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在通过火焰原子吸收光谱法测定之前,使用没食子酸改性硅胶对铅(II)、铜(II)、镉(II)和镍(II)进行固相萃取。

Solid phase extraction of lead (II), copper (II), cadmium (II) and nickel (II) using gallic acid-modified silica gel prior to determination by flame atomic absorption spectrometry.

作者信息

Xie Fazhi, Lin Xucong, Wu Xiaoping, Xie Zenghong

机构信息

The Department of Chemistry, Fuzhou University, Fuzhou, Fujian 350002, China.

出版信息

Talanta. 2008 Jan 15;74(4):836-43. doi: 10.1016/j.talanta.2007.07.018. Epub 2007 Jul 26.

Abstract

The immobilization of gallic acid on the surface of amino group-containing silica gel phases for the formation of a newly chelating matrix (GASG) is described. The newly synthesized extractant, characterized by the diffuse reflectance infrared Fourier transformation spectroscopy and elemental analysis, was used to preconcentrate Pb(II), Cu(II), Cd(II) and Ni(II). The pH ranges for quantitative sorption and the concentrations of HCl for eluting Pb(II), Cd(II), Cu(II) and Ni(II) were opimized, respectively. The sorption capacity of the matrix has been found to be 12.63, 6.09, 15.38, 4.62mg/g for Pb(II), Cd(II), Cu(II) and Ni(II), respectively, with the preconcentration factor of approximately 200 ( approximately 100 for Cd(II)). The effects of flow rates, the eluants, the electrolytes and cations on the metal ions extraction, as well as the chelating matrix stability and reusability, were also studied. The extraction behavior of the matrix was conformed with Langmuir's equation. The present preconcentration and determination method was successfully applied to the analysis of synthetic metal mixture solution and river water samples. The 3sigma detection limit and 10sigma quantification limit for Pb(II), Cu(II), Cd(II) and Ni(II) were found to be 0.58, 0.86, 0.65, 0.92microg/L and 1.08, 1.23, 0.87, 1.26microg/L, respectively.

摘要

本文描述了将没食子酸固定在含氨基硅胶相表面以形成新型螯合基质(GASG)的过程。通过漫反射红外傅里叶变换光谱和元素分析对新合成的萃取剂进行了表征,并用于预富集Pb(II)、Cu(II)、Cd(II)和Ni(II)。分别优化了定量吸附的pH范围以及洗脱Pb(II)、Cd(II)、Cu(II)和Ni(II)的HCl浓度。已发现该基质对Pb(II)、Cd(II)、Cu(II)和Ni(II)的吸附容量分别为12.63、6.09、15.38、4.62mg/g,预富集因子约为200(Cd(II)约为100)。还研究了流速、洗脱剂、电解质和阳离子对金属离子萃取的影响,以及螯合基质的稳定性和可重复使用性。该基质的萃取行为符合朗缪尔方程。所提出的预富集和测定方法成功应用于合成金属混合溶液和河水样品的分析。发现Pb(II)、Cu(II)、Cd(II)和Ni(II)的3σ检测限和10σ定量限分别为0.58、0.86、0.65、0.92μg/L和1.08、1.23、0.87、1.26μg/L。

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