摘要/Abstract
电化学反应是连续的动态变化过程,伴随着瞬时中间体和复杂结构物质的产生,因此,精确而有效地捕捉反应过程中的一系列产物,有助于准确推导其电化学反应机理,进而优化反应条件,提高反应效率.目前,主流的电化学在线监测技术包括光谱法、循环伏安法和线性极化曲线等,这些方法能够胜任反应过程中大部分物质的结构及组成变化检测,然而,为了更加系统和精确地掌握电化学反应过程中所有产物的信息,仍需进一步拓展实时、原位反应监测技术.质谱具有灵敏度高、选择性好、分析速度快、可以结构解析等特点,是一种理想的电化学反应研究手段.近年来,采用质谱法研究电化学反应机理的报道越来越多,尤其是采用以电喷雾离子源(Electrospray Ionization,ESI)及其衍生离子源为代表的常压离子源对电化学反应过程进行实时、原位监测已经成为研究热点.本综述主要介绍了近期发表的电化学-质谱联用技术,详细描述了其针对不同类型电化学反应监测要求而设计和开发的电化学离子源装置.
关键词: 电化学, 质谱, 微分电化学质谱, 电喷雾质谱, 敞开式离子源, 反应监测
Electrochemical reaction is a continuous dynamic process, accompanied by generation of short-lived intermediates and complex structural substances. Therefore, precisely and effectively capturing the products of the reaction process is helpful to accurately deduce its reaction mechanism, optimize the reaction parameters and improve the reaction efficiency. At present, the mainstream electrochemical on-line monitoring techniques include spectroscopy, cyclic voltammetry and linear polarization curves. These methods are capable to detect the structure and composition changes of most substances in the reaction process. However, in order to more systematically and accurately grasp the information of all products, the real-time and in situ reaction monitoring technologies needs to be further expanded. Mass spectrometry (MS) has the advantages of high sensitivity, good selectivity, rapid response time and structural analysis, making itself an ideal research method for electrochemical reactions. In recent years, more and more reports on the study of electrochemical reaction by MS have been published. In particular, ambient ionization sources such as electrospray ionization (ESI) and its derived ionization techniques developed for electrochemistry have become a research hotspot. This review introduced the recently published electrochemistry-mass spectrometry (EC-MS) techniques, and described the electrochemical ion sources that designed and developed for different types of electrochemical reactions.
Key words: electrochemistry, mass spectrometry, differential electrochemical mass spectrometry, electrospray ionization, ambient ionization, reaction monitoring
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