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为建立饮用水中7种挥发性卤代烃的顶空气相色谱测定法,对水中的三氯甲烷、四氯化碳、三氯乙烯、一溴二氯甲烷、二溴一氯甲烷、四氯乙烯、三溴甲烷经顶空提取后,采用DB-5毛细管色谱柱分离,以程序升温恒定流量方式进行气相色谱(GC)分析,以保留时间定性,外标法定量。结果显示,在0~97.5μg/L范围内,三氯甲烷的线性方程为y=14.40x+9.579,检出限为0.0975μg/L;在0~4.80μg/L范围内,四氯化碳的线性方程为y=221.1x+10.49,检出限为0.0080μg/L;在0~39.4μg/L范围内,三氯乙烯的线性方程为y=38.90x+19.20,检出限为0.118μg/L;在0~40.1μg/L范围内,一溴二氯甲烷的线性方程为y=40.37x-4.037,检出限为0.0401μg/L;在0~40.3μg/L范围内,二溴一氯甲烷的线性方程为y=19.69x+9.674,检出限为0.0807μg/L;在0~16.3μg/L范围内,四氯乙烯的线性方程为y=179.7x-2.743,检出限为0.0163μg/L;在0~80.9μg/L范围内,三溴甲烷的线性方程为y=4.883x+7.217,检出限为0.486μg/L;各回归方程均r≥0.999。该方法所得的平均回收率为85.6%~110.3%,RSD为1.24%~6.10%。表明该方法具有灵敏度高、检出限低、操作便捷、结果准确的优点,适用于同时测定水中7种挥发性卤代烃。
In order to establish a headspace gas chromatographic method for the determination of seven volatile halogenated hydrocarbons in drinking water, the determination of trichloromethane, carbon tetrachloride, trichlorethylene, bromodichloromethane, dibromochloromethane, tetrachloro Ethylene and tribromomethane were separated by headspace and separated on a DB-5 capillary column. Gas chromatography (GC) was performed with a constant temperature programmed flow method. The retention time was qualitative and the external standard method was used for quantification. The results showed that the linear equation of chloroform was y = 14.40x + 9.579 with a detection limit of 0.0975μg / L in the range of 0 ~ 97.5μg / L. In the range of 0 ~ 4.80μg / L, carbon tetrachloride The linear equation was y = 221.1x + 10.49 with a detection limit of 0.0080μg / L. The linear equation of trichlorethylene was y = 38.90x + 19.20 in the range of 0-39.4μg / L with a detection limit of 0.118μg / L; the linear equation of bromodichloromethane was y = 40.37x-4.037 in the range of 0 ~ 40.1μg / L with the detection limit of 0.0401μg / L; in the range of 0 ~ 40.3μg / L, The linear equation of methyl chloroform was y = 19.69x + 9.674, the detection limit was 0.0807μg / L. The linear equation of tetrachlorethylene was y = 179.7x-2.743 in the range of 0 ~ 16.3μg / L with the detection limit The linear equation of tribromomethane was y = 4.883x +7.217, the detection limit was 0.486μg / L; the regression equation was all r≥0.999. The average recoveries of this method ranged from 85.6% to 110.3% with RSDs ranging from 1.24% to 6.10%. It shows that this method has the advantages of high sensitivity, low detection limit, convenient operation and accurate result. It is suitable for the simultaneous determination of seven kinds of volatile halogenated hydrocarbons in water.