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目的探讨生活饮用水中二氯甲烷、1,1-二氯乙烷及1,2-二氯乙烷的顶空气相色谱(HS-GC)测定方法。方法水中的微量二氯甲烷、1,1-二氯乙烷及1,2-二氯乙烷经顶空提取后,用DB-624毛细管色谱柱,采用程序升温方式进行分析,采用ECD作为检测器,以保留时间定性,外标法定量。结果二氯甲烷的线性范围为1.5μg/L~244μg/L;1,1-二氯乙烷的线性范围为5.0μg/L~216μg/L;1,2-二氯乙烷的线性范围为1.7μg/L~414μg/L,二氯甲烷、1,1-二氯乙烷和1,2-二氯乙烷最低检出浓度分别为0.5μg/L、1.7μg/L和0.6μg/L,二氯甲烷回收率范围为95.1%~107%,RSD为3.9%;1,1-二氯乙烷回收率范围为91.3%~111%,RSD为4.9%;1,2-二氯乙烷回收率范围为99.5%~103%,RSD为2.3%。结论该方法具有准确度高、选择性好、检出限低、线性范围宽等特点,满足生活饮用水中二氯甲烷、1,1-二氯乙烷及1,2-二氯乙烷的定量分离测定。
Objective To investigate the determination of dichloromethane, 1,1-dichloroethane and 1,2-dichloroethane in domestic drinking water by headspace gas chromatography (HS-GC). Methods Dichloromethane, 1,1-dichloroethane and 1,2-dichloroethane in water were extracted by headspace and analyzed by DB-624 capillary column with programmed temperature increasing method. ECD was used as detection To qualitative retention time, external standard method. Results The linear range of dichloromethane was 1.5μg / L ~ 244μg / L; the linear range of 1,1-dichloroethane was 5.0μg / L ~ 216μg / L; the linear range of 1,2-dichloroethane was 1.7μg / L ~ 414μg / L, dichloromethane, 1,1-dichloroethane and 1,2-dichloroethane were 0.5μg / L, 1.7μg / L and 0.6μg / L , The recoveries of dichloromethane ranged from 95.1% to 107%, RSD was 3.9%, the recoveries of 1,1-dichloroethane ranged from 91.3% to 111% with a RSD of 4.9%. 1,2-Dichloroethane The recoveries ranged from 99.5% to 103% with a RSD of 2.3%. Conclusion The method has the characteristics of high accuracy, good selectivity, low detection limit and wide linear range, which meets the requirements of dichloromethane, 1,1-dichloroethane and 1,2-dichloroethane in drinking water Quantitative separation assay.