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硅胶固相萃取-2-(2-氧代乙基)肼二硫代甲酰胺分离富集痕量汞(II)及其电感耦合等离子体原子发射光谱法测定。

Solid phase extraction of trace Hg(II) on silica gel modified with 2-(2-oxoethyl)hydrazine carbothioamide and determination by ICP-AES.

机构信息

Department of Chemistry, Lanzhou University, Tianshui Road 222, Lanzhou, Gansu 730000, PR China.

出版信息

Talanta. 2010 Oct 15;82(5):1791-6. doi: 10.1016/j.talanta.2010.07.076. Epub 2010 Aug 5.

Abstract

In this work, a new 2-(2-oxoethyl)hydrazine carbothioamide modified silica gel (SG-OHC) sorbent was prepared and applied for preconcentration of trace mercury(II) prior to the measurement by inductively coupled plasma atomic emission spectrometry (ICP-AES). The optimization of some analytical parameters affecting the adsorption of the analyte such as acidity, shaking time, sample flow rate and volume, eluent condition, and interfering substances were investigated. At pH 3, the maximum static adsorption capacity of Hg(II) onto the SG-OHC was 37.5 mg g(-1). The quantitative recovery (>95%) of Hg(II) could be obtained using 2 mL of 0.5 mol L(-1)HCl and 1% CS(NH(2))(2) solution as eluent. Common coexisting substances did not interfere with the separation of mercury(II) under optimal conditions. The detection limit of present method was 0.10 ng mL(-1), and the relative standard deviation (RSD) was lower than 4.0% (n=8). The prepared sorbent was successfully applied for the preconcentration of trace Hg(II) in certified and water samples with satisfactory results.

摘要

在这项工作中,制备了一种新型的 2-(2-氧代乙基)肼基硫代甲酰胺改性硅胶(SG-OHC),并将其应用于电感耦合等离子体原子发射光谱法(ICP-AES)测定前痕量汞(II)的预富集。考察了影响分析物吸附的一些分析参数的优化,如酸度、振摇时间、样品流速和体积、洗脱液条件和干扰物质。在 pH 3 时,SG-OHC 对 Hg(II)的最大静态吸附容量为 37.5mg g(-1)。使用 2 mL 0.5 mol L(-1)HCl 和 1% CS(NH(2))(2)溶液作为洗脱液,可以定量回收(>95%)Hg(II)。在最佳条件下,常见共存物质不干扰汞(II)的分离。本方法的检出限为 0.10ng mL(-1),相对标准偏差(RSD)低于 4.0%(n=8)。制备的吸附剂成功地应用于痕量 Hg(II)在认证和水样中的预富集,结果令人满意。

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