利用微波消解和高效液相色谱荧光检测法测定环境水样中痕量硒

摘　要：基于微波消解和正相液相色谱-荧光检测测硒法，实现了对环境水样中亚纳克级硒的测定。考察了HNO₃和H₂SO₄-H₂O₂两种消化体系及其工作条件，方法检出限分别可达7.2和10.4pgSe，对标准参考物质的回收率分别为99.4±2.0和97.8±2.5%，在0～1.5ngSe范围内有线性关系(r2＜0.996)。对北京地区4种不同类型水体水样含硒量进行了分析测定(2mL样品)，其浓度范围为0.20～0．90μg/L，标准加入回收率为99.1%～103.4%。

关键词：硒，微波消解，液相色谱，环境水样

分类号：065　文献标识码：A

Determination of Trace Selenium in Environmental Waters After Microwave Digestion and Fluorometric Determination with 2,3-Diamino-naphthalene

Gao Yuxi（State Key Laboratory of Environmental Aquatic Chemistry, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085）　
Wang Zijian（State Key Laboratory of Environmental Aquatic Chemistry, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085）　
Leng Chunhua（State Key Laboratory of Environmental Aquatic Chemistry, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085）　

Abstract：A new approach, combining microwave digestion and sensitive determination of selenium by a normal-phase high performance liquid chromatography after derivatization with 2,3-diamino-naphthalene was proposed to the measurements of trace selenium concentration in natural waters. Two digestions systems, i.e. HNO₃ and H₂SO₄-H₂O₂, were evaluated and their working conditions were optimized. Under optimal conditions, this approach provides a detection limit of 7.2 pg (with HNO₃）or 10.4 pg (with H₂SO₄-H₂O₂）, a recovery of 99.1%～103.4%, as well as a linear range of 0～1.5 ng Se(Ⅳ). The approach was applied to determine Se concentration in 4 different types of environmental waters (sample volume: 2 mL) and the concentration levels of 0.20～0．90 μg/L were found, with recoveries of 99.1%～103．4％ by standard addition.
Keywords：Selenium, microwave digestion, liquid chromatography, environmental waters

参考文献：

［1］Xu Huibi(徐辉碧), Huang Kaixun(黄开勋). Selenium: Its Chemistry, Biochemistry and Application in Life Science(硒的化学、生物化学及其在生命科学中的应用). Wuhan(武汉)： Huazhong University of Science and Technology Press(华中理工大学出版社), 1994, 80～86,268～273
［2］Peng An(彭安), Wang Zijian(王子健), Whanger P D, Combs G F, Yeh J Y. Environmental Bio-inorganic Chemistry of Selenium(硒的环境生物无机化学). Beijing(北京): China Environmental Science Press(中国环境科学出版社), 1995, 4～23
［3］Wang Zijian(王子健), Peng An(彭安). Chinese J. Anal. Chem.(分析化学), 1988, 16(7):644～646
［4］Haygarth H M, rowland Q P, Stürp S, Jones K C. Analyst, 1993, 118:1303～1308
［5］Chen Guozhen(陈国珍), Xu Jingou(许金钩), Huang Xianzhi(黄贤智). Fluorescence Analysis(荧光分析法).2nd ed.(第二版). Beijing(北京):Science Press(科学出版社), 1990, 432～433
［6］Lalonde L, Jean Y. Clin. Chem., 1982, 28:172～174
［7］Wang Zijian(王子健), Sun Jingfang(孙景芳). Acta Scientiae Ciecumstantiae(环境科学学报), 1988, 8(1):121～124
［8］Wang Zijian(王子健), Xie Shenmeng(谢申猛), Gao Yuxi(高愈希), Peng An(彭安). Chinese J. Anal. Chem.(分析化学), 1999, 27(10):1200～1203
［9］Wen X H, Wu L Z, Zhang Y, Chu Y. Fresenius′ J. Anal. Chem., 1997, 357:1111～1115
［10］Novozamsky I, Van de Lee H J, Houba V J G. Mikrochim. Acta, 1995, 119:183～189
［11］Welz B, Melcher M. Anal. Chim. Acta, 1984, 165:131
［12］Conde J E, Sanz Alaejos M. Chem. Rev., 1997, 97:1979～2003

收稿日期：2000年7月6日

修稿日期：2000年10月30日

出版日期：2001年6月1日