ELECTROCHEMICAL METHODS Fundamentals and Applications - Allen.J.Bard

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Acquisitions Editor David Harris Senior Production Editor Elizabeth Swain Senior Marketing Manager Charity Robey Illustration Editor Eugene Aiello This book was set in 10/12 Times Roman by University Graphics and printed and bound by Hamilton. The cover was printed by Phoenix. This book is printed on acid-free paper, oo Copyright 2001 © John Wiley & Sons, Inc. All rights reserved. No part of this publication may be reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, scanning or otherwise, except as permitted under Sections 107 or 108 of the 1976 United States Copyright Act, without either the prior written permission of the Publisher, or authorization through payment of the appropriate per-copy fee to the Copyright Clearance Center, 222 Rosewood Drive, Danvers, MA 01923, (978) 750-8400, fax (978) 750-4470. Requests to the Publisher for permission should be addressed to the Permissions Department, John Wiley & Sons, Inc., 605 Third Avenue, New York, NY 10158-0012, (212) 850-6011, fax (212) 850-6008, E-Mail: PERMREQ@WILEY.COM. To order books or for customer service, call 1 (800)-CALL-WILEY (225-5945). Library of Congress Cataloging in Publication Data: Bard, Allen J. Electrochemical methods : fundamentals and applications / Allen J. Bard, Larry R. Faulkner.— 2nd ed. p. cm. Includes index. ISBN 0-471-04372-9 (cloth : alk. paper) 1. Electrochemistry. I. Faulkner, Larry R., 1944- II. Title. QD553.B37 2000 541.3'7_dc21 Printed in the United States of America 10 987654321 00-038210
PREFACE In the twenty years since the appearance of our first edition, the fields of electrochemistry and electroanalytical chemistry have evolved substantially. An improved understanding of phenomena, the further development of experimental tools already known in 1980, and the introduction of new methods have all been important to that evolution. In the preface to the 1980 edition, we indicated that the focus of electrochemical research seemed likely to shift from the development of methods toward their application in studies of chemical behavior. By and large, history has justified that view. There have also been important changes in practice, and our 1980 survey of methodology has become dated. In this new edition, we have sought to update the book in a way that will extend its value as a general introduction to electrochemical methods. We have maintained the philosophy and approach of the original edition, which is to provide comprehensive coverage of fundamentals for electrochemical methods now in widespread use. This volume is intended as a textbook and includes numerous problems and chemical examples. Illustrations have been employed to clarify presentations, and the style is pedagogical throughout. The book can be used in formal courses at the senior undergraduate and beginning graduate levels, but we have also tried to write in a way that enables self-study by interested individuals. A knowledge of basic physical chemistry is assumed, but the discussions generally begin at an elementary level and develop upward. We have sought to make the volume self-contained by developing almost all ideas of any importance to our subject from very basic principles of chemistry and physics. Because we stress foundations and limits of application, the book continues to emphasize the mathematical theory underlying methodology; however the key ideas are discussed consistently apart from the mathematical basis. Specialized mathematical background is covered as needed. The problems following each chapter have been devised as teaching tools. They often extend concepts introduced in the text or show how experimental data are reduced to fundamental results. The cited literature is extensive, but mainly includes only seminal papers and reviews. It is impossible to cover the huge body of primary literature in this field, so we have made no attempt in that direction. Our approach is first to give an overview of electrode processes (Chapter 1), showing the way in which the fundamental components of the subject come together in an electrochemical experiment. Then there are individual discussions of thermodynamics and potential, electron-transfer kinetics, and mass transfer (Chapters 2-4). Concepts from these basic areas are integrated together in treatments of the various methods (Chapters 5-11). The effects of homogeneous kinetics are treated separately in a way that provides a comparative view of the responses of different methods (Chapter 12). Next are discussions of interfacial structure, adsorption, and modified electrodes (Chapters 13 and 14); then there is a taste of electrochemical instrumentation (Chapter 15), which is followed by an extensive introduction to experiments in which electrochemistry is coupled with other tools (Chapters 16-18). Appendix A teaches the mathematical background; Appendix В provides an introduction to digital simulation; and Appendix С contains tables of useful data.
Page 1: SECOND EDITION ELECTROCHEMICAL METH
Page 5 and 6: CONTENTS MAJOR SYMBOLS ix STANDARD
Page 7 and 8: Major Symbols Symbol Meaning Usual
Page 9 and 10: xii Major Symbols Symbol Meaning Us
Page 11 and 12: xiv Major Symbols Symbol Meaning Us
Page 13 and 14: xvi Major Symbols Symbol Meaning Us
Page 15 and 16: xviii Major Symbols Symbol Meaning
Page 17 and 18: xx Major Symbols Abbreviation Meani
Page 19 and 20: CHAPTER 1 INTRODUCTION AND OVERVIEW
Page 21 and 22: Pt H 2 1.1 Introduction 3 Zn Ag С
Page 23 and 24: 1.1 Introduction 5 Power supply -Ag
Page 25 and 26: 1.1 Introduction 7 idation of Br~ t
Page 27 and 28: 1.1 Introduction Hg/I-Г, ВГ(1 М
Page 29 and 30: 1.2 Nonfaradaic Processes and the N
Page 37 and 38: 1.3 Faradaic Processes and Factors
Page 47 and 48: 1.4 Introduction to Mass-Transfer-C
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1.4 Introduction to Mass-Transfer-C
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1.5 Semiempirical Treatment of Nems
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1.6 The Literature of Electrochemis
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1.6 The Literature of Electrochemis
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1.8 Problems 43 1.6 For the electro
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Thus the net cell reaction is 1 Zn
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2.1 Basic Electrochemical Thermodyn
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2.2 A More Detailed View of Interfa
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(a) Properties of the Electrochemic
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2.3 Liquid