FUNDAMENTALS OF ELECTRO- ANALYTICAL CHEMISTRY
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1 FUNDAMENTALS OF ELECTRO- ANALYTICAL CHEMISTRY Paul Monk Manchester Metropolitan University, Manchester, UK JOHN WILEY & SONS LTD Chichester New York Weinheim Brisbane Toronto Singapore
2 Contents Series Preface Preface Acronyms, Abbreviations and Symbols About the Author xi xiii xv xxi 1 Explanatory Foreword Electroanalysis Nomenclature and Terminology (IUPAC and Non-IUPAC) This Book 9 Reference 10 2 Introductory Overview and Discussion of Experimental Methodology Overview of the Differences between Equilibrium and Dynamic Measurements The Magnitude of the Current: Rates of Electron Transfer, Mass Transport, and their Implications The Implications of Using Diffusive or Convective Control 23 Reference 24 3 Equilibrium Measurements: 'Frustrated' Equilibrium with No Net Electron Transfer Introduction: What is 'Equilibrium'? Concepts of 'Frustrated' Equilibrium 26
3 Fundamentals of Electroanalytical Chemistry 3.2 Revision: emf, Electrode Potentials and the SHE Terminology and Symbolisms Reference Electrodes The Nernst Equation and its Permutations Limitations of the Nernst Equation Differences between Concentration and Activity Brief Discourse on Ion-Ion Interactions Activities Activity Coefficients Revision of Debye-Hückel Theory Applications Based on Calculations with the Nernst Equation ph Determination and the ph Electrode Ion-Selective Electrodes Potentiometrie Determination of Solubility Constants Causes and Treatment of Errors Current Passage through a Cell Causing Internal Compositional Changes Current Passage through Reference Electrodes Determination of Concentration when the Mean lonic Activity Coefficient is Unknown Cell Design and the Effects of l IR Drop' Additional Sources of Potential Owing to lonic Transport and Junction Potentials 75 Potentiometry: True Equilibrium and Monitoring Systems with Electron Transfer Introduction to Potentiometry Redox Titrations: End Points and Shapes of Curves Determination of Equilibrium Constants and Solubility Constants Redox Indicators Treatment of Errors Routine Errors Errors Caused by Low Precision of Volume Determination: Use of Gran Plots Errors Caused by Poor ISE Selectivity 105 Coulometry Introduction to Coulometry and Faraday's Laws Faradaic and Non-Faradaic Charge 115
4 Contents vu The Effects of Absorption, Capacitance and the Electrode Double-Layer Stripping Microelectrodes Introduction to Electron Mediation Treatment of Errors Analysis by Dynamic Measurement, A: Systems under Diffusion Control Experimental Introduction to Dynamic Electrochemistry Chronoamperometry: Current Determined with Time The Nernst Layer ('Depletion' Layer) The Cottrell Equation Polarography at Hg Electrodes The Polarographic Experiment Polarography: the Dropping-Mercury Electrode Treatment of Polarographic Data: Obtaining Eiß and its Use Determination of Equilibrium Constants: Shifts in E\ß on Complexation Linear-Sweep and Cyclic Voltammetry at Solid Electrodes The Randles-Sevcik Equation The Effect of Slow Electron Transfer: Semiconducting Electrodes Quantification of Diffusion Phenomena Mechanistic Data from Voltammetry Improving Sensitivity: Pulse Methods Normal Pulse Voltammetry Differential Pulse Voltammetry Square-Wave Pulse Voltammetry Stripping Voltammetry The Glucose Sensor: a Worked Example of Voltammetric Analysis Causes and Treatment of Errors Polarographic 'Peaks' IR Drop: the Luggin Capillary Analysis by Dynamic Measurement, B: Systems under Convection Control Introduction to Convective Systems 196
5 Vlll Fundamentals of Electroanalytical Chemistry 7.2 The Rotated Disc Electrode Discussion of the Experiment The Levich Equation Flow Cells, Channel Electrodes and Wall-Jet Electrodes Flow Cells and Channel Electrodes The Wall-Jet Electrode The Rotated Ring-Disc Electrode Rate Constants of Electron Transfer The Tafel Approach to Electrode Kinetics The Butler-Volmer Approach Koutecky-Levich Plots and Measurement of the Rates of Electron Transfer Causes and Treatment of Errors 234 Reference Additional Methods Spectroelectrochemistry Introduction: What is Spectroelectrochemistry? Electrochemical UV-Visible Spectroscopy Electrochemical EPR Spectroscopy Electroanalytical Measurements Involving Impedance What is Impedance? Impedances of Real Cells: Quantification of Diffusion Phenomena and the Warburg Impedance Causes and Treatment of Errors Discontinuities in an OTE Conductor Total Internal Reflection in UV-Visible Spectroscopy Large Absorbances and the Optical Band Edge Stray EPR Absorptions 273 Reference 274 Electrode Preparation Preparation and Characterization of Solid Electrode Surfaces Cleaning Electrode Surfaces Manufacturing Electrodes Making Reference Electrodes Microelectrodes Screen-Printed Electrodes 287 Reference 288
6 Contents ix 10 Data Processing Simulation of Electrochemical Data Sample Programs Simulation Packages Web-Based Resources 302 References 304 Appendices Named Electroanalysis Equations Used in the Text Writing a Cell Schematic The Electrode Potential Series (against the SHE) 307 Responses to Self-Assessment Questions 311 Bibliography 329 Glossary of Terms 337 SI Units and Physical Constants 347 Periodic Table 351 Index 353
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