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采用中空纤维液相微萃取技术在电热原子吸收光谱法测定前对环境样品中无机碲和硒的超痕量同时形态分析和预浓缩。

Simultaneous speciation and preconcentration of ultra traces of inorganic tellurium and selenium in environmental samples by hollow fiber liquid phase microextraction prior to electrothermal atomic absorption spectroscopy determination.

机构信息

Department of Chemistry, Faculty of Science, Shahid Beheshti University, Tehran, Iran.

出版信息

J Hazard Mater. 2010 Sep 15;181(1-3):491-6. doi: 10.1016/j.jhazmat.2010.05.040. Epub 2010 May 13.

Abstract

A simple and effective speciation and preconcentration method based on hollow fiber liquid phase microextraction (HF-LPME) was developed for simultaneous separation of trace inorganic tellurium and selenium in environmental samples prior to electrothermal atomic absorption spectroscopy (ETAAS) determination. The method involves the selective extraction of the Te (IV) and Se (IV) species by HF-LPME with the use of ammonium pyrrolidinecarbodithioate (APDC) as the chelating agent. The complex compounds were extracted into 10 microL of toluene and the solutions were injected into a graphite furnace for the determination of Te (IV) and Se (IV). To determine the total tellurium and selenium in the samples, first Te (VI) and Se (VI) were reduced to Te (IV) and Se (IV), and then the microextraction method was performed. The experimental parameters of HF-LPME were optimized using a central composite design after a 2(n-1) fractional factorial experimental design. Under optimum conditions, enrichment factors of up to 520 and 480 were achieved for Te (IV) and Se (IV), respectively. The detection limits were 4 ng L(-1) with 3.5% RSD (n=5, c=2.0 microg L(-1)) for Te (IV) and 5 ng L(-1) with 3.1% RSD for Se (IV). The applicability of the developed technique was evaluated by application to spiked, environmental water and soil samples.

摘要

基于中空纤维液相微萃取(HF-LPME)的简单、有效的形态分析和预浓缩方法,用于在电热原子吸收光谱法(ETAAS)测定之前,从环境样品中同时分离痕量无机碲和硒。该方法涉及使用氨丙基二硫代氨基甲酸盐(APDC)作为螯合剂,通过 HF-LPME 选择性萃取 Te(IV)和 Se(IV)物种。将配合物萃取到 10μL 甲苯中,并将溶液注入石墨炉中测定 Te(IV)和 Se(IV)。为了测定样品中的总碲和硒,首先将 Te(VI)和 Se(VI)还原为 Te(IV)和 Se(IV),然后进行微萃取方法。在 2(n-1)分数阶实验设计之后,使用中心复合设计优化 HF-LPME 的实验参数。在最佳条件下,Te(IV)和 Se(IV)的富集因子分别高达 520 和 480。Te(IV)的检测限为 4ng L(-1),相对标准偏差为 3.5%(n=5,c=2.0μg L(-1)),Se(IV)的检测限为 5ng L(-1),相对标准偏差为 3.1%。通过对加标、环境水和土壤样品的应用评估了所开发技术的适用性。

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