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氧化铌-二氧化硅在用于火焰原子吸收光谱法测定铜和镉的自动化在线预富集系统中的应用。

Use of Nb(2)O(5)-SiO(2) in an automated on-line preconcentration system for determination of copper and cadmium by FAAS.

作者信息

da Silva Edson Luiz, Ganzarolli Edgard Moreira, Carasek Eduardo

机构信息

Departamento de Quimica, Universidade Federal de Santa Catarina, Florianópolis, SC 88040-900, Brazil.

出版信息

Talanta. 2004 Mar 10;62(4):727-33. doi: 10.1016/j.talanta.2003.09.014.

Abstract

A procedure for the determination of trace level of copper(II) and cadmium(II) by FAAS using an on-line preconcentration system has been proposed. In this system, copper and cadmium ions were adsorbed onto a minicolumn packed with silica gel modified with niobium(V) oxide (Nb(2)O(5)-SiO(2)), followed by nitric acid elution in reverse mode and determination on-line by flame atomic absorption spectrometry (AAS) without interference of the matrix. Chemical and flow variables as well as concomitant ions were studied in the developed procedure. The enrichment factor for copper(II) and cadmium(II) was 34.2 and 33.0, respectively, using a preconcentration time of 2min. The limit of detection for copper(II) and cadmium(II) was 0.4, and 0.1mugl(-1), respectively. The precision of the method, evaluated as the relative standard deviation in solutions containing 15mugl(-1) of copper and 10mugl(-1) of cadmium, by analyzing a series of seven replicates, was 1.8 and 1.6%, respectively. The accuracy was assessed through recovery experiments of certified material and water samples.

摘要

提出了一种使用在线预富集系统通过火焰原子吸收光谱法(FAAS)测定痕量铜(II)和镉(II)的方法。在该系统中,铜离子和镉离子被吸附到填充有经五氧化二铌(Nb₂O₅-SiO₂)改性的硅胶的微型柱上,然后用硝酸以反向模式洗脱,并通过火焰原子吸收光谱法(AAS)在线测定,不受基质干扰。对所开发方法中的化学和流量变量以及共存离子进行了研究。使用2分钟的预富集时间时,铜(II)和镉(II)的富集因子分别为34.2和33.0。铜(II)和镉(II)的检测限分别为0.4和0.1μg l⁻¹。通过分析一系列七个重复样,在含有15μg l⁻¹铜和10μg l⁻¹镉的溶液中评估该方法的精密度,相对标准偏差分别为1.8%和1.6%。通过对有证标准物质和水样的加标回收实验评估了准确度。

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