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碳纳米管作为一种固相吸附剂用于铬、锰、铁、钴、镍、铜、锌和铅的预富集,然后进行波长色散 X 射线荧光光谱分析。

Carbon nanotubes as a solid sorbent for the preconcentration of Cr, Mn, Fe, Co, Ni, Cu, Zn and Pb prior to wavelength-dispersive X-ray fluorescence spectrometry.

机构信息

Institute of Chemistry, University of Silesia, Szkolna 9, 40-006 Katowice, Poland.

出版信息

Talanta. 2012 Sep 15;99:918-23. doi: 10.1016/j.talanta.2012.07.059. Epub 2012 Jul 31.

Abstract

The preconcentration of trace elements on multiwalled carbon nanotubes (MWCNTs) followed by a wavelength-dispersive X-ray fluorescence analysis (WDXRF) has been investigated. The proposed preconcentration procedure is based on the sorption of trace elements on MWCNTs dispersed in analyzed solution. After sorption, the MWCNTs with the metal ions were collected onto the filter, and then the preconcentrated elements were determined directly by WDXRF. The preconcentration method was optimized, and in consequence, in order to obtain satisfactory recoveries using 100 mL of samples, the sorption process was performed with 1mg of MWCNTs within 5 min. Some conditions of the preconcentration process such as the pH of analyte solution, amounts of MWCNTs, the volume of the sample, the contact time between analytes and MWCNTs (stirring time), and the effects of foreign metals are discussed in detail in the paper. Adsorption onto raw and oxidized MWCNTs was also studied. The proposed procedure allows obtaining the detection limits of 0.6, 0.6, 1.0, 0.7, 0.6, 0.5, 0.9 and 1.9 ng mL(-1) for Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and Pb(II), respectively. The recoveries of determined elements were about 100%. Because the analytes are not eluted from the sorbent before WDXRF analysis, the risk of contamination and loss of analytes is reduced to minimum. Moreover, because the samples are analyzed as a thin layer, the matrix effects can be neglected. The proposed preconcentration method using MWCNTs coupled with WDXRF spectrometry was successfully applied to determine trace elements in natural water samples.

摘要

本文研究了将微量元素预富集在多壁碳纳米管(MWCNTs)上,然后用波长色散 X 射线荧光分析(WDXRF)进行分析。该预浓缩程序基于分散在分析溶液中的 MWCNTs 对微量元素的吸附。吸附后,将带有金属离子的 MWCNTs 收集在过滤器上,然后直接用 WDXRF 测定预浓缩元素。对预浓缩方法进行了优化,结果表明,为了使用 100 mL 样品获得满意的回收率,在 5 分钟内用 1mg 的 MWCNTs 进行吸附过程。本文详细讨论了预浓缩过程的一些条件,如分析物溶液的 pH 值、MWCNTs 的用量、样品的体积、分析物与 MWCNTs 之间的接触时间(搅拌时间)以及外来金属的影响。还研究了原始和氧化 MWCNTs 上的吸附。该方法允许获得 Cr(III)、Mn(II)、Fe(III)、Co(II)、Ni(II)、Cu(II)、Zn(II)和 Pb(II)的检测限分别为 0.6、0.6、1.0、0.7、0.6、0.5、0.9 和 1.9ng mL(-1)。测定元素的回收率约为 100%。由于在 WDXRF 分析之前,分析物不会从吸附剂上洗脱出来,因此可以将分析物的污染和损失风险降至最低。此外,由于样品以薄层形式进行分析,可以忽略基质效应。使用 MWCNTs 与 WDXRF 光谱法相结合的预浓缩方法成功地应用于天然水样中痕量元素的测定。

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