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一种新型离子液体/微量反萃取程序结合火焰原子吸收光谱法用于测定营养相关样品中的痕量镍。

A novel ionic liquid/micro-volume back extraction procedure combined with flame atomic absorption spectrometry for determination of trace nickel in samples of nutritional interest.

机构信息

Department of Chemistry, Faculty of Science, Yazd University, 89195/74, Yazd, Iran.

出版信息

J Hazard Mater. 2010 Jan 15;173(1-3):534-8. doi: 10.1016/j.jhazmat.2009.08.118. Epub 2009 Aug 31.

Abstract

A simple, highly sensitive and environment-friendly method for the determination of trace amount of nickel ion in different matrices is proposed. In the preconcentration step, the nickel from 10 mL of an aqueous solution was extracted into 500 microL of ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate [C(4)MIM][PF(6)], containing PAN as complexing agent. Subsequently, the PAN complex was back-extracted into 250 microL of nitric acid solution, and 100 microL of it was analyzed by flow injection flame atomic absorption spectrometry (FI-FAAS). The main parameter influencing the extraction and determination of nickel, such as pH, concentration of PAN, extraction time and temperature, ionic strength, and concentration of stripping acid solution, were optimized. An enhancement factor of 40.2 was achieved with 25 mL sample. The limit of detection (LOD) and quantification obtained under the optimum conditions were 12.5 and 41.0 microg L(-1), respectively. To validate the proposed methods two certified reference materials 681-I and BCR No. 288 were analyzed and the results were in good agreement with the certified values. The proposed method was successfully applied to determination of nickel in water samples, rice flour and black tea.

摘要

提出了一种简单、灵敏、环境友好的方法,用于测定不同基质中痕量镍离子。在预浓缩步骤中,从 10mL 水溶液中提取镍,用含有 PAN 作为络合剂的 1-丁基-3-甲基咪唑六氟磷酸盐([C(4)MIM][PF(6)])萃取到 500μL 中。随后,将 PAN 络合物反萃取到 250μL 硝酸溶液中,取 100μL 进行流动注射火焰原子吸收光谱(FI-FAAS)分析。优化了影响镍萃取和测定的主要参数,如 pH 值、PAN 浓度、萃取时间和温度、离子强度以及洗脱酸溶液浓度。用 25mL 样品实现了 40.2 的增强因子。在最佳条件下,检测限(LOD)和定量限分别为 12.5 和 41.0μg L(-1)。为了验证所提出的方法,分析了两个认证参考材料 681-I 和 BCR No. 288,结果与认证值吻合良好。该方法成功应用于水样、米粉和红茶中镍的测定。

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