氢化物发生-原子荧光光谱法直接测定土壤水溶态Sb(Ⅲ)和Sb(Ⅴ)

doi:10.3964/j.issn.1000-0593(2009)12-3405-04

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摘要：在HCl介质中，Sb(Ⅲ)和Sb(Ⅴ)在氢化物发生过程中的化学反应效率不同，通过测定经还原剂还原后和还原前Sb的荧光强度，求解联立方程计算出Sb(Ⅲ)和Sb(Ⅴ)的含量，据此建立了氢化物发生-原子荧光光谱法直接测定土壤水溶态Sb(Ⅲ)和Sb(Ⅴ)方法，操作简便，实用性强。考察了HCl浓度和KBH₄浓度对Sb(Ⅲ)和Sb(Ⅴ)测定灵敏度的影响以及共存元素的干扰情况，并比较了两种还原剂对Sb(Ⅴ)的还原效果。方法检出限为Sb(Ⅲ)1.11 ng·g^-1 ，Sb(Ⅴ)1.57 ng·g^-1。加标回收试验表明方法准确、可靠。

关键词：氢化物发生;原子荧光光谱法;Sb(Ⅲ);Sb(Ⅴ);土壤

Abstract：A simple, rapid and useful method for the determination of water-soluble antimony(Ⅲ) and antimony(Ⅴ) in soil was established using hydride generation atomic fluorescence spectrometry. The method was based on the different chemical reaction efficiency between Sb(Ⅲ) and Sb(Ⅴ) with KBH₄ in the media of HCl. The amounts of Sb(Ⅲ) and Sb(Ⅴ) can be obtained through measuring antimony fluorescence intensities before and after reduction with reductant. The effects of HCl and KBH₄ on the sensitivities of Sb(Ⅲ) and Sb(Ⅴ) were investigated, and the interferences from coexistent elements were studied. The reduction efficiencies of both reductants were compared. The detection limits of the method were 1.11 ng·g^-1 for Sb(Ⅲ) and 1.57 ng·g^-1 for Sb(Ⅴ). The accuracy of the method was verified by recovery experiments on spiked real soil samples.

Key words：Hydride generation;Atomic fluorescence spectrometry;Sb(Ⅲ);Sb(Ⅴ);Soil

收稿日期: 2008-11-08 修订日期: 2009-02-12

中图分类号:

O657.3

通讯作者: 于兆水 E-mail: yzs2006@163.com

引用本文:

于兆水，张勤. 氢化物发生-原子荧光光谱法直接测定土壤水溶态Sb(Ⅲ)和Sb(Ⅴ)[J]. 光谱学与光谱分析, 2009, 29(12): 3405-3408.
YU Zhao-shui,ZHANG Qin. Direct Determination of Water-Soluble Antimony(Ⅲ) and Antimony(Ⅴ) in Soil by Hydride Generation Atomic Fluorescence Spectrometry . SPECTROSCOPY AND SPECTRAL ANALYSIS, 2009, 29(12): 3405-3408.

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