气相色谱法测定不同水质中的二氯乙酸和三氯乙酸
GC Determination of Dichloroacetic Acid and Trichloroacetic Acid in Different Water
摘 要
采用气相色谱法测定水中二氯乙酸和三氯乙酸的含量。并且检测了地表水、海水、污水处理厂进口和化工废水等不同水质实际样品。水样中加入氯化钠,经硫酸酸化,甲基叔丁基醚萃取后,以硫酸-甲醇(20+80)溶液作为衍生试剂,衍生温度为50 ℃时,气相色谱-电子捕获检测器测定。在优化分离条件下,分流比为5比1,二氯乙酸和三氯乙酸具有良好的分离效果。二氯乙酸、三氯乙酸的检出限分别为0.21,0.14 μg·L-1,加标回收率在97.4%~105%之间,测定值的相对标准偏差(n=6)小于6%。
二氯乙酸
三氯乙酸
水
GC
Dichloroacetic acid
Trichloroacetic acid
Water
Abstract
Dichloroacetic acid and trichloroacetic acid in different water samples, such as surface water, sea water, sewage treatment plant influent and chemical waste water, were quantitated by GC. Sodium chloride was added to water samples then the samples were acidified by sulfuric acid, followed by extraction using methyl tert-butyl ether the mixture of sulfuric acid and methanol (20+80) was used as derivatization reagent at 50 ℃, and derivatization with methyl alcohol before determined using GC-ECD. Good separation of dichloroacetic acid and trichloroacetic acid was obtained with split ratio of 5∶1 under optimal condition. Detection limits of dichloroacetic acid and trichloroacetic acid were 0.21 μg·L-1 and 0.14 μg·L-1 respectively. Values of recovery found standard addition method were in the range of 97.4%-105%, with RSD (n=6) less than 6%.
中图分类号 O657.7 X832
所属栏目 工作简报
基金项目
收稿日期 2013/10/30
修改稿日期
网络出版日期
作者单位点击查看
备注肖洋(1982-),男,山东淄博人,工程师,博士,主要从事环境监测分析工作。
引用该论文: XIAO Yang,WANG Xin-juan,HAN Wei. GC Determination of Dichloroacetic Acid and Trichloroacetic Acid in Different Water[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(8): 979～982
肖洋,王新娟,韩伟. 气相色谱法测定不同水质中的二氯乙酸和三氯乙酸[J]. 理化检验－化学分册, 2014, 50(8): 979～982
共有人对该论文发表了看法，其中：
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】童小萍,冀元堂.氯化消毒饮用水与生殖发育毒性关系的研究进展［J］.卫生毒理学杂志, 2003,17(3):185-187.
【2】张子秋,罗茜,王东红,等.饮用水中9种卤乙酸的同时测定方法［J］.环境化学, 2011,30(2):500-505.
【3】GB/T 5750.10-2006生活饮用水标准检验方法 消毒副产物指标［S］.
【4】周学永.法扬司法在氯乙酸分析中的应用［J］.化学工程师, 1992(2):25-26.
【5】CARDADOR M J, SERRANO A, GALLEGO M. Simultaneous liquid-liquid microextraction/methylation for the determination of haloacetic acids in drinking waters by headspace gas chromatography［J］. Journal of Chromatography A, 2008,1209(1/2):61-69.
【6】汪昆平,邓荣森,李伟民.气相色谱-质谱法测定饮用水中的卤乙酸［J］.色谱, 2006,24(1):26-29.
【7】BRUZZONITI M C, DE CARLO R M, HORVATH K, et al. High performance ion chromatography of haloacetic acids on macrocyclic cryptand anion exchanger［J］. Journal of Chromatography A, 2008,1187(2):188-196.
【8】齐剑英,吴颖娟,张平,等.离子色谱法测定饮用水中二氯乙酸和三氯乙酸［J］.理化检验-化学分册, 2007,43(11):947-949.
【9】李金燕,李晓玲.反相液相色谱/电喷雾质谱法分离水体中6种卤乙酸［J］.中国给水排水, 2007,23(16):81-84.
【10】MENG Li-ping, WU Shi-min, MA Fu-jun, et al. Trace determination of nine haloacetic acids in drinking water by liquid chromatography-electrospray tandem mass spectrometry［J］. Journal of Chromatography A, 2010,1217(29):4873-4876.
【11】刘肖,史亚利,王碗,等.离子色谱-串联电喷雾质谱法检测自来水中二氯乙酸和三氯乙酸［J］.分析化学, 2007,35(2):221-226.
【12】阮小林,黄汉林,越飞,等.衍生化气相色谱法同时测定尿中三氯乙烯的3种氯代乙酸代谢产物［J］.分析测试学报, 2013,32(3):377-380.
【13】LI Xin, REN Yue-ming, QIANG Liang-sheng, et al. Researches on formation of haloacetic acids in chlorination of drinking water by a novel technique［J］. Chemical Research in Chinese Universities, 2004,20(3):285-288.
【2】张子秋,罗茜,王东红,等.饮用水中9种卤乙酸的同时测定方法［J］.环境化学, 2011,30(2):500-505.
【3】GB/T 5750.10-2006生活饮用水标准检验方法 消毒副产物指标［S］.
【4】周学永.法扬司法在氯乙酸分析中的应用［J］.化学工程师, 1992(2):25-26.
【5】CARDADOR M J, SERRANO A, GALLEGO M. Simultaneous liquid-liquid microextraction/methylation for the determination of haloacetic acids in drinking waters by headspace gas chromatography［J］. Journal of Chromatography A, 2008,1209(1/2):61-69.
【6】汪昆平,邓荣森,李伟民.气相色谱-质谱法测定饮用水中的卤乙酸［J］.色谱, 2006,24(1):26-29.
【7】BRUZZONITI M C, DE CARLO R M, HORVATH K, et al. High performance ion chromatography of haloacetic acids on macrocyclic cryptand anion exchanger［J］. Journal of Chromatography A, 2008,1187(2):188-196.
【8】齐剑英,吴颖娟,张平,等.离子色谱法测定饮用水中二氯乙酸和三氯乙酸［J］.理化检验-化学分册, 2007,43(11):947-949.
【9】李金燕,李晓玲.反相液相色谱/电喷雾质谱法分离水体中6种卤乙酸［J］.中国给水排水, 2007,23(16):81-84.
【10】MENG Li-ping, WU Shi-min, MA Fu-jun, et al. Trace determination of nine haloacetic acids in drinking water by liquid chromatography-electrospray tandem mass spectrometry［J］. Journal of Chromatography A, 2010,1217(29):4873-4876.
【11】刘肖,史亚利,王碗,等.离子色谱-串联电喷雾质谱法检测自来水中二氯乙酸和三氯乙酸［J］.分析化学, 2007,35(2):221-226.
【12】阮小林,黄汉林,越飞,等.衍生化气相色谱法同时测定尿中三氯乙烯的3种氯代乙酸代谢产物［J］.分析测试学报, 2013,32(3):377-380.
【13】LI Xin, REN Yue-ming, QIANG Liang-sheng, et al. Researches on formation of haloacetic acids in chlorination of drinking water by a novel technique［J］. Chemical Research in Chinese Universities, 2004,20(3):285-288.
相关信息
