Electrochemistry in Nonaqueous Solutions

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1 К. Izutsu Electrochemistry in Nonaqueous Solutions WILEY-VCH

2 Contents Preface V Part I Fundamentals of Chemistry in Non-Aqueous Solutions: Electrochemical Aspects 1 Properties of Solvents and Solvent Classification Properties of Solvents Physical Properties of Solvents Chemical Properties of Solvents Structural Aspects of Solvents Toxicity and Hazardous Properties of Solvents Classification of Solvents Effects of Solvent Properties on Chemical Reactions (an Outline) References 23 2 Solvation and Complex Formation of Ions and Behavior of Electrolytes Influence of Ion Solvation on Electrolyte Dissolution Some Fundamental Aspects of Ion-Solvation Ion-Solvent Interactions Affecting Ion Solvation Structure of Solvated Ions Ultrafast Ion-Solvation Dynamics Comparison of Ionic Solvation Energies in Different Solvents and Solvent Effects on Ionic Reactions and Equilibria Gibbs Energies of Transfer and Transfer Activity Coefficients of Ions Prediction of Solvent Effects by the Use of Transfer Activity Coefficients Solvent Effects on the Complexation of Metal Ions Selective Solvation of Ions in Mixed Solvents Ion Association and Solvent Permittivities References 56

3 X Contents 3 Acid-Base Reactions in Non-Aqueous Solvents Solvent Effects on Acid-Base Reactions Acid-Base Reactions in Amphiprotic Solvents of High Permittivit Acid-Base Reactions in Aprotic Solvents of High Permittivity Acid-Base Reactions in Amphiprotic Solvents of Low Permittivity Acid-Base Reactions in Aprotic Solvents of Low Permittivity ph-scales in Non-Aqueous Solutions Definition of ph in Non-Aqueous Solutions ph Windows in Non-Aqueous Solvents and ph Scales Common to Multi Solvents References 82 4 Redox Reactions in Non-Aqueous Solvents Solvent Effects on Various Types of Redox Reactions Fundamentals of Redox Reactions Solvent Effects on Redox Potentials and Redox Reaction Mechanisms Dynamical Solvent Effects on the Kinetics of Redox Reactions Redox Properties of Solvents and Potential Windows Redox Titrations in Non-Aqueous Solutions Titrations with Oxidizing Agents Titrations with Reducing Agents References 106 Part II Electrochemical Techniques and Their Applications in Non-Aqueous Solutions 5 Overview of Electrochemical Techniques Classification of Electrochemical Techniques Fundamentals of Electrode Reactions and Current-Potential Relations Current-Potential Relation for Electron Transfer at the Electrode Current-Potential Relations and Mass Transport DC Polarography - Methods that Electrolyze Electroactive Species Only Partially (1) New Types of Polarography - Methods that Electrolyze Electroactive Species Only Partially (2) AC Polarography SW Polarography Pulse Polarography Voltammetry and Related New Techniques - Methods that Electrolyze Electroactive Species Only Partially (3) 129

4 Contents XI Linear Sweep Voltammetry Cyclic Voltammetry Voltammetry at Rotating Disk and Rotating Ring-Disk Electrodes Ultramicroelectrodes Modified Electrodes Combination of Voltammetry and Non-Electrochemical Methods Voltammetry at the Interface Between Two Immiscible Electrolyte Solutions Electrogravimetry and Coulometry - Methods that Completely Electrolyze Electroactive Species Controlled-Potential Electrolysis and Controlled-Current Electrolysis Electrogravimetry Coulometry and Coulometric Titrations Potentiometry - A Method that Does Not Electrolyze Electroactive Species Potentiometrie Indicator Electrodes and Reference Electrodes Potentiometrie Titrations Conductimetry - A Method that is Not Based on Electrode Reactions Electrochemical Instrumentation - Roles of Operational Amplifiers and Microcomputers Application of Operational Amplifiers in Electrochemical Instrumentation Applications of Personal Computers in Electrochemical Instrumentation References Potentiometry in Non-Aqueous Solutions Basic Techniques of Potentiometry in Non-Aqueous Solutions Potentiometrie Indicator Electrodes for Non-Aqueous Solutions Reference Electrodes for Non-Aqueous Solutions Method of Reporting Electrode Potentials in Non-Aqueous Solutions (IUPAC Recommendation) Liquid Junction Potential Between Electrolyte Solutions in the Same Solvent ph Measurements in Non-Aqueous Solutions ph Measurements in Aqueous Solutions Methods of ph Measurements in Non-Aqueous and Mixed Solvents Determination of Autoprotolysis Constants Applications of Potentiometry in Non-Aqueous Solutions Acid-Base Reactions in Non-Aqueous Solvents Precipitation Reactions in Non-Aqueous Solutions Complex Formation Reactions in Non-Aqueous Solutions 186

