聚邻苯二胺/镍氢氧化物修饰电极的研究  

Investigation of nickel hydroxide/poly-o-phenylenediamine modified electrode

作　　者：刘有芹[1] 乐文志[1] 颜芸[1] 徐悦华[1] 田秀英[1] 

机构地区：[1]华南农业大学理学院生物材料研究所,广东广州510642

出　　处：《化学研究与应用》2011年第6期661-666,共6页Chemical Research and Application

基　　金："211工程"重点学科建设项目(2009B010100001)资助;广东省自然科学基金博士科研启动基金资助项目(5300842)

摘　　要：采用循环伏安法（CV）在聚邻苯二胺修饰玻碳电极表面络合Ni2＋,然后将其置于NaOH溶液中CV扫描成功制备了镍氢氧化物/聚邻苯二胺/玻碳修饰电极（Ni（OH）2/PoPD/GC）。通过CV探讨了聚合和负载机理,电化学交流阻抗谱（EIS）表征了电极修饰过程中界面阻抗变化,扫描电镜表征了PoPD膜负载Ni（OH）2后的形态结构。发现负载Ni（OH）2后界面电子传递阻抗显著减小,CV和CA（计时电流法）结果表明Ni（OH）2/PoPD/GC电极对H2O2氧化有显著的电催化活性,H2O2氧化峰电位0.4 V,起始氧化电位低至0.1 V。对H2O2电催化氧化的线性方程：Δi/μA=1.621＋0.332c/μmol/L（R=0.9976,n=17）,线性范围：2.4×10-7~7.2×10-5mol/L,检出限：3.6×10-8mol/L（3S/k）。考察了制备条件对Ni（OH）2/PoPD/GC电极电催化活性的影响,最佳Ni2＋络合扫描次数为20、浓度为5 mmol/L。该复合材料修饰电极制备方法简单、可控,电极灵敏度高、稳定性好,可用于实际样品中H2O2测定。A nickel hydroxide loaded poly-o-phenylenediamine film modified glassy carbon electrode（Ni（OH）2/PoPD/GC） was successfully prepared.First,Ni2＋was complexed on PoPD/GC electrode surface in phosphate buffer solution by cyclic voltammetry（CV）,then the Ni2＋-PoPD/GC electrode was scanned in NaOH solution by CV.The mechanism of polymerization and loading was discussed by CV.The impedance changes of GC electrode surface during the modification process were characterized by electrochemical AC impedance spectroscopy and the surface morphology of Ni（OH）2/PoPD film was characterized by scanning electron microscope,finding that the interface electron transfer resistance significantly reduced after the load of Ni（OH）2 on PoPD film.The results of CV and CA（chronoamperometry） showed that Ni（OH）2/PoPD/GC electrode had significant electrocatalytic activity toward H2O2 oxidation.The oxidation peak potential of H2O2 is 0.4 V and initial oxidation potential is as low as 0.1 V.The linear regression equation for H2O2 oxidation was Δi/μA = 1.621＋0.332c/μmol/L（R=0.9976,n=17） and the linear range was 2.4×10-7~7.2×10-5mol/L with a detection limit of 3.6×10-8mol/L（3S/k）.The factors influencing the electrocatalytic activity of Ni（OH）2/PoPD/GC electrode were investigated,showing that the optimal scanning number for Ni2＋ complexing was 20 and Ni2＋ concentration was 5 mmol/L.The preparation process of Ni（OH）2/PoPD/GC composite electrode is simple and manageable,which has high sensitivity and good stability and can be used for H2O2 determination in actual sample.

关 键 词：邻苯二胺 镍氢氧化物 玻碳电极 过氧化氢 电催化 

分 类 号：O657.1[理学—分析化学]