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萃取-光谱法测定高纯铝盐中的铅。

Extraction-spectrometric determination of lead in high-purity aluminium salts.

机构信息

Research Institute of Inorganic Chemistry, Revolucni 84, 400 01 Usti nad Labem, Czech Republic.

出版信息

Talanta. 2002 Aug 23;58(2):325-30. doi: 10.1016/s0039-9140(02)00247-3.

DOI:10.1016/s0039-9140(02)00247-3
PMID:18968757
Abstract

Trace amounts of lead were determined in high purity aluminium salts (especially in ammonium aluminium sulfate) using inductively coupled plasma-optical emission spectrometry (ICP-OES) after extractive pre-concentration and matrix separation. Metals were extracted from the aluminium matrix in the form of chelates with ammonium pyrolidine dithoocarbamate into methyl isobutyketone. The organic extract was digested with nitric acid and hydrogen peroxide. The limit of detection for the determination of lead in crystalline ammonium aluminium sulfate was ca. 0.044 mug g(-1). The relative expanded uncertainty of the lead determination was ca. 23% at the level of 0.2 mug g(-1) and ca. 16% at the level of 1.0 mug g(-1). The main uncertainty contribution was associated with repeatability of the whole analytical procedure.

摘要

采用电感耦合等离子体发射光谱法(ICP-OES),通过萃取预浓缩和基体分离,测定高纯铝盐(特别是硫酸铝铵)中的痕量铅。金属以与氨 基吡咯烷二硫代氨基甲酸盐形成的螯合物的形式从铝基体中提取出来,进入甲基异丁基酮。用硝酸和过氧化氢消解有机提取物。在结晶硫酸铝铵中测定铅的检出限约为 0.044 微克/克。在 0.2 微克/克的水平下,铅测定的相对扩展不确定度约为 23%,在 1.0 微克/克的水平下,相对扩展不确定度约为 16%。主要的不确定度贡献与整个分析程序的重复性有关。

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