自组装3-氨丙基三甲氧基硅烷-磷钼酸膜修饰电极  

Self-assembled 3-aminopropyltrimethoxysilane-phosphomolybdic acid film modified electrode

作　　者：魏培海[1] 刘光增[1] 张琦[1] 石聪文[1] 

机构地区：[1]齐鲁师范学院化学系,山东济南250013

出　　处：《山东大学学报（工学版）》2010年第6期94-99,共6页Journal of Shandong University（Engineering Science）

基　　金：山东省优秀中青年科学家科研奖励基金资助项目(2008BS04031)

摘　　要：通过在C—O—Si键在电化学活化玻碳电极表面自组装3-氨丙基三甲氧基硅烷(3-aminopropyltrimethoxysilane,APMS),再于其表面连接Keggin型结构杂多酸阴离子PMo12O403-,制备了复合膜修饰玻碳电极,采用XPS和循环伏安法研究了复合膜的基本性质。结果表明,PMo12O403-通过库仑作用力与APMS的表面—NH2结合(PMo12O403--APMS),可极大提高电极的稳定性,与溶液中的PMo12O403-相比,PMo12O403--APMS修饰电极表现出具有较小峰-峰分裂的PMo12O403-的三对可逆氧化还原过程,并能在较大pH范围内保持稳定。研究了修饰电极对ClO3-、BrO3-、IO3-还原的催化性能,与PMo12O403-修饰玻碳电极相比,该电极对三种离子均具有良好的电催化活性,对应的检出限分别为1.5×10-5、1.0×10-6、5×10-7mol/L。A composite film modified glassy carbon electrode containing heteropolyanion was fabricated by attaching a Keggin-type heteropolyanion, H3 （PMo12O40） · H2O, to a 3-aminopropyltrirnethoxysilane （ APMS ） layer, which was self-assembled on an electrochemically activated glassy carbon electrode through the formation of C-O-Si bond. XPS and cyclic voltammetry were used for the characterization of the composite film. The results showed that PMo12O40^3- was linked with APMS through the coulombic interaction between PMo12O40^3- and amine groups of APMS （ PMo12O40^3- -APMS ）, which greatly improved the film stability. The PMo12O40^3- -APMS modified electrode showed three reversible redox pairs of PMo12O40^3- with a smaller peak-to-peak separation, which was stable in a larger pH range compared with that in the solution phase. The catalytic properties of the modified electrode for those reduction of ClO3^ - ,BrO3^ - and IO3^- were studied. The modified electrode exhibited better electrocatalytic activities for those three anions compared with the PMo12O40^3- modified glassy carbon electrode. The detection limits were 1.5×10^-5, 1.0×10^-6, 5×10^-7mol/L for ClO3^ - ,BrO3^ - and IO3^- seperately.

关 键 词：杂多酸 3-氨丙基三甲氧基硅烷 自组装膜 修饰电极 

分 类 号：O646[理学—物理化学]