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电化学氢化物发生原子吸收光谱法测定镉

Electrochemical hydride generation atomic absorption spectrometry for determination of cadmium.

作者信息

Arbab-Zavar M H, Chamsaz M, Youssefi A, Aliakbari M

机构信息

Department of Chemistry, Faculty of Science, Ferdowsi University, Mashhad, Iran.

Pare-Taavous Research Institute, Mashhad, Iran.

出版信息

Anal Chim Acta. 2005 Aug 1;546(1):126-132. doi: 10.1016/j.aca.2005.05.011. Epub 2005 Jun 13.

Abstract

An electrolytic hydride generation system for determination of another hydride forming element, cadmium, by catholyte variation electrochemical hydride generation (EcHG) atomic absorption spectrometry is described. A laboratory-made electrolytic cell with lead-tin alloy as cathode material is designed as electrolytic generator of molecular hydride. The influences of several parameters on the analytical signal have been evaluated using a Plackett-Burman experimental design. The significant parameters such as cathode surface area, electrolytic current, carrier gas flow rate and catholyte concentration have been optimized using univariate method. The analytical figures of merit of procedure developed were determined. The calibration curve was linear up to 20ngmlof cadmium. The concentration detection limit (3σ, n=8) of 0.2ngml and repeatability (relative standard deviation, n=7) of 3.1% were achieved at 10.0ngml. It was shown that interferences from major constituents at high concentrations were significant. The accuracy of method was verified using a real sample (spiked tap water) by standard addition calibration technique. Recovery of 104% was achieved for Cd in the spiked tap water sample.

摘要

描述了一种用于通过阴极电解液变化电化学氢化物发生(EcHG)原子吸收光谱法测定另一种氢化物形成元素镉的电解氢化物发生系统。设计了一种以铅锡合金为阴极材料的自制电解池作为分子氢化物的电解发生器。使用Plackett-Burman实验设计评估了几个参数对分析信号的影响。使用单变量方法对阴极表面积、电解电流、载气流速和阴极电解液浓度等重要参数进行了优化。确定了所开发方法的分析性能指标。校准曲线在镉含量高达20ng/ml时呈线性。在10.0ng/ml时,浓度检测限(3σ,n = 8)为0.2ng/ml,重复性(相对标准偏差,n = 7)为3.1%。结果表明,高浓度主要成分的干扰显著。通过标准加入校准技术使用实际样品(加标自来水)验证了方法的准确性。加标自来水样品中镉的回收率为104%。

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