超声萃取-冷蒸气-原子荧光光谱法测定沉积物和土壤样品中甲基汞
CV-AFS Determination of Methyl Mercury in Sediment and Soil Samples with Ultrasonic Extraction
摘 要
样品中甲基汞用6 mol·L-1盐酸超声提取2 h,离心分离后,上层清液用二氯甲烷萃取.取出有机相,加适量去离子水,于60 ℃吹氮赶去二氯甲烷,甲基汞保留在水相中.水溶液用9 mol·L-1硫酸酸化后,加入溴化钾和溴酸钾混合溶液将甲基汞转化为无机汞离子,并用冷蒸气-原子荧光光谱法测定其含量.方法的检出限(3S/N)为0.1 pg·g-1,所提出的方法用于土壤及沉积物样品中甲基汞的测定,测定结果的相对标准偏差(n=6)均小于5%.用标准加入法测定了方法的回收率,结果达93.6%.
超声提取
沉积物
土壤
甲基汞
Cold vapour-atomic fluorescence spectrometry
Ultrasonic extraction
Sediment
Soil
Methyl mercury
Abstract
Methyl mercury in the sample was extracted ultrasonically with 6 mol·L-1 HCl for 2 h.After centrifugation,the supernatant extract was extracted with dichloromethane.The organic phase was taken and de-ionized water was added.Dichloromethane was expelled by evaporation with N2-blowing at 60 ℃ and methyl mercury was retained in the water phase.The water solution was acidified with 9 mol·L-1 H2SO4 and treated with mixed solution of KBrO3 and KBr to transform the methyl mercury into inorganic mercury ion,which was determined by CV-AFS.Detection limit (3S/N) of the method found was 0.1 pg·g-1.The proposed method was used in determination of methyl mercury in samples of soil and sediment,giving values of RSD′s (n=6) less than 5%.Average recovery found by standard addition method attained to a value of 93.6%.
中图分类号 O657.31
所属栏目 工作简报
基金项目 中国科学院知识创新工程重要方向项目(KZCX3-SW-437)
收稿日期 2008/11/3
修改稿日期
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备注张少庆(1980-),男,烟台人,硕士研究生,主要研究方向为污染物环境行为及其控制研究.
引用该论文: ZHANG Shao-qing,WANG Qi-chao,CUI Jun-tao,SUN Xiao-jing,ZHENG Dong-mei. CV-AFS Determination of Methyl Mercury in Sediment and Soil Samples with Ultrasonic Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(11): 1273～1275
张少庆,王起超,崔俊涛,孙晓静,郑冬梅. 超声萃取-冷蒸气-原子荧光光谱法测定沉积物和土壤样品中甲基汞[J]. 理化检验－化学分册, 2009, 45(11): 1273～1275
被引情况:
【1】刘稚,张庆建,丁仕兵,郭兵,李晨,闵国华,孙瑞昌, "固体进样测汞仪测定矿物中汞",理化检验－化学分册 49, 1512-1513(2013)
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参考文献
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【3】FALTER R,SCHOLER H F.A new pyrrolidinedithiocarbamate screening method for the determination of methylmercury and inorganic mercury relation in hair samples by HPLC-UV-PCO-CVAAS[J].Anal Chem,1996,354:492．
【4】LIANG L,HORVAT M,BLOOM N S.An improved speciation method for mercury by GC/CVAFS after aqueous phase ethylation and room temperature precollection[J].Talanta,1994,41(3):371．
【5】TU Q,QIAN J,FRECH W J.Rapid determination of methylmercury in biological materials by GC-MIP-AES or GC-ICP-MS following simultaneous ultrasonic-assisted in situ ethylation and solvent extraction[J].Anal At Spectrom,2000,15:1583．
【6】牟仁祥,陈铭学,朱智伟,等.微波消解-氢化物发生-原子荧光光谱法测定大米中痕量汞[J].光谱学与光谱分析,2004,24(2):236-237．
【7】仇广乐,冯新斌,梁琏,等.溶剂萃取-水相乙基化衍生GC-CVAFS联用测定苔藓样品中的甲基汞[J].分析测试学报,2005,24(1):29．
【8】EIDEN R,FALTER R,AGUSTIN-CASTRO B,et al.Distillation,on-line RP C18 preconcentration and HPLC-UV-PCO-CVAAS as a new combination for the determination of methylmercury in sediments and fish tissue Fresenius[J].Fresenius J Anal Chem,1997,357:439．
【9】ENTEBORG H,BJORKLUND E,ODMAN F,et al.Determination of methylmercury in sediments using supercritical fluid extraction and gas chromatography coupled with microwave-induced plasma atomic emission spectrometry[J].Analyst,1996,121(1):19．
【10】LOGAR M,HORVAT M,FALNOGA I,et al.Influence of the Sostanj coal-fired thermal power plant on mercury and methyl mercury concentrations in lake velenje,slovenia fresenius[J].Anal Chem,2000,366:453．
【11】孙瑾,陈春英,李玉锋,等.超声波辅助溶剂萃取-电感耦合等离子体质谱法测定生物样品中的总汞和甲基汞[J].光谱学与学谱分析,2007,27(1):173-176．
【12】国家环境保护局.水和废水监测分析方法[M].北京:中国环境科学出版社,1989:169．
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