汞滴电极上的张力电化学测量及电化学池内电位降落补偿新方法的研究分析化学专业论文.docxVIP

中困科学技术人学博I：学位论义 中困科学技术人学博I：学位论义 摘要 补充。比较了不同电化学极化模式与采样方法下的界面张力电化学测量方法发 现，NPV法具有较高的灵敏度，因而在研究微量物质的吸附方面明显优于LSV 法的极化模式。 发展了电位降落的池内补偿方法，采用辅助工作电极接地的方法首次得到了 无振荡影响的100％补偿及过补偿。并用CV、SWV币llI--t等不同的电化学技术验 证了池内方法补偿的『F确性。实验结果表明，多种电化学技术都证明了采用池内 补偿的方法能够得到满意的100％补偿和过补偿。对影响补偿效果的因素进行了 探讨。实验结果表明，任何能够增加反馈电流的因素都可以提高补偿效果；影响 反馈电阻的因素为电解池的尺寸、LwE．RP的大小和电解液的性质，儿是能够增大 反馈电阻的因素皆可增加补偿的效率。对诸如电极的材质、电极在电化学池中摆 放的位置以及电解池的形状等其它能够影响补偿效果的因素进行了实验验证和 初步分析。该方法的建立为实现电位降落的补偿提供了一条可供选择的新途径。 初步进行了电位降落池内补偿方法的应用研究。采用本方法可以进行峰电位 相近物质的分离检测、提高电化学检测的灵敏度和线性范围，并可应用于无支持 电解质溶液的电化学参数的测量，为电分析化学和电化学的研究提供了一种新手 段。 V ABSTRACTTwo ABSTRACT Two subjects，in—situ measurement of electrochemical interfacial tension and in-cell iRu compensation，have been investigated in detailed． The first part of this dissertation includes four chapters．The theory and technology of interfacial tension measuring was reviewed in Chapter 1．In Chapter 2， setup for the measurement of interfacial tension a mercury drop electrode(MDE) sitting on the bottom of an electrochemical was designed，and characterized．In Chapter 3 and 4，series investigations on three chemical systems were studied，data were treated for obtaining thermodynamic parameters of the adsorption，and analyzing the mechanism of molecular adsorption，orientation and electrochemical reactions．In the second part，the technology of compensating the solution’S resistance was reviewed in Chapter 5，then an in-cell compensating technique was developed by adding a grounded auxiliary working electrode(AWE)to electrochemical cell，the experimental verification and investigation of factors influenced the compensation were studied．Following results were obtained By combining a home—made interfacial tension electrode，electrochemical cell and an electrochemical working station，in—situ and continuous interfacial tension curves at MDE／solution interface was obtained simultaneously with voltam