the error of 30 μl manual direct injection every time, and reduce the difference of saturated vapor pressure of each headspace bottle caused by the instability of water bath heating. Conclusion The method has the advantages of sensitivity, accurate and high efficiency. It is suitable for analyzing the content of trichloromethane and carbon tetrachloride in large quantities of water samples.
Objective To establish an metal bath automatic headspace gas chromatography method for the determination of trichloromethane and carbon tetrachloride in water, and detect the content of trichloromethane and carbon tetrachloride in railway drinking water and industrial waste water by this method. Methods Weak polarity HP-5 high elasticity quartz capillary column, agilent metal bath automatic headspace instrument, electron capture detector and external standard method were used. Results Trichloroform had a good linear relationship in the concentration range of 20-200 μg/L, the correlation coefficient was r=0.999 9 and the recoveries rate was 91.3%-99.1%, and the RSD was 3.3%-5.2%. The detection limit was0.1 μg/L. The detection limit for carbon tetrachloride had a good linear relationship in the concentration range of 1-10 μg/L, the correlation coefficient was r=0.999 5 and the recoveries rate was 91.1%-99.0%,and the RSD was 4.8%-9.5%. The detection limit of this method was 0.01 μg/L. This method can reduce the sample sampling amount, avoid the error of 30 μl manual direct injection every time, and reduce the difference of saturated vapor pressure of each headspace bottle caused by the instability of water bath heating. Conclusion The method has the advantages of sensitivity, accurate and high efficiency. It is suitable for analyzing the content of trichloromethane and carbon tetrachloride in large quantities of water samples.
引文
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[2]李新伟,崔永学,张扬,等.济南市市政供水三氯甲烷和四氯化碳含量及风险评估[J].环境卫生学杂志,2018,8(1):42-45.
[3]陈玉凤.气相色谱法测定生活饮用水中三氯甲烷四氯化碳的方法探讨[J].微量元素与健康研究,2018,35(3):58-59.
[4]杨姣兰,董梦萌,曹宁涛,等.全国实验室生活饮用水中三氯甲烷的测定能力验证研究[J].环境与健康杂志,2016,33(12):1101-1104.