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磁硫掺杂多孔碳用于环境水样中痕量汞的 ICP-MS 检测前的预浓缩。

Magnetic sulfur-doped porous carbon for preconcentration of trace mercury in environmental water prior to ICP-MS detection.

机构信息

Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, P R China.

出版信息

Analyst. 2017 Nov 20;142(23):4570-4579. doi: 10.1039/c7an01195d.

Abstract

A novel magnetic sulfur-doped porous carbon (MSPC) was fabricated via a simple one-step carbonization of a mixture of sucrose, basic magnesium sulfate whiskers and FeO@SiO nanoparticles. Due to the high S content, the prepared MSPC possessed high adsorption capacity for Hg (343 mg g) with good selectivity. Based on this, a method coupling magnetic solid phase extraction (MSPE) with inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of trace Hg in environmental water samples. Various parameters such as pH, desorption solvent and its concentration, desorption volume and time, sample volume, and adsorption time that affect the determination have been optimized. Under the optimal conditions, a high enrichment factor of 100-fold was obtained, the limit of detection (LOD) was found to be 0.52 pg mL with a relative standard deviation (c = 10 pg mL, n = 7) of 7.1%, and a good linearity was obtained within the concentration range of 2-5000 pg mL for Hg. Besides, the proposed method has very fast adsorption/desorption kinetics, target Hg could be rapidly adsorbed on the prepared MSPC in 2 min and desorbed from the MSPC in 2 min with the assistance of a permanent magnet. Therefore, the proposed method of MSPE-ICP-MS exhibits good application potential in the determination of trace Hg in environmental water samples.

摘要

一种新型磁性硫掺杂多孔碳(MSPC)是通过蔗糖、碱式硫酸镁晶须和 FeO@SiO 纳米粒子混合物的一步碳化简单制备的。由于高 S 含量,所制备的 MSPC 对 Hg 具有高吸附容量(343 mg g)和良好的选择性。基于此,开发了一种将磁性固相萃取(MSPE)与电感耦合等离子体质谱(ICP-MS)相结合的方法,用于测定环境水样中的痕量 Hg。研究了影响测定的各种参数,如 pH 值、解吸溶剂及其浓度、解吸体积和时间、样品体积和吸附时间等。在最佳条件下,获得了 100 倍的高富集因子,检测限(LOD)为 0.52 pg mL,相对标准偏差(c = 10 pg mL,n = 7)为 7.1%,Hg 的浓度范围为 2-5000 pg mL 时具有良好的线性关系。此外,所提出的方法具有非常快速的吸附/解吸动力学,目标 Hg 可以在 2 分钟内通过在永久磁铁的帮助下快速吸附在制备的 MSPC 上,并在 2 分钟内从 MSPC 上解吸。因此,MSPE-ICP-MS 方法在测定环境水样中的痕量 Hg 方面具有良好的应用潜力。

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