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液液萃取气相色谱法同时测定饮用水中的11种卤代酸 被引量:1

Determination of eleven halogenated acids in drinking water by liquid-liquid extraction and gas chromatography with electron capture detector
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摘要 目的建立液液萃取气相色谱法测定饮用水和水源水中9种卤代乙酸和2种除草剂共11种卤代酸的方法。方法采用甲基叔丁基醚为萃取溶剂,1,2-二溴丙烷为内标溶剂,在酸性条件下加氯化钠萃取水中的卤代酸。取甲基叔丁基醚层加入硫酸酸化的甲醇溶液,在酸性条件下,50℃酯化反应1 h,采用气相色谱法进行检测。结果方法的线性范围为2.0μg/L^100.0μg/L,线性相关系数为0.999 0~0.999 9,检出限为0.09μg/L^0.65μg/L;在2.0μg/L、20.0μg/L、100.0μg/L 3个添加水平范围内的平均加标回收率分别为83.5%~106.2%、89.0%~104.1%、87.1%~99.3%;相对标准偏差(RSD)为0.36%~6.23%。结论该方法在测定饮用水和水源水中的11种卤代酸时,具有操作简单、干扰少、快速、准确可靠等特点,适合用于居民生活饮用水和水源水的日常监控。 Objective A method was established for rapid determination of the eleven halogenated acids( nine haloacetic acids and two herbicides) in drinking waters by liquid - liquid extraction and gas chromatography with electron capture detector. Methods Methyl tert - butyl ether and 1,2 - dibromide propane were used as extraction solvent and an internal standard, re- spectively. Under acidic conditions, the esterification reaction was conducted for 1 h at 50 ℃ in acidic conditions. The obtained product was detected by gas chromatography. Results The calibration curves of eleven halogenated acids showed good linearity in the range of 2.0 μg/L - 100.0 μg/L with the correlation coefficient in the range of 0. 999 0 -0. 999 9. The detection limit of the method was from 0.09μg/L to 0.65 μg/L. The spiked at three levels ranged 83.5% - 106.2% (2.0μg/L), 89.0% - 104.1%(20.0 μg/L) and87.1% -99.3%(100.0 μg/L), andRSDwasO. 36% -6.23%. Conclusion The method for determination of eleven halogenated acids in drinking water and source water by gas chromatography with electron capture detec- tor was of operation convenience, less interference from impurities and good accuracy, which could used in monitoring quality of drinking water and source water.
出处 《中国卫生检验杂志》 CAS 2015年第9期1332-1335,1356,共5页 Chinese Journal of Health Laboratory Technology
关键词 卤代酸 除草剂 液液萃取 气相色谱法 饮用水 Haloacetic acids Herbicides Liquid - liquid extraction Gas chromatography Drinking water
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