【作者】 于海琴；

【导师】 周长利；

【作者基本信息】 南京工业大学 ， 应用化学， 2002， 硕士

【摘要】 本文详细介绍了配位吸附波的特点、分类和形成条件，概述了配位吸附波在分析化学中的应用研究、现状和趋势。在此基础上，系统地研究了Pb（Ⅱ）、In（Ⅲ）与二溴邻苯二胺双草酰胺（dbac）、N-邻羧基苯基-N′-（2-氨基乙基）草酰胺（opac）两种配位体形成的配位吸附波体系的电化学行为，并应用于实际样品的测定。本文主要包括以下四部分： 一．草酰胺电化学行为研究 应用示波极谱法、循环伏安法等实验技术研究了二溴邻苯二胺双草酰胺（dbac）和N-邻羧基苯基-N′-（2-氨基乙基）草酰胺（opac）两种试剂在汞电极上的电化学行为。通过测定吸附量确定了dbac、opac吸附模式，讨论了试剂的电极反应机理和取代基效应对吸附性和电活性影响。研究表明，dbac、opac在一定的底液中均能产生2e不可逆吸附还原峰，其极谱行为受pH影响较大。两者在汞电极上都具有较强的吸附性，且符合Frumkin吸附等温式。 二．Pb（Ⅱ）、In（Ⅲ）-二溴邻苯二胺双草酰胺（dbac）配合物电化学行为研究 在本章中，以dbac为配位体，研究了Pb（Ⅱ）、In（Ⅲ）与其形成的配合物的电化学行为。确定了以下两种配位吸附波体系：①Pb（Ⅱ）-dbac体系。②In（Ⅲ）-dbac体系。对这两种体系系统地进行了机理研究和理论探讨。 1．研究了两种体系配位吸附波的形成和影响因素。结果表明，底液在形成配位吸附波时起着重要作用。为了得到灵敏的极谱波，应遵循一定的原则选择底液。底液的组成及浓度，溶液pH，配体浓度和仪器条件通常会对峰电流产生很大影响。 2．通过各种电化学、光化学实验技术研究了配合物的稳定性、吸附性和电活性，探讨了电极反应机理，比较和讨论了金属离子、配位体对配位吸附波的影响。结果表明，两体系电极过程均符合配位吸附波的CAEM过程。 3．线性范围和检出限。通过大量的条件实验，选择了两体系测定金属离子的最佳条件，建立了示波极谱法测定Pb（Ⅱ）、In（Ⅲ）两种离子的分析方法。线性范围在10^-6～10^-8mol／L，检出限可达10^-8mol／L。方法具有灵敏度高、选择性好、操作简便、快捷等特点。 摘 要 三．In（lll）－一邻波基苯基一N’一口一氨基乙基)草酸胺（opa）配合物电化学行为研究 研究了In（ll）与opac形成的配位吸附波及影响因素。通过对电活性配合物的稳定性、吸附性和电活性研究，探讨了电极反应机理。在大量实验基础上，确定了该体系最佳条件，建立了配位吸附波测定 n0)的新方法。检出限为 SX10－smp皿，线性范围在10－5一 10”7mo凡之间。 四．应用研究 介绍了电化学分析测定Ph（II、In＊）的研究现状，重点叙述了配位吸附波测定PhOIXIn（Ill）的研究进展。首次将草酸胺Nbac、opac闯入配位吸附波领域，建立了测定Ph(II、In(lll的新方法，实现了Ph（11）、In（Ill）的同时狈定。用于陶瓷颜料、矿石及人发样品的测定，结果令人满意。更多还原

【Abstract】 The thesis reviews the basic theories of adsorption wave, introduces the characterisitics, classification and formation conditions of the complex adsorption wave. Its applications in various fields of analytical chemistry were described .On the basis of that, the electrochemical behavior and applications of the complex of Lead(Ⅱ),Indium(Ⅲ) metal ions with dibrom-o-benzenediamine-diacetamide ester(dbac) and N-o-carboxypheny-N’-(2-aminoethyl) acetamide(opac) have been studied systematically. The thesis consists of the following four parts:1. Study on the electrochemical behavior of acetamideThe electrochemical behavior of dibrom-o-benzenediamine-diacetamide ester(dbac) and N-o-carboxypheny-N’-(2-aminoethyl) acetamide(opac) on the mercury electrode have been studied by many electrochemical experiments such as oscillopolarography, cyclic voltammetry, etc. The adsorption modes of dbac and opac were found by determination of adsorption amount. The mechanism of the electrode process and the effects of displacement group on the ability of adsorption and the electroactivity were discussed. The experimental results shows that the adsorption reduce wave of dbac and opac produced in suitable supporting electrolyte. The effect of pH on the polarographic behavior of the agent was large. The interfacial electrochemical reduction of the agent was an irreversible process with two electron. Two agents have strong adsorption on the mercury electrode, the adsorption modes correspond to Frumkin adsorption isotherm.2. Study on the electrochemical behavior of the complex of Pb(II), In(III) metal ions with dbacIn this chapter, the electrochemical behavior of the complex of Pb(Ⅱ), In(Ⅲ) metal ions with dbac has been investigated. The following Pb(Ⅱ)-dbac system and In(Ⅲ)-dbac system were determined:On the base, he following theoretical has been studied:(1). The formation and influence factors of complex adsorption wave have been investigated. The results demonstrated that the supporting electrolyte is important to formingcomplex adsorption wave, and its selection should obey certainly principles.The effects of composition and concentration of supporting electrolyte, pH, the concentration of complexant and apparatus conditions, etc, on the peak current are great.(2). The mechanism of electrode reaction was discussed through studying the stability,adsorption and electroactivity of complex in systems mentioned above. The effects of metal ions and complexants on the complex adsorption wave were compared and discussed. Results demonstrated that the electrode process of complex corresponded with CAEM process of complex adsorption wave.(3). The liner range and the limit of detection. The optimized analytical conditions were selected and oscillopolarography of the determination of Pb(Ⅱ), In(Ⅲ) have been found. Thelinear range was 10-6 ~10-8 mol/L. The limit of detection was general 10-8 mol/L.3. Study on the electrochemical behavior of the complex of In(Ⅲ) metal ions with opacThe formation and influence factors of complex adsorption wave have been investigated. The mechanism of electrode reaction was discussed through studying the stability, adsorption and electroactivity of complex based on numerous experiments the optimized condition and oscillopolarography of determination of In(III) have been found. In general,the limit ofdetection and the linear range were 5.0 10-8 mol/L and 10-5~10-7 mol/L respectively.4. Analytical applicationsThis part focuses on the current sitiuation of the electrochemical analysis to determination Lead(Ⅱ), Indium(Ⅲ), and mainly on the development of reseach on the complex adsorption wave to determination Lead(Ⅱ), Indium(Ⅲ). In addition, the new method of determinating Lead(Ⅱ), Indium(Ⅲ) introduces, for the first time, acetamide to the field of the complex adsorption wave. In this field, we can determinate Lead(Ⅱ), Indium(Ⅲ) at same time. These methods have been applied to the determination of Lead(Ⅱ), Indium(Ⅲ) in pottery color ,mineral and hu更多还原