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使用流动系统和火焰原子吸收光谱法,利用化学固定在硅胶表面的锆(IV)和磷酸锆(IV)进行铬形态分析和预富集。

Chromium speciation and preconcentration using zirconium(IV) and zirconium(IV) phosphate chemically immobilized onto silica gel surface using a flow system and F AAS.

作者信息

Maltez Heloisa França, Carasek Eduardo

机构信息

Departamento de Química, Universidade Federal de Santa Catarina, Florianópolis 88040900, SC, Brazil.

出版信息

Talanta. 2005 Jan 30;65(2):537-42. doi: 10.1016/j.talanta.2004.07.017.

Abstract

A procedure for chromium speciation by F AAS using a flow system has been proposed. In this system, Cr(III) and Cr(VI) ions were adsorbed sequentially onto a mini-column packed with silica gel modified with zirconium phosphate and a mini-column packed with silica gel modified with zirconium oxide, respectively. The elution of Cr(III) and Cr(VI) was made with, respectively, nitric acid solution and tris(hydroxymethyl)methylamine (THAM) solution in reverse mode and determination by flame atomic absorption spectrometry without interference of the matrix. Chemical and flow variables as well as concomitant ions were studied in the developed procedure. The enrichment factor for Cr(III) and Cr(VI) was 20.8 and 24.9, respectively, using a preconcentration time of 3.75min. The limit of detection for Cr(III) and Cr(VI) was 1.9, and 2.3mugl(-1), respectively. The precision of the method, evaluated as the relative standard deviation in solutions containing 100mugl(-1) of chromium species, by analyzing a series of seven replicates, was lower than 3.0%. The accuracy was assessed through recovery experiments of water samples and using another methodology.

摘要

提出了一种使用流动系统通过火焰原子吸收光谱法进行铬形态分析的方法。在该系统中,Cr(III)和Cr(VI)离子分别依次吸附到填充有磷酸锆改性硅胶的微型柱和填充有氧化锆改性硅胶的微型柱上。Cr(III)和Cr(VI)分别用硝酸溶液和三(羟甲基)甲胺(THAM)溶液以反向模式洗脱,并通过火焰原子吸收光谱法测定,不受基质干扰。对所开发方法中的化学和流动变量以及共存离子进行了研究。使用3.75分钟的预浓缩时间,Cr(III)和Cr(VI)的富集因子分别为20.8和24.9。Cr(III)和Cr(VI)的检测限分别为1.9和2.3μg l⁻¹。通过分析一系列七个重复样品,在含有铬形态100μg l⁻¹的溶液中评估该方法的精密度,相对标准偏差低于3.0%。通过水样的回收率实验并使用另一种方法评估了准确性。

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