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浊点萃取-火焰原子吸收光谱法用于水样中痕量镉的预富集和测定。

Cloud point extraction-flame atomic absorption spectrometry method for preconcentration and determination of trace cadmium in water samples.

作者信息

Ning Jinyan, Jiao Yang, Zhao Jiao, Meng Lifen, Yang Yaling

机构信息

Faculty of Life Science and Technology, Kunming University of Science and Technology, Yunnan Province 650500, China E-mail:

College of Architecture and City Planning, University of Wisconsin Madison, Madison, WI 53706, USA.

出版信息

Water Sci Technol. 2014;70(4):605-11. doi: 10.2166/wst.2014.263.

Abstract

A method based on cloud point extraction (CPE) separation/preconcentration of trace cadmium (Cd) as a prior step to its determination by flame atomic absorption spectrometry has been developed. Cadmium reacted with 8-hydroxyquinoline to form hydrophobic chelates, which were extracted into the micelles of nonionic surfactant oligoethylene glycol monoalkyl ether (Genapol X-080) in an alkaline medium. Octanol was used to depress the cloud point of Genapol X-080 in the extraction process. The chemical variables that affect the CPE, such as pH of complexation reaction, amount of chelating agent, Genapol X-080 and octanol were evaluated and optimized. Under optimized conditions, linearity was obeyed in the range of 10-500 μg/L, with the correlation coefficient of 0.9993. For 5 mL of sample solution, the enhancement factor was about 20. The limit of detection and limit of quantification of the method were 0.21 and 0.63 μg/L, respectively. The relative standard deviations (n = 6) was 3.2% for a solution containing 100 μg/L of Cd. The accuracy of the preconcentration system was evaluated by recovery measurements on spiked water samples. Recoveries of spiked samples varied in the range of 94.1-103.8%.

摘要

本文建立了一种基于浊点萃取(CPE)的痕量镉(Cd)分离/预富集方法,该方法作为火焰原子吸收光谱法测定镉的前处理步骤。镉与8-羟基喹啉反应形成疏水螯合物,在碱性介质中被萃取到非离子表面活性剂低聚乙二醇单烷基醚(Genapol X-080)的胶束中。萃取过程中使用辛醇降低Genapol X-080的浊点。评估并优化了影响浊点萃取的化学变量,如络合反应的pH值、螯合剂用量、Genapol X-080和辛醇用量。在优化条件下,线性范围为10-500 μg/L,相关系数为0.9993。对于5 mL样品溶液,富集因子约为20。该方法的检测限和定量限分别为0.21和0.63 μg/L。对于含100 μg/L Cd的溶液,相对标准偏差(n = 6)为3.2%。通过对加标水样的回收率测定评估了预富集系统的准确性。加标样品的回收率在94.1-103.8%范围内。

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