HPLC-HG-AFS测定大气颗粒物中砷的形态  

Determination of arsenic speciation in atmospheric particles by HPLC-HG-AFS

作　　者：龚仓[1] 徐殿斗[2] 马玲玲[2] 贺婷婷[2] 杨国胜[2] 李柏[2] 

机构地区：[1]武警黄金第十二支队化验室,成都611732 [2]中国科学院高能物理研究所核技术应用研究中心,核分析技术重点实验室,北京100049

出　　处：《分析试验室》2014年第6期664-667,共4页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(11075171;11275216;11375212);中国地质调查局专项(12120113002400)资助

摘　　要：采用高效液相色谱-氢化物发生原子荧光光谱联用测定了北京大气颗粒物中As（Ⅲ）,As（Ⅴ）,二甲基砷酸（DMA）和一甲基砷酸（MMA）的含量。研究了仪器条件、流动相组成和梯度洗脱程序对砷形态分离的影响。实验结果显示,在优化的色谱与氢化原子荧光检测条件下,采用pH6.0,浓度为10 mmol/L和200 mmol/L NH4H2PO4为流动相A和B,在1～3 min内用60%的A和40%的B洗脱使砷的4种形态达到最佳分离效。As（Ⅲ）,As（Ⅴ）,DMA和MMA的检出限为1.45,1.22,1.91和1.64 mg/L,回收率为90.5%～93.2%,相对标准偏差为0.38%～1.7%。方法适用于大气颗粒物中砷的形态分析研究。A method for analyzing the contents of As （Ⅲ ）, As （ V ）, dimethylarsinic acid （ DMA ） and monomethylarsonic acid （MMA） in atmospheric particulates in Beijing by high-performance liquid chromatography coupled with hydride generation and atomic fluorescence spectrometry （HPLC-HG-AFS） was developed. Various effects of the instrument settings, mobile phase constitution and gradient elution on the separation of arsenic species were investigated. The experimental results showed that the optimal conditions for separating of arsenic species are the mobile phase composed of A 10 mmol/L NH4H2PO4 （pH 6.0） and B 200 mmol/L NH4H2PO4 （pH6.0） , and the gradient elution conditions are mobile phase A 60% and mobile phase B 40% in 1 -3 min. The detection limits of As（Ⅲ）, As（V）, DMA and MMA are 1.45, 1.22, 1.91 and 1.64 mg/L. The recoveries and RSD are 90.5% -93.2% and 0.38% - 1.7%, respectively. This method is characterized by its sensitivity, high accuracy and simple operation, and it is suitable for speciation analysis of arsenic in atmospheric particulates.

关 键 词：HPLC-HG-AFS 大气颗粒物 砷 形态 环境污染物 

分 类 号：O657.5[理学—分析化学] O657.3[理学—化学]