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山东大学学报(工学版) ›› 2010, Vol. 40 ›› Issue (6): 94-99.

• 化学与化工 • 上一篇    下一篇

自组装3-氨丙基三甲氧基硅烷-磷钼酸膜修饰电极

魏培海,刘光增,张琦,石聪文   

  1. 齐鲁师范学院化学系, 山东 济南 250013
  • 收稿日期:2010-05-07 出版日期:2010-12-16 发布日期:2010-05-07
  • 作者简介:魏培海(1965-),男,山东平原人,教授,博士,主要研究方向为电化学分析、毛细管电泳. E-mail:weipeihai@163.com
  • 基金资助:

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

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

WEI Pei-hai, LIU Guang-zeng, ZHANG Qi, SHI Cong-wen   

  1. Department of Chemistry, Qilu Normal University, Jinan 250013, China
  • Received:2010-05-07 Online:2010-12-16 Published:2010-05-07

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。

关键词: 杂多酸, 3-氨丙基三甲氧基硅烷, 自组装膜, 修饰电极

Abstract:

 A composite film modified glassy carbon electrode containing heteropolyanion was fabricated by attaching a Keggin—type heteropolyanion, H3(PMo12O40)·H2O, to a 3-aminopropyltrimethoxysilane (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 PMo12O403- was linked with APMS through the coulombic interaction between PMo12O403-and amine groups of APMS (PMo12O403--APMS), which greatly improved the film stability. The PMo12O403--APMS modified electrode showed three reversible redox pairs of PMo12O403- 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 PMo12O403- 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.

Key words: phosphomolybdic acid, 3-aminopropyltrimethoxysilane, self-assembled film, modified electrode

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