石墨烯-金纳米粒子复合膜修饰电极的制备及对双酚A的测定

doi:10.7503/cjcu20150137

高等学校化学学报 ›› 2015, Vol. 36 ›› Issue (8): 1491.doi: 10.7503/cjcu20150137

石墨烯-金纳米粒子复合膜修饰电极的制备及对双酚A的测定

方燕¹, 马琳琳², 陕多亮², 卢小泉²()

1.甘肃省分析测试中心, 兰州 730000
2. 甘肃省生物电化学与环境分析重点实验室, 西北师范大学化学化工学院, 兰州 730070

收稿日期:2015-02-09 出版日期:2015-08-10 发布日期:2015-07-17
作者简介:联系人简介: 卢小泉, 男, 博士, 教授, 主要从事分析化学和电化学方面的研究. E-mail:luxq@nwnu.edu.cn
基金资助:
国家自然科学基金(批准号: 21327005, 21175108)、教育部长江学者和创新团队发展计划(批准号: IRT1283)、甘肃省创新研究群体计划(批准号: 1210RJIA001)和兰州市人才创新创业科技计划(批准号: 2014-RC-39)资助

Preparation of Graphene/Gold Nanoparticle Composite Film Modified Electrode and Its Application for Determination of Bisphenol A^†

FANG Yan¹, MA Linlin², SHAN Duoliang², LU Xiaoquan^2,^*()

1. The Analysis and Research Center of Gansu Province, Lanzhou 730000, China
2.Key Laboratory of Bioelectrochemistry & Environmental Analysis of Gansu Province,College of Chemistry & Chemical Engineering, Northwest Normal University, Lanzhou 730070, China

Received:2015-02-09 Online:2015-08-10 Published:2015-07-17
Contact: LU Xiaoquan E-mail:luxq@nwnu.edu.cn
Supported by:
† Supported by the National Natural Science Foundation of China(Nos.21327005, 21175108), the Program for Changjiang Scholars and Innovative Research Team, Ministry of Education, China(No;IRT1283), the Program for Innovative Research Group of Gansu Province, China(No.1210RJIA001) and the Program of Innovation and Entrepreneurial for Talent in Lanzhou, China(No.2014-RC-39)

摘要/Abstract

摘要：

采用电化学还原技术, 通过一步电沉积制备了石墨烯-金纳米粒子复合膜修饰电极(ERGO-Au/GCE). 采用透射电子显微镜(TEM)和循环伏安(CV)法对修饰电极进行了表征, 并研究了双酚A(BPA)在该修饰电极上的电化学行为. 结果表明, 所制备的复合物修饰电极对双酚A有明显的电催化效果. 在pH=6.0的磷酸盐缓冲溶液中, 双酚A在0.3~1.0 V扫描电位范围内有1个不可逆的氧化还原峰出现. 在优化的条件下, 双酚A的浓度在3.00×10^-8~1.30×10^-5 mol/L范围内与其氧化峰电流呈线性关系, 检出限为1.0×10^-8 mol/L(S/N=3). 将该修饰电极用于饮用水和塑料制品中双酚A含量的测定, 回收率为96.4%~103.5%.

关键词: 金纳米粒子, 石墨烯, 双酚A, 修饰电极

Abstract:

A graphene-Au nanocomposite film(ERGO-Au) modified electrodewas prepared using coelectrodeposition technique. The morphology and electrochemical properties of this hybrid membrane were characte-rized by means of transmission electron microscopy(TEM) and cyclic voltammetry(CV), respectively. The electrocatalytic activity of ERGO-Au nanocomposite for the electrooxidation of bisphenol A(BPA) was also investigated. The cyclic voltammetry of bisphenol A on the modified electrode exhibits a well defined irreversible anodic peak. Under the optimum conditions, the oxidation peak current was proportional to bisphenol A concentration in the range from 3.0×10^-8 mol/L to 1.30×10^-5 mol/L. The limit of detection(LOD) is 1.0×10^-8 mol/L(S/N=3). The proposed method was applied for detection of bisphenol A in tap water and plastic products. The described sensor was used for the determination of BPA in tap water and plastic products with good recovery, ranging from 96.4% to 103.5%.

