Chicharro Manuel, Arribas Alberto Sánchez, Moreno Mónica, Bermejo Esperanza, Zapardiel Antonio
Departamento de Química Analítica y Análisis Instrumental, Facultad de Ciencias, Universidad Autónoma de Madrid, 28049 Madrid, Spain.
Talanta. 2007 Dec 15;74(3):376-86. doi: 10.1016/j.talanta.2007.07.034. Epub 2007 Aug 7.
This work reports on a comparative study of the electrochemical performance of carbon nanotubes-based electrodes in micellar media and their application for amperometric detection in micellar electrokinetic capillary chromatography (MEKC) separations. These electrodes were prepared in two different ways: immobilization of a layer of carbon nanotubes dispersed in polyethylenimine (PEI), ethanol or Nafion onto glassy carbon electrodes or preparation of paste electrodes using mineral oil as binder. Scanning electron microscopy (SEM) was employed for surface morphology characterization while cyclic voltammetry of background electrolyte was used for capacitance estimation. The amperometric responses to hydrogen peroxide, amitrol, diuron and 2,3-dichlorophenol (2,3CP) in the presence and in the absence of sodium dodecylsulphate (SDS) were studied by flow injection analysis (FIA), demonstrating that the electrocatalytic activity, background current and electroanalytical performance were strongly dependent on the electrodes preparation procedure. Glassy carbon electrodes modified with carbon nanotubes dispersed in PEI (GC/(CNT/PEI)) displayed the most adequate performance in micellar media, maintaining good electrocatalytic properties combined with acceptable background currents and resistance to passivation. The advantages of using GC/(CNT/PEI) as detectors in capillary electrophoresis were illustrated for the MEKC separations of phenolic pollutants (phenol, 3-chlorophenol, 2,3-dichlorophenol and 4-nitrophenol) and herbicides (amitrol, asulam, diuron, fenuron, monuron and chlortoluron).
本工作报道了基于碳纳米管的电极在胶束介质中的电化学性能的比较研究及其在胶束电动毛细管色谱(MEKC)分离中的安培检测应用。这些电极通过两种不同方式制备:将分散在聚乙烯亚胺(PEI)、乙醇或Nafion中的一层碳纳米管固定在玻碳电极上,或使用矿物油作为粘合剂制备糊剂电极。采用扫描电子显微镜(SEM)进行表面形态表征,同时利用背景电解质的循环伏安法进行电容估计。通过流动注射分析(FIA)研究了在存在和不存在十二烷基硫酸钠(SDS)的情况下对过氧化氢、杀草强、敌草隆和2,3 - 二氯苯酚(2,3CP)的安培响应,结果表明电催化活性、背景电流和电分析性能强烈依赖于电极制备程序。用分散在PEI中的碳纳米管修饰的玻碳电极(GC/(CNT/PEI))在胶束介质中表现出最适宜的性能,保持了良好的电催化性能,同时具有可接受的背景电流和抗钝化能力。对于酚类污染物(苯酚、3 - 氯苯酚、2,3 - 二氯苯酚和4 - 硝基苯酚)和除草剂(杀草强、杀草敏、敌草隆、非草隆、灭草隆和绿麦隆)的MEKC分离,说明了使用GC/(CNT/PEI)作为毛细管电泳检测器的优势。