石墨烯/纳米氧化铝修饰电极方波阳极溶出伏安法测定土壤中锑  

Determination of antimony in soil by square wave anodic stripping voltammetry based on graphene/nano-aluminum oxide modified electrode

作　　者：徐俊晖[1] 胡思泉[1] 鲁珍[1] 王亚珍[1] XU Jun-hui;HU Si-quan;LU Zhen;WANG Ya-zhen(Hubei Key Laboratory of Industrial Fume & Dust Pollution Control, School of Chemistry and EnvironmentalEngineering, Jianghan University, Wuhan 430056, China)

机构地区：[1]江汉大学工业烟尘污染控制湖北省重点实验室/化学与环境工程学院,湖北武汉430056

出　　处：《冶金分析》2020年第6期37-42,共6页Metallurgical Analysis

基　　金：工业烟尘污染控制湖北省重点实验室开放基金(HBIK2019-02);武汉研究院开放性课题(IWHS20192089)。

摘　　要：锑是一种有毒且应用广泛的工业添加剂,但锑是可疑致癌物,对人体及环境生物具有毒性作用,因此锑含量的测定是环境评价的必然要求。实验制备了一种石墨烯/纳米氧化铝复合膜修饰电极,探讨了Sb(Ⅲ)在该修饰电极上的伏安溶出特性,建立了方波溶出伏安法测定Sb(Ⅲ)的方法。该复合膜呈疏松多孔结构,具有较大的比表面积和良好的导电性,对Sb(Ⅲ)具有灵敏的电化学响应。在优化的实验条件下,溶出峰电流与Sb(Ⅲ)浓度在1.0×10^-7~1.0×10^-5 mol/L范围内呈良好的线性关系,检出限为1×10^-7 mol/L。对某工厂周边土壤样品微波消解处理后,采用方波阳极溶出伏安法测定了锑含量,结果的相对标准偏差(RSD,n=6)为3.1%~3.9%;土壤样品中锑的含量在0.901~1.290mg/kg;与原子吸收光谱法的测量结果进行对比,一致性较好。Antimony is a toxic metal element which is widely used as industry additive.It is one of suspected carcinogens and has toxic effect on human body and environmental biology.Therefore,the determination of antimony is the necessary requirement for environmental evaluation.A kind of graphene/nano-Al2O3 composite film modified electrode was prepared.The voltammetric stripping characteristics of Sb(Ⅲ)on this modified electrode were discussed.The determination method of Sb(Ⅲ)by square wave anodic stripping voltammetry was established.This composite film had loose and porous structure,and it exhibited large specific surface area and good electrical conductivity.The electrode had sensitive electrochemical response to Sb(Ⅲ).Under the optimized experimental conditions,the striping peak currents were linear with the concentration of Sb(Ⅲ)in the range of 1.0×10^-7-1.0×10^-5 mol/L.The limit of detection was 1×10^-7 mol/L.The soil samples from surroundings of one factory were treated by microwave digestion.The content of antimony was determined by square wave anodic stripping voltammetry.The relative standard deviations(RSD,n=6)were between 3.1%and 3.9%.The measured content of antimony in soil sample was in range of 0.901-1.290mg/kg,which was consistent with those obtained by atomic absorption spectrometry.

关 键 词：阳极溶出伏安法 纳米氧化铝 石墨烯 修饰电极 土壤 锑 

分 类 号：O657.1[理学—分析化学]