铋膜电极阳极溶出伏安法检测痕量Cd金属

doi:10.15541/jim20180169

摘要/Abstract

摘要：

镉氧化产生的溶出电流与样品中Cd²⁺的浓度有关。本研究通过方波阳极溶出伏安法(SWASV)在活化铋膜电极(Activated BFE)上对低浓度μg/L水平的Cd(II)进行测定。通过电化学方法对电极进行初步改性, 然后电沉积制备铋膜再次对电极进行改进, 从而增强了对痕量目标Cd²⁺的敏感性。对改性前后的玻碳电极(GCE)表面进行SEM、CV、EIS和SWV的表征。为了将这种伏安法传感器应用于含有低浓度Cd²⁺的实际样品中, 对检测Cd²⁺的实验参数进行了研究。使用选定的条件, 在10 min的预富集条件下Cd²⁺的检测限为1 μg/L。

关键词: 铋膜, 阳极溶出伏安法, 化学修饰电极, 电化学检测, 镉离子

Abstract:

The stripping current arising from the oxidation of Cd was related to the concentration of Cd²⁺ in the sample. This study presents the determination of Cd(II) at low concentration μg/L levels by square wave anodic stripping voltammetry (SWASV) on an activated bismuth-film electrode (BFE). The electrode was initially modified by an electrochemical method, and then the electrodeposited bismuth-film was prepared again to improve the electrode, thereby enhancing the sensitivity to trace amounts of target Cd²⁺. The surface of glassy carbon electrode (GCE) before and after modification was characterizad by SEM, CV, EIS, and SWV. The parameters for the determination of the Cd²⁺ were investigated with the view of its application toward real samples containing low concentrations of Cd²⁺. Using the selected conditions, the limit of detection is 1 μg/L for Cd²⁺ at a preconcentration time of 10 min.

Key words: bismuth-film, anodic stripping voltammetry, chemically modified electrode, electrochemical detection, Cd²⁺

中图分类号:

TQ174

要美娜, 杨贤金, 崔振铎, 朱胜利, 李朝阳, 梁砚琴. 铋膜电极阳极溶出伏安法检测痕量Cd金属[J]. 无机材料学报, 2019, 34(1): 91-95.

YAO Mei-Na, YANG Xian-Jin, CUI Zhen-Duo, ZHU Sheng-Li, LI Zhao-Yang, LIANG Yan-Qin. Detection of Cd²⁺ by Square Wave Anodic Stripping Voltammetry Using an Activated Bismuth-film Electrodes[J]. Journal of Inorganic Materials, 2019, 34(1): 91-95.

图/表 4

图1 三种不同电极的SEM照片

Fig. 1 SEM images of the three Electrodes (a) I; (b) Ⅱ; (c) Ⅲ

图2 (A)在0.1 mol/L KCl中(a)裸露、(b)活化、(c)铋膜修饰和(d)活化后铋膜修饰的玻碳电极表面处5 mmol/L [Fe(CN)6]3-/4-的循环伏安图(扫描速率: 50 mV/s); (B)相同条件下不同电极的奈奎斯特图

Fig. 2 (A) Cyclic voltammograms of 5 mmol/L [Fe(CN)6]3-/4- in 0.1 mol/L KCl: (a) GCE, (b) activated GCE, (c) Bi/GCE and (d) activated Bi/GCE (Scan rate: 50 mV/s); (B) Nyquist plots of different electrodes under the same conditions

图3 用活化的Bi/GCE研究Bi(III)浓度对Cd(II)溶出峰电流的影响

Fig. 3 Effect of Bi(III) concentration on the stripping peak current of Cd(II) using activated Bi/GCE

图4 (A)不同浓度的Cd(II)在活化铋膜电极上的方波阳极溶出伏安图, (B)Cd2+的线性校准曲线

Fig. 4 (A) Square-wave anodic stripping voltammograms for different concentrations of Cd(II) on the bismuth-film electrode, (B) the linear calibration curves of Cd2+

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