荧光（反射）光谱电化学和电化学石英晶体微天平新方法及其初步应用
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摘要
光谱电化学(SEC)将光谱学和电化学结合起来，具有比经典电化学更好的选择性，且提供了在分子或原子水平上研究电极表面过程及机理的可能；电化学石英晶体微天平(EQCM)技术将压电传感器用与电化学联用，能现场监测电化学过程中伴随的质量效应，其监测下限低至纳克级；压电光谱电化学是将压电与光谱电化学技术有机结合的新技术，能现场提供压电、光谱、电化学多维信息，有助于对实际体系的深入了解。
本文在文献基础上，在荧光(反射)光谱电化学及压电-荧光光谱电化学联用新方法及应用等方面做了一些探索性的工作。
1．综述了光谱电化学及压电光谱电化学研究近年相关文献。
2．建立了单电位阶跃计时荧光法(SPS／CF)测定异相电子转移动力学参数的理论模型，据此测定了邻联甲苯胺在1mol l~(-1) HClO_4+0.5mol l~(-1) HAc溶液中电氧化过程的标准速率常数(K_s)和电子转移系数(α)，结果与常规的计时库仑法测定的结果吻合。结果表明该模型推广到循环伏安法也是可行的。
3．提出了一种将荧光、石英晶体微天平(QCM)和电化学技术有机结合的新方法，并用该方法研究了盐酸吡哆醇在碱性条件下金电极上的吸附／脱附及电化学行为。另外，建立了伏安电生荧光法用于测定药剂中盐酸吡哆醇含量，结果满意。
4．提出了一种将反射光谱、石英晶体微天平(QCM)和电化学技术有机结合的新方法，初步用于监测吡咯、氮甲基吡咯的聚合及聚合膜氧化还原过程中电流(I)、反射强度(RI，)、共振频率(Δf_0)、动态电阻
(△Rl)的响应，结果满意
荧光反射，QCM频率，
界面表面现象有一定意义
。我们认为这种实验技术能同时原位获得
阻抗，电化学等多维数据，对于现场研究
Spectroelectrochemistry (SEC), which is the combination of spectroscopy and electrochemistry, is of higher selectivity than conventional electrochemisty and feasible to investigate the electrochemical process at the molecular or atomic level. Electrochemical piezoelectric quartz crystal microbalance (EQCM) provides a useful tool for in situ measuring concurrent mass loading on the electrode surface by using a piezoelectric crystal sensor in electrochemical processes. Piezoelectric Spectroelectrochemistry, which combines piezoelectric sensor with Spectroelectrochemistry, can provide piezoelectric, spectral and electrochemical information in one experiment and thus lead to less ambiguity in the description of a practical electrochemical process.
The studies in the thesis are summarized as follows:
1. The recent progress of Spectroelectrochemistry and piezoelectric Spectroelectrochemistry researches is reviewed
2. The theory underlying the single potential-step chronofluorometric (SPS/CF) determination of heterogeneous electron transfer rate constants using a long optical pathlength spectroelectrochemical cell has presented. The resulting expressions have been verified via experiments of o-tolidine oxidation at a platinum electrode in 1 M HC1O4+ 0.5 M HAc medium. Results show that a modification of the present model to
fit cyclic voltammetry is also feasible.
3. A simultaneous EQCM-fluorescence method has been proposed as a novel and informative tool for the study of adsorption/desorption and oxidation for vitamin Be (pyridoxol) at a polycrystalline Au electrode in aqueous KOH. In addition, the voltammetrically electrogenerated fluorescence is proposed as a new and sensitive method for assay of pyridoxol with satisfactory results.
4. Piezoelectric reflectance spectroelectrochemistry (PRSEC), a new technique of SEC in combination with QCM detection, has been proposed. The simultaneous measurements of reflectance spectra on the electrode surface, the QCM frequency and resistance as well as the electrochemical signals have been performed during growth and redox switching of polypyrrole and poly(N-methylpyrrole) film. This technique can provide in situ multidimensional information in an electrochemical process and is thus recommended for wider applications to surface/interface phenomena studies.
本文在文献基础上，在荧光(反射)光谱电化学及压电-荧光光谱电化学联用新方法及应用等方面做了一些探索性的工作。
1．综述了光谱电化学及压电光谱电化学研究近年相关文献。
2．建立了单电位阶跃计时荧光法(SPS／CF)测定异相电子转移动力学参数的理论模型，据此测定了邻联甲苯胺在1mol l~(-1) HClO_4+0.5mol l~(-1) HAc溶液中电氧化过程的标准速率常数(K_s)和电子转移系数(α)，结果与常规的计时库仑法测定的结果吻合。结果表明该模型推广到循环伏安法也是可行的。
3．提出了一种将荧光、石英晶体微天平(QCM)和电化学技术有机结合的新方法，并用该方法研究了盐酸吡哆醇在碱性条件下金电极上的吸附／脱附及电化学行为。另外，建立了伏安电生荧光法用于测定药剂中盐酸吡哆醇含量，结果满意。
4．提出了一种将反射光谱、石英晶体微天平(QCM)和电化学技术有机结合的新方法，初步用于监测吡咯、氮甲基吡咯的聚合及聚合膜氧化还原过程中电流(I)、反射强度(RI，)、共振频率(Δf_0)、动态电阻
(△Rl)的响应，结果满意
荧光反射，QCM频率，
界面表面现象有一定意义
。我们认为这种实验技术能同时原位获得
阻抗，电化学等多维数据，对于现场研究
Spectroelectrochemistry (SEC), which is the combination of spectroscopy and electrochemistry, is of higher selectivity than conventional electrochemisty and feasible to investigate the electrochemical process at the molecular or atomic level. Electrochemical piezoelectric quartz crystal microbalance (EQCM) provides a useful tool for in situ measuring concurrent mass loading on the electrode surface by using a piezoelectric crystal sensor in electrochemical processes. Piezoelectric Spectroelectrochemistry, which combines piezoelectric sensor with Spectroelectrochemistry, can provide piezoelectric, spectral and electrochemical information in one experiment and thus lead to less ambiguity in the description of a practical electrochemical process.
The studies in the thesis are summarized as follows:
1. The recent progress of Spectroelectrochemistry and piezoelectric Spectroelectrochemistry researches is reviewed
2. The theory underlying the single potential-step chronofluorometric (SPS/CF) determination of heterogeneous electron transfer rate constants using a long optical pathlength spectroelectrochemical cell has presented. The resulting expressions have been verified via experiments of o-tolidine oxidation at a platinum electrode in 1 M HC1O4+ 0.5 M HAc medium. Results show that a modification of the present model to
fit cyclic voltammetry is also feasible.
3. A simultaneous EQCM-fluorescence method has been proposed as a novel and informative tool for the study of adsorption/desorption and oxidation for vitamin Be (pyridoxol) at a polycrystalline Au electrode in aqueous KOH. In addition, the voltammetrically electrogenerated fluorescence is proposed as a new and sensitive method for assay of pyridoxol with satisfactory results.
4. Piezoelectric reflectance spectroelectrochemistry (PRSEC), a new technique of SEC in combination with QCM detection, has been proposed. The simultaneous measurements of reflectance spectra on the electrode surface, the QCM frequency and resistance as well as the electrochemical signals have been performed during growth and redox switching of polypyrrole and poly(N-methylpyrrole) film. This technique can provide in situ multidimensional information in an electrochemical process and is thus recommended for wider applications to surface/interface phenomena studies.
引文
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