Key words: Gold nanoparticles, Graphene, Bisphenol A, Modified electrode

中图分类号:

O657.1

TrendMD:

方燕, 马琳琳, 陕多亮, 卢小泉. 石墨烯-金纳米粒子复合膜修饰电极的制备及对双酚A的测定. 高等学校化学学报, 2015, 36(8): 1491.

FANG Yan, MA Linlin, SHAN Duoliang, LU Xiaoquan. Preparation of Graphene/Gold Nanoparticle Composite Film Modified Electrode and Its Application for Determination of Bisphenol A^†. Chem. J. Chinese Universities, 2015, 36(8): 1491.

图/表 11

Scheme 1 Preparation of the ERGO-Au/GCE

Fig.1 TEM image of ERGO-Au composite film

Fig.2 Cyclic voltammetry(CV) curves of the ERGO/GCE(a) and ERGO-Au/GCE(b) in 0.5 mol/L H2SO4 solution

Fig.3 CV curves of the bare GCE(a), ERGO/GCE(b) and ERGO-Au/GCE (c) in 0.1 mol/L KCl solution containing 1.0 mmol/L [Fe(CN)6]3-/4-

Fig.4 CV curves of bare GCE(a), ERGO/GCE(b) and ERGO-Au/GCE(c) in 0.1 mol/L PBS containing 5.0×10-5 mol/L BPA

Fig.5 Effect of the polymerization cycles(n) on the oxidation peak currents of 3.0×10-5 mol/L BPA

Fig.6 CV curves of ERGO-Au/GCE in PBS solutions(0.1 mol/L) with different pH values(4.0—8.0) containing 5.0×10-4 mol/L BPA(A), influences of pH on the oxidation peak currents(B) and the oxidation peak potentials of BPA(C)

Fig.7 CV curves for the 1.0×10-5 mol/L BPA in PBS(pH=6.0) on the ERGO-Au/GCE with different scan rates(A) and plot of peak current density vs. scan rate for BPA(B)Scan rate/(mV·s-1): a. 20; b. 60; c. 100; d. 140; e. 180; f. 220; g. 260; h. 300.

Fig.8 Effects of accumulation potential(A) and accumulation time(B) on the oxidation peak currents of 5.0×10-5 mol/L BPA

Fig.9 DPV curves of BPA on the ERGO-Au/GCE in 0.1 mol/L PBS(pH=6.0) containing different concentrations of BPA(A) and plots of the peak current vs. the concentration of BPA(B)c/(mol·L-1): a. 0; b. 3.00×10-8; c. 1.00×10-7; d. 5.99×10-7; e. 2.09×10-6; f. 3.24×10-6; g. 5.02×10-6; h. 7.12×10-6; i. 9.00×10-6; j. 1.10×10-5; k. 1.30×10-5.

Table 1 Determination of BPA in practical samples*

Sample	Measured/(mol·L^-1)	Added/(mol·L^-1)	Found/(mol·L^-1)	RSD(%)	Recovery(%)
Tap water	-	5.00×10^-6	4.82×10^-6	3.3	96.4
Baby’s nipple	-	5.00×10^-6	4.93×10^-6	3.5	98.6
PP cup	-	5.00×10^-6	5.18×10^-6	4.1	103.5

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石墨烯-金纳米粒子复合膜修饰电极的制备及对双酚A的测定

Preparation of Graphene/Gold Nanoparticle Composite Film Modified Electrode and Its Application for Determination of Bisphenol A^†

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石墨烯-金纳米粒子复合膜修饰电极的制备及对双酚A的测定

Preparation of Graphene/Gold Nanoparticle Composite Film Modified Electrode and Its Application for Determination of Bisphenol A†

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Preparation of Graphene/Gold Nanoparticle Composite Film Modified Electrode and Its Application for Determination of Bisphenol A^†