Anthemidis Aristidis N, Adam Ibrahim S I
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, Thessaloniki, Greece.
Anal Chim Acta. 2009 Jan 26;632(2):216-20. doi: 10.1016/j.aca.2008.10.078. Epub 2008 Nov 14.
A novel automatic sequential injection (SI) single-drop micro-extraction (SDME) system is proposed as versatile approach for on-line metal preconcentration and/or separation. Coupled to electrothermal atomic absorption spectrometry (ETAAS) the potentials of this SI scheme are demonstrated for trace cadmium determination in water samples. A non-charged complex of cadmium with ammonium diethyldithiophosphate (DDPA) was produced and extracted on-line into a 60 microL micro-drop of di-isobutyl ketone (DIBK). The extraction procedure was performed into a newly designed flow-through extraction cell coupled on a sequential injection manifold. As the complex Cd(II)-DDPA flowed continuously around the micro-droplet, the analyte was extracting into the solvent micro-drop. All the critical parameters were optimized and offered good performance characteristics and high preconcentration ratios. For 600 s micro-extraction time, the enhancement factor was 10 and the sampling frequency was 6h(-1). The detection limit was 0.01 microg L(-1) and the precision (RSD at 0.1 microg L(-1) of cadmium) was 3.9%. The proposed method was evaluated by analyzing certified reference material.
提出了一种新型自动顺序注射(SI)单滴微萃取(SDME)系统,作为一种用于在线金属预富集和/或分离的通用方法。与电热原子吸收光谱法(ETAAS)联用,展示了该SI方案在测定水样中痕量镉方面的潜力。镉与二乙基二硫代磷酸铵(DDPA)形成不带电的络合物,并在线萃取到60微升的二异丁基酮(DIBK)微滴中。萃取过程在一个新设计的流通萃取池中进行,该萃取池连接在顺序注射歧管上。当镉(II)-DDPA络合物围绕微滴连续流动时,分析物被萃取到溶剂微滴中。所有关键参数均经过优化,具有良好的性能特征和高预富集率。在600秒的微萃取时间下,富集因子为10,采样频率为6小时-1。检测限为0.01微克/升,精密度(镉浓度为0.1微克/升时的相对标准偏差)为3.9%。通过分析有证标准物质对所提出的方法进行了评估。