5 XII Contents Redox Reactions in Non-Aqueous Solutions Potentiometrie Characterization of Solvents Potentiometrie Study of Ion Solvation - Applications that Compare Electrode Potentials in Different Solvents Liquid Junction Potentials between Different Solvents References Conductimetry in Non-Aqueous Solutions Dissociation of Electrolytes and Electrolytic Conductivity Molar Conductivity of Dilute Solutions of Symmetrical Strong Electrolytes Molar Conductivity and Association Constants of Symmetrical Weak Electrolytes Molar Conductivity and the Formation of Triple Ions Conductivity of Solutions of Symmetrical Strong Electrolytes at Moderate to High Concentrations Molar Conductivity and Ion Association of Asymmetric Electrolytes Ionic Conductivities and Solvents Stokes' Law and Walden's Rule - Role of Ultrafast Solvent Dynamics Method for the Determination of Limiting Molar Conductivities of Ions Applications of Conductimetry in Non-Aqueous Solutions Study of the Behavior of Electrolytes (Ionophores) Conductimetric Studies of Acid-Base Equilibria References Polarography and Voltammetry in Non-Aqueous Solutions Basic Experimental Techniques in Non-Aqueous Solutions Experimental Apparatus for Non-Aqueous Systems Solvents and Supporting Electrolytes Polarography and Voltammetry of Inorganic Species Polarographic Reductions of Metal Ions Polarography and Voltammetry of Metal Complexes Polarography and Voltammetry of Anions Electrode Reactions of Dissolved Oxygen, Dissolved Hydrogen, Carbon Dioxide, and Solvated Electrons Polarography and Voltammetry of Organic Compounds Reduction of Organic Compounds Oxidation of Organic Compounds Cyclic Voltammetry for Electrochemical Studies in Non-Aqueous Solutions Digital Simulation in Cyclic Voltammetry Ultramicroelectrodes in Cyclic Voltammetry 262

6 Contents XIII Low Temperature Electrochemistry and Cyclic Voltammetry References Other Electrochemical Techniques in Non-Aqueous Solutions Use of Electrolytic and Coulometric Techniques in Non-Aqueous Solutions Combination of Electrochemical and Nonelectrochemical Techniques Spectroelectrochemistry Electrochemical-ESR Method Electrochemical Mass Spectroscopy Use of Electrochemical Quartz Crystal Microbalance (EQCM) Use of Scanning Electrochemical Microscopy (SECM) References Purification of Solvents and Tests for Impurities Effects of Solvent Impurities on Electrochemical Measurements Procedures for the Purification of Solvents Tests for Purity of Solvents Purification Methods for Solvents in Common Use References Selection and Preparation of Supporting Electrolytes Selection of Supporting Electrolytes for Electrochemical Measurements Solubility and Conductivity of Supporting Electrolytes Potential Windows and Supporting Electrolytes Influences of Supporting Electrolytes on Electrode Reactions in Non-Aqueous Solutions Methods for Preparing and Purifying Supporting Electrolytes References Use of Non-Aqueous Solutions in Modern Electrochemical Technologies New Batteries Using Non-Aqueous Solutions (Lithium Batteries) New Capacitors Using Non-Aqueous Solutions Supercapacitors Aluminum Electrolytic Capacitors Conducting Polymers and Electrochemistry in Non-Aqueous Solutions Electrochemical Reduction of C0 2 in Non-Aqueous Solvents Use of Acetonitrile in Electrowinning and Electrorefining of Copper Electrodeposition of Metals from Non-Aqueous Solutions 324

7 XIV Contents 12.7 Electrochemical Use of Supercritical Fluids and Ionic Liquids as Benign Solvents Supercritical Fluid Solvents Room-temperature Ionic Liquids References 329 Index 331

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