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目的建立饮用水中氯仿(CHCl3)和四氯化碳(CCl4)的顶空固相微萃取(HS-SPME)-气相色谱(GC)分析方法。方法样品经顶空固相微萃取后,进行毛细管柱气相色谱分析,优化后的分析条件为二乙烯基苯-碳分子筛-聚二甲基硅氧烷(DVB-CAR-PDMS,膜厚50μm)萃取头,吸附平衡时间为10min,解吸时间为3min,水浴温度为40℃,水浴平衡时间为60min。气化室温度为220℃,柱箱温度为40℃,检测器(ECD)温度为260℃,载气(氮气,N2)柱流量为3.5ml/min。结果氯仿的线性范围在1～10μg/L之间,所得回归方程为y=32567x-4489.3,相关系数为0.9997,检出限为0.024μg/L;四氯化碳的线性范围在0.1～1.0μg/L之间,所得回归方程为y=197521x-4096.4,相关系数为0.9995,检出限为0.0042μg/L。该方法所得的平均回收率为94.2%～108.0%,RSD为0.6%～2.4%。采用HS-SPME-GC法和国标法测定氯仿和四氯化碳的混合溶液,结果间差异无统计学意义。结论该方法具有操作简便,灵敏度高,结果准确的优点,适用于饮用水中氯仿和四氯化碳的测定。
Objective To establish a headspace solid-phase microextraction (HS-SPME) -chromatography (GC) method for the determination of chloroform (CHCl3) and carbon tetrachloride (CCl4) in drinking water. The sample was analyzed by capillary gas chromatography after headspace solid-phase microextraction. The optimized analytical conditions were DVB-CAR-PDMS (50μm film thickness) Extraction head, adsorption equilibrium time of 10min, desorption time of 3min, water bath temperature of 40 ℃, water bath balance time of 60min. Gasification chamber temperature was 220 ° C, oven temperature was 40 ° C, detector (ECD) temperature was 260 ° C, and carrier gas (N2, N2) flow was 3.5 ml / min. Results The linear range of chloroform was 1 ~ 10μg / L. The regression equation was y = 32567x-4489.3, the correlation coefficient was 0.9997, the detection limit was 0.024μg / L. The linear range of CCl_4 was 0.1 ~ 1.0μg / L, the regression equation was y = 197521x-4096.4, the correlation coefficient was 0.9995, the detection limit was 0.0042μg / L. The average recovery of the method was 94.2% ~ 108.0%, RSD was 0.6% ~ 2.4%. HS-SPME-GC method and the national standard method for the determination of chloroform and carbon tetrachloride mixed solution, the results showed no significant difference. Conclusion The method has the advantages of simple operation, high sensitivity and accurate results. It is suitable for the determination of chloroform and carbon tetrachloride in drinking water.