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目的建立同时测定生活饮用水中二氯甲烷、三氯甲烷、1,1,1-三氯乙烷、1,2-二氯乙烷、四氯化碳、三溴甲烷6种卤代烃的顶空毛细管气相色谱方法。方法采用顶空自动进样,平衡温度为50℃,平衡时间为50 min,DB-5毛细管色谱柱(60 m×0.25 mm,0.25μm)分离,柱温35℃保持10 min,程序升温至150℃,进样口温度为200℃,分流比为20∶1,ECD检测器温度为300℃,柱流速为1.0 ml/min,进样量为1.0 ml。结果 6种卤代烃能较好地分离,在0μg/L~300μg/L时,线性相关系数在0.999 0以上,峰面积与其浓度均具有良好的线性关系;检出限为0.003μg/L~5.60μg/L;相对标准偏差为1.98%~3.37%;平均加标回收率为96.4%~101.5%。结论该方法灵敏度高,操作简便,可同时测定生活饮用水中多种挥发性卤代烃,改进了国标方法中不能同时测定的不足,提高了工作效率,能够满足日常检测的要求。
OBJECTIVE To establish a method for the simultaneous determination of six topical halocarbons in dichloromethane, trichloromethane, 1,1,1-trichloroethane, 1,2-dichloroethane, carbon tetrachloride and tribromomethane in drinking water Empty capillary gas chromatography method. Methods The headspace autosampler was used. The equilibrium temperature was 50 ℃ and the equilibration time was 50 min. The separation was performed on a DB-5 capillary column (60 m × 0.25 mm, 0.25 μm). The column temperature was maintained at 35 ℃ for 10 min. The temperature was raised to 150 ° C, the inlet temperature was 200 ° C, the split ratio was 20: 1, the ECD detector temperature was 300 ° C, the column flow rate was 1.0 ml / min and the injection volume was 1.0 ml. Results The six halohydrocarbons could be well separated. The linear correlation coefficient was above 0.999 0 at 0μg / L ~ 300μg / L with a good linear relationship between the peak area and the concentration. The detection limit was 0.003μg / L ~ 5.60 μg / L; the relative standard deviations were 1.98% -3.37%; the average recoveries were 96.4% -101.5%. Conclusion The method is sensitive, easy to operate and can be used for the simultaneous determination of many volatile halohydrocarbons in drinking water. It can improve the efficiency of the method and meet the requirements of routine testing.