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在与电热原子吸收光谱检测联用的顺序注射阀上实验室(SI-LOV)系统中,通过螯合琼脂糖珠进行在线分离和预富集来测定痕量金属离子。

Determination of trace metal ions via on-line separation and preconcentration by means of chelating Sepharose beads in a sequential injection lab-on-valve (SI-LOV) system coupled to electrothermal atomic absorption spectrometric detection.

作者信息

Long Xiangbao, Hansen Elo Harald, Miró Manuel

机构信息

Department of Chemistry, Technical University of Denmark, Kemitorvet, Building 207, DK-2800 Kgs. Lyngby, Denmark.

出版信息

Talanta. 2005 Jun 15;66(5):1326-32. doi: 10.1016/j.talanta.2005.01.056. Epub 2005 Mar 2.

DOI:10.1016/j.talanta.2005.01.056
PMID:18970125
Abstract

The analytical performance of an on-line sequential injection lab-on-valve (SI-LOV) system using chelating Sepharose beads as sorbent material for the determination of ultra-trace levels of Cd(II), Pb(II) and Ni(II) by electrothermal atomic absorption spectrometry (ETAAS) is described and discussed. The samples are adjusted to pH 5.0 on-line in the system for optimum operation. The target ions are adsorbed by chelation on the surface of the beads, contained in a 20mul microcolumn within the LOV, and following elution by 50mul 2M nitric acid, the eluate is, as sandwiched by air segments, introduced into the ETAAS. Based on the consumption of 1.8ml sample solution, retention efficiencies of 95, 75 and 90%, enrichment factors of 34, 27 and 32, and determination limits of 0.001, 0.07 and 0.02mugl(-1) were obtained for Cd(II), Pb(II) and Ni(II), respectively. The beads can be used repeatedly for at least 20 times without decrease of performance, yet can be replaced at will if the circumstances should so dictate. The optimized procedural parameters showed that 12 samples per hour could be prepared and successfully analyzed. The results obtained for three standard reference materials agreed very well with the certified values.

摘要

描述并讨论了一种在线顺序注射阀上实验室(SI-LOV)系统的分析性能,该系统使用螯合琼脂糖珠作为吸附材料,通过电热原子吸收光谱法(ETAAS)测定超痕量水平的Cd(II)、Pb(II)和Ni(II)。样品在系统中在线调节至pH 5.0以实现最佳操作。目标离子通过螯合作用吸附在位于LOV内20微升微柱中的珠子表面,在用50微升2M硝酸洗脱后,洗脱液被空气段夹送引入ETAAS。基于消耗1.8毫升样品溶液,Cd(II)、Pb(II)和Ni(II)的保留效率分别为95%、75%和90%,富集因子分别为34、27和32,测定限分别为0.001、0.07和0.02微克/升。这些珠子可重复使用至少20次而性能不降低,但如果情况需要也可随意更换。优化后的程序参数表明每小时可制备并成功分析12个样品。三种标准参考物质的测定结果与认证值非常吻合。

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