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微波辅助水相消解- 胶体金富集分离- 电感耦合等离子体原子发射光谱法测定地质样品中的痕量金

Microwave assisted aqua regia extraction of thallium from sediment and coal fly ash samples and interference free determination by continuum source ETAAS after cloud point extraction.

机构信息

National Center for Compositional Characterization of Materials, Bhabha Atomic Research Centre, ECIL Post, Hyderabad 500 062, India.

出版信息

Talanta. 2013 Jan 30;104:180-6. doi: 10.1016/j.talanta.2012.11.002. Epub 2012 Nov 10.

Abstract

A simple cloud point extraction method is described for the separation and pre-concentration of thallium from the microwave assisted aqua regia extracts of sediment and coal fly ash samples. The method is based on the formation of extractable species of thallium and its interaction with hydrophobic solubilizing sites of Triton X-114 micelles in the presence of aqua regia and electrolyte NaCl. These interactions of micelles are used for extraction of thallium from a bulk aqueous phase into a small micelles-rich phase. The potential chloride interferences are eliminated effectively, which enabled interference free determination of thallium from aqua regia extracts using continuum source ETAAS. The parameters affecting the extraction process are optimized. Under the optimized conditions, pre-concentration factor and limit of detection are 40 and 0.2 ng g(-1), respectively. The recoveries are in the range of 95-102%. A characteristic mass, 13 pg was obtained. The accuracy of the method is verified by analyzing certified reference materials such as NIST 1633b coal fly ash, NIST 1944 marine sediment and GBW 07312 stream sediments. The results obtained are in good agreement with the certified values and method is also applied to real samples.

摘要

本文介绍了一种简单的浊点萃取方法,用于从沉积物和粉煤灰样品的微波辅助王水提取液中分离和预浓缩铊。该方法基于铊的可萃取物种的形成及其与 Triton X-114 胶束的疏水性增溶部位在王水和电解质 NaCl 存在下的相互作用。这些胶束的相互作用用于将铊从大量水相萃取到富含胶束的小相中。有效消除了潜在的氯离子干扰,从而可以使用连续光源 ETAAS 从王水提取物中无干扰地测定铊。优化了影响萃取过程的参数。在优化条件下,预浓缩因子和检测限分别为 40 和 0.2ng g(-1)。回收率在 95-102%之间。获得了 13pg 的特征质量。通过分析 NIST 1633b 粉煤灰、NIST 1944 海洋沉积物和 GBW 07312 溪流沉积物等标准参考物质验证了该方法的准确性。所得结果与认证值吻合良好,该方法也适用于实际样品。

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