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汞(II)印迹硫醇功能化介孔吸附剂微柱对痕量汞的预富集及电感耦合等离子体发射光谱法测定

Hg(II)-imprinted thiol-functionalized mesoporous sorbent micro-column preconcentration of trace mercury and determination by inductively coupled plasma optical emission spectrometry.

作者信息

Fan Zhefeng

机构信息

Department of Chemistry, Shanxi Normal University, Linfen 041004, PR China.

出版信息

Talanta. 2006 Dec 15;70(5):1164-9. doi: 10.1016/j.talanta.2006.03.021. Epub 2006 Apr 18.

DOI:10.1016/j.talanta.2006.03.021
PMID:18970895
Abstract

Hg(II)-imprinting thiol-functionalized mesoporous sorbent was prepared by a sol-gel method and characterized by X-ray diffraction (XRD), FT-IR spectroscopy and nitrogen gas adsorption-desorption. The static adsorption capacity of the Hg(II)-imprinted and non-imprinted sorbent was 78.5 and 26.6mgg(-1), respectively. The breakthrough capacity was 4.46mgg(-1), and the relative selectivity coefficient for Hg(II) in the presence of Cd and Pb was 3.3 and 3.9, respectively. A new method using a micro-column packed with Hg(II)-imprinting thiol-functionalized mesoporous sorbent has been developed for preconcentration of trace mercury prior to its determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The effects of pH, sample flow rate and volume, elution solution and interfering ions on the recovery of the analyte have been investigated. The limit of detection was 0.39ngml(-1) with a concentration factor of 150 times. The developed method has been applied to the determination of trace mercury in some biological and environmental samples with satisfactory results. The accuracy was assessed through recovery experiments and analysis of certified reference material.

摘要

通过溶胶 - 凝胶法制备了汞(II)印迹硫醇功能化介孔吸附剂,并采用X射线衍射(XRD)、傅里叶变换红外光谱(FT - IR)和氮气吸附 - 脱附对其进行了表征。汞(II)印迹吸附剂和非印迹吸附剂的静态吸附容量分别为78.5和26.6mg g⁻¹。穿透容量为4.46mg g⁻¹,在镉和铅存在下汞(II)的相对选择性系数分别为3.3和3.9。开发了一种新方法,该方法使用填充有汞(II)印迹硫醇功能化介孔吸附剂的微柱,用于在通过电感耦合等离子体发射光谱法(ICP - OES)测定之前对痕量汞进行预富集。研究了pH值、样品流速和体积、洗脱液以及干扰离子对分析物回收率的影响。检测限为0.39ng ml⁻¹,浓缩因子为150倍。所开发的方法已应用于一些生物和环境样品中痕量汞的测定,结果令人满意。通过回收率实验和有证标准物质分析评估了准确性。

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