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采用微波辅助萃取-高效液相色谱-氢化物发生原子荧光光谱法分析煤样中的无机砷形态。

Speciation analysis of inorganic arsenic in coal samples by microwave-assisted extraction and high performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry.

机构信息

CAS Key Laboratory of Crust-Mantle Materials and Environment, School of Earth and Space Sciences, University of Science and Technology of China, Hefei, Anhui 230026, China.

出版信息

Talanta. 2013 Mar 15;106:8-13. doi: 10.1016/j.talanta.2012.12.012. Epub 2012 Dec 14.

DOI:10.1016/j.talanta.2012.12.012
PMID:23598089
Abstract

A new method was developed for the speciation analysis of inorganic arsenic in coal samples by high performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry after microwave-assisted extraction. Effective extract of As(III) and As(V) in coal sample was achieved by 1.0 mol L(-1)H₃PO₄ and 0.1 mol L(-1)ascorbic acid. Under the optimized conditions, the limits of detection (LOD) were 0.01 μg L(-1) and 0.02 μg L(-1), the relative standard deviations (RSD) were 2.4% and 3.3% (c=10.0 μg L(-1), n=7), recoveries were 102.5% and 96.5% for As(III) and As(V). The proposed method was successfully applied for the determination of speciation of inorganic arsenic in coal samples and GBW11117 coal standard reference material with complex matrix.

摘要

建立了微波辅助萃取-高效液相色谱-氢化物发生原子荧光光谱法测定煤中无机砷形态的分析方法。在 1.0 mol·L(-1)H₃PO₄-0.1 mol·L(-1)抗坏血酸体系中实现了煤样中 As(III)和 As(V)的有效提取。在优化条件下,方法的检出限分别为 0.01 μg·L(-1)和 0.02 μg·L(-1),相对标准偏差分别为 2.4%和 3.3%(c=10.0 μg·L(-1),n=7),加标回收率分别为 102.5%和 96.5%。该方法成功地应用于复杂基体煤样品和 GBW11117 煤标准物质中无机砷形态的测定。

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