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用 1-酰基硫代缩氨基脲化学改性的活性炭,用于选择性固相萃取和预浓缩水样中的痕量 Cu(II)、Hg(II)和 Pb(II)。

Chemically modified activated carbon with 1-acylthiosemicarbazide for selective solid-phase extraction and preconcentration of trace Cu(II), Hg(II) and Pb(II) from water samples.

机构信息

Department of Chemistry, Lanzhou University, Lanzhou 730000, PR China.

出版信息

J Hazard Mater. 2009 Dec 15;172(1):324-9. doi: 10.1016/j.jhazmat.2009.07.014. Epub 2009 Jul 10.

Abstract

A new sorbent 1-acylthiosemicarbazide-modified activated carbon (AC-ATSC) was prepared as a solid-phase extractant and applied for removing of trace Cu(II), Hg(II) and Pb(II) prior to their determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The separation/preconcentration conditions of analytes were investigated, including effects of pH, the shaking time, the sample flow rate and volume, the elution condition and the interfering ions. At pH 3, the maximum static adsorption capacity of Cu(II), Hg(II) and Pb(II) onto the AC-ATSC were 78.20, 67.80 and 48.56 mg g(-1), respectively. The adsorbed metal ions were quantitatively eluted by 3.0 mL of 2% CS(NH2)2 and 2.0 mol L(-1) HCl solution. Common coexisting ions did not interfere with the separation. According to the definition of IUPAC, the detection limits (3sigma) of this method for Cu(II), Hg(II) and Pb(II) were 0.20, 0.12 and 0.45 ng mL(-1), respectively. The relative standard deviation under optimum conditions is less than 4.0% (n=8). The prepared sorbent was applied for the preconcentration of trace Cu(II), Hg(II) and Pb(II) in certified and water samples with satisfactory results.

摘要

一种新型的 1-酰基硫代半卡巴腙修饰的活性炭(AC-ATSC)被制备为固相萃取剂,并应用于电感耦合等离子体发射光谱法(ICP-OES)测定痕量 Cu(II)、Hg(II)和 Pb(II)之前的分离/预浓缩。研究了分析物的分离/预浓缩条件,包括 pH 值、振摇时间、样品流速和体积、洗脱条件和干扰离子的影响。在 pH 3 时,AC-ATSC 对 Cu(II)、Hg(II)和 Pb(II)的最大静态吸附容量分别为 78.20、67.80 和 48.56 mg g(-1)。吸附的金属离子可通过 3.0 mL 2% CS(NH2)2 和 2.0 mol L(-1) HCl 溶液定量洗脱。常见共存离子不干扰分离。根据 IUPAC 的定义,该方法对 Cu(II)、Hg(II)和 Pb(II)的检测限(3sigma)分别为 0.20、0.12 和 0.45 ng mL(-1)。在最佳条件下,相对标准偏差小于 4.0%(n=8)。该制备的吸附剂用于痕量 Cu(II)、Hg(II)和 Pb(II)在认证和水样中的预浓缩,结果令人满意。

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