单壁碳纳米管-纳米金-离子液体修饰玻碳电极用于线性伏安法测定辛硫磷
Linear Voltammetric Determination of Phoxim Using SWCNTs-nano Au-BMIMPF6 Modified GCE as Working Electrode
摘 要
将单壁碳纳米管(SWCNTs)悬浊液和纳米金(nano Au)溶液混匀后滴涂在玻碳电极表面,自然干燥后再将离子液体BMIMPF6的甲醇溶液滴涂在上述电极上,制得单壁碳纳米管-纳米金-离子液体修饰玻碳电极(SWCNTs-nano Au-BMIMPF6/GCE)。用循环伏安方法研究了辛硫磷在pH 4.0的磷酸盐支持电解质中,在电位-1.1~-0.1 V(vs.SCE)范围内,在修饰电极上的电化学行为。结果表明:在电位-0.81 V处可见明显的还原峰,且其峰电流与辛硫磷的浓度在6.0×10-7~1.2×10-3mmol·L-1范围内呈线性关系,检出限(3S/N)为3.0×10-7mmol·L-1。据此提出了用线性伏安法测定辛硫磷的方法,用标准加入法测得其回收率在96.0%~105.5%之间,测定值的相对标准偏差(n=6)在3.3%~3.9%之间。
离子液体
单壁碳纳米管
纳米金
电化学行为
Phoxim
Ionic liquid
Single-walled carbon nanotubes
Nano Au
Electrochemical behavior
Abstract
A mixture of dispersion of SWCNTs and nano Au solution was added dropwise onto the surface of glassy carbon electrode (GCE), after air-drying, methanol solution of ionic liquid, BMIMPF6 was added dropwise onto the surface of the above electrode. The modified electrode, designated as SWCNTs-nano Au-BMIMPF6/GCE was thus prepared. Electrochemical behavior of phoxim at the modified electrode was studied by cyclic voltammetry in a phosphate buffer supporting electrolyte of pH 4.0 in the potential range of -1.1 to -0.1 V (vs.SCE). As shown by the experimental results, a significant reduction peak was observed at -0.81 V, and linear relationship between values of reduction peak current and concentration of phoxim was kept in the range of 6.0×10-7 to 1.2×10-3mmol·L-1, with detection limit (3S/N) of 3.0 ×10-7mmol·L-1. Based on these findings, a method for determination of phoxim by linear voltammetry was proposed. Recovery was tested by standard addition method, giving values of recovery and RSD′s (n=6) in the ranges of 96.0%-105.5% and 3.3%-3.9% respectively.
中图分类号 O657.14
所属栏目 工作简报
基金项目 国家自然科学基金资助项目(20763009);云南省教育厅科学研究基金资助项目(09Y039)
收稿日期 2011/11/12
修改稿日期
网络出版日期
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备注刘拥军(1971-),男,云南昆明人,工程师,硕士,主要从事电化学传感器及纳米材料研究。
引用该论文: LIU Yong-jun,WANG Guang-can,SHI Zhen,YI Han-xi,HE Wen-jin,PENG Fang-zhi. Linear Voltammetric Determination of Phoxim Using SWCNTs-nano Au-BMIMPF6 Modified GCE as Working Electrode[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(9): 1058～1062
刘拥军,王光灿,师真,易汉希,何雯瑾,彭芳芝. 单壁碳纳米管-纳米金-离子液体修饰玻碳电极用于线性伏安法测定辛硫磷[J]. 理化检验－化学分册, 2012, 48(9): 1058～1062
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参考文献
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【3】EDER D. Carbon nanotube-inorganic hybrids［J］. Chem Rev, 2010,110:1348-1385.
【4】CHU Hai-bin, WEI Li, CUI Rong-li, et al. Carbon nanotubes combined with inorganic nanomaterials: Preparations and applications［J］. Coordin Chem Rev, 2010,254:1117-1134.
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【6】WING-SZE H V, KAGAN K. Gold electrodeposition on carbon nanotubes for the enhanced electrochemical detection of homocysteine［J］. Electrochemistry Communications, 2011,13:328-330.
【7】LI He, LIU Run, ZHAO Rong-xiang, et al. Morphology control of electrodeposited Cu2O crystals in aqueous solutions using room temperature hydrophilic ionic liquids［J］.Cryst Growth Des, 2006,6:2795-2798.
【8】ZHAO Feng, WU Xue-e, WANG Ming-kui, et al. Electrochemical and bioelectrochemistry properties of room-temperature ionic liquids and carbon composite materials［J］. Anal Chem, 2004,76:4960-4967.
【9】FAN Shuang-shuang, XIAO Fei, LIU Li-qin, et al. Sensitive voltammetric response of methylparathion on single-walled carbon nanotube paste coated electrodes using ionic liquid as binder［J］.Sensors and Actuators B, 2008,132:34-39.
【10】WANG Zhi-juan, ZHANG Qi-xian, DAN K, et al. The synthesis of ionic-liquid-functionalized multiwalled carbon nanotubes decorated with highly dispersed Au nanoparticles and their use in oxygen reduction by electrocatalysis［J］. Carbon, 2008,46:1687-1692.
【11】SHI Yu, YANG Rui-zhi, YUET P K. Easy decoration of carbon nanotubes with well dispersed gold nanoparticles and the use of the material as an electrocatalyst［J］. Carbon, 2009,47:1146-1151.
【12】MASATAKE H. Size-and support-depeddency in the catalysis of gold［J］. Catalysis Today, 1997,36:153-166.
【13】MITSUTAKA O, YASUTAKA K, MASATAKE H, et al. DFT studies of interaction between O2 and Au clusters: The rule of anionic surface Au atoms on Au clusters for catalyzed oxygenation［J］. Chemical Physics Letters, 2001,346:163-168.
【14】杨书昌,师真,刘拥军,等.用多壁碳纳米管修饰玻碳电极为工作电极循环伏安法测定辛硫磷［J］.理化检验-化学分册, 2011,47(1):50-53.
【15】BROWN K R, WALTER D G, NATAN M J. Seeding of colloidal Au nanoparticle solutions. 2. improved control of particle size and shape［J］. Chem Mater, 2000,12:306-313.
【16】TSANG S C, CHEN Y K, HARRIS P J F, et al. A simple chemical method of opening and filling carbon nanotubes［J］. Nature, 1994,372:159-162.
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