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以固定化8-羟基喹啉为吸附剂,采用流动注射-火焰原子吸收光谱法在线微柱分离/预富集技术对铊进行形态分析和测定。

Speciation and determination of thallium by on-line microcolumn separation/preconcentration by flow injection-flame atomic absorption spectrometry using immobilized oxine as sorbent.

作者信息

Dadfarnia S, Assadollahi T, Haji Shabani A M

机构信息

Depatrment of Chemistry, Yazd University, Safaieh, 89195 Yazd, Iran.

出版信息

J Hazard Mater. 2007 Sep 5;148(1-2):446-52. doi: 10.1016/j.jhazmat.2007.02.059. Epub 2007 Mar 3.

Abstract

A flow injection analysis (FIA) system incorporation a microcolumn of immobilized oxine on surfactant-coated alumina had been devised for performing rapid thallium enrichment/matrix removal in flame atomic absorption spectrometry (FAA). The preconcentration is based on the deposition of thallium(I) on microcolumn and subsequent elution with 500 microl of sodium thiosulfate (1 moll(-1)). In the presence of EDTA, only Tl(I) was retained on the microcolumn. Total thallium was determined after reduction of Tl(III) to Tl(I) by hydroxyl amine hydrochloride. A sample volume of 25 ml resulted in a preconcentration factor of 77. Precision at 30 microgl(-1) was 2.6% RSD (n=10). With 25 ml sampling volume a detection limit of 2.5 microgl(-1) was determined. The effect of potential interfering ions on the determination was studied. The method was applied for the determination of thallium in water, waste water, hair, nail, coal, and standard reference alloys. The accuracy was assessed through recovery experiment, independent analysis by Furnace-AAS, and analysis of certified reference alloys.

摘要

已设计出一种流动注射分析(FIA)系统,该系统包含一个固定在表面活性剂包覆氧化铝上的8-羟基喹啉微柱,用于在火焰原子吸收光谱法(FAA)中快速富集铊/去除基体。预富集基于铊(I)在微柱上的沉积以及随后用500微升硫代硫酸钠(1 mol l⁻¹)洗脱。在乙二胺四乙酸(EDTA)存在下,只有铊(I)保留在微柱上。通过用盐酸羟胺将铊(III)还原为铊(I)后测定总铊。25毫升的样品体积产生了77的预富集因子。30 μg l⁻¹时的精密度为2.6%相对标准偏差(n = 10)。采用25毫升进样体积时,测定的检出限为2.5 μg l⁻¹。研究了潜在干扰离子对测定的影响。该方法用于测定水、废水、头发、指甲、煤和标准参考合金中的铊。通过回收率实验、炉原子吸收光谱法(Furnace-AAS)独立分析以及有证参考合金分析来评估准确度。

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