基于无序介孔碳的全固态自支撑聚合物膜铅离子选择性微型电极  

Preparation of an All-solid-state Self-supported Pb^(2+)-selective Miniaturized Electrode Based on Disordered Mesoporous Carbon

作　　者：高杨[1,3] 丁家旺 尹坦姬[1,2] 秦伟[1,2] GAO Yang;DING Jia-wang;YIN Tan-ji;QIN Wei(CAS Key Laboratory of Coastal Environmental Processes and Ecological Remediation,Shandong Key Laboratory of Coastal Environmental Processes,Yantai Institute of Coastal Zone Research,Chinese Academy of Sciences,Yantai 264003,China;Center for Ocean Mega-Science,Chinese Academy of Sciences,Qingdao 266071,China;University of Chinese Academy of Sciences,Beijing 100049,China)

机构地区：[1]中国科学院海岸带环境过程与生态修复重点实验室,山东省海岸带环境过程重点实验室,中国科学院烟台海岸带研究所,山东烟台264003 [2]中国科学院海洋大科学研究中心,山东青岛266071 [3]中国科学院大学,北京100049

出　　处：《分析测试学报》2021年第8期1219-1223,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金(21677172,41706110);国家重点研发计划重点专项(2016YFC1400700);山东省泰山学者计划(TSPD20181215)。

摘　　要：将无序介孔碳材料填充到尖端直径约150μm的毛细玻璃管内,利用其多孔结构将铅离子选择性敏感膜吸附于电极尖端内部,制备了基于无序介孔碳的全固态自支撑聚合物膜铅离子选择性微型电极(Pb^(2+)-ISμE)。采用循环伏安法(CV)和电化学阻抗法对所制备电极的电化学性质进行表征,并考察了其电位响应性能。结果表明,基于无序介孔碳的微型电极具有微电极所特有的"S"型循环伏安曲线,且由于电极材料的多孔性表现出较大的双电层电容特性,所构建的Pb^(2+)-ISμE测定Pb^(2+)的线性范围为1.0×10^(-7)^1.0×10^(-4)mol/L,响应斜率为(28.9±0.5)mV/dec,检出限为4.0×10^(-8)mol/L。该Pb^(2+)-ISμE表现出良好的选择性、稳定性和重复性,并成功应用于海岸带沉积物加标孔隙水中Pb^(2+)的测定。该文为微型电极的制备提供了一种简单、便捷的方法,并为微环境或微量样品中离子的测定提供了一种有效的检测手段。An all-solid-state self-supported Pb^(2+)-selective miniaturized electrode(Pb^(2+)-ISμE)based on disordered mesoporous carbon was fabricated by filling the disordered mesoporous carbon as the self-supporting material into a capillary glass tube with a tip diameter about 150μm,and adsorbing the ion-selective polymeric membrane into the porous structure of disordered mesoporous carbon.The electrochemical behaviors of the proposed electrode were characterized by using cyclic voltammetry and electrochemical impedance spectroscopy,and the potentiometric performance of the Pb^(2+)-ISμE was also investigated.Experiments results indicated that the disordered mesoporous carbon-based miniaturized electrode showed a typical"S"cyclic voltammogram and a large double-layer capacitance because of the porous structure,and the proposed Pb^(2+)-ISμE exhibited a Nernstian potentiometric response in the linear range of 1.0×10^(-7)-1.0×10^(-4) mol/L with a response slope of(28.9±0.5)mV/dec and a detection limit of 4.0×10^(-8)mol/L.In addition,the proposed electrode showed excellent selectivity,stability and reproducibility,and was successfully applied in the determination of Pb^(2+)in pore water.This work provides a simple and convenient method for the preparation of the miniaturized electrodes,and is promising for the determination of ions in micro-environments or with micro/small volumes.

关 键 词：聚合物膜离子选择性电极 微型电极 无序介孔碳 全固态 铅离子 

分 类 号：O657.1[理学—分析化学] O614.433[理学—化学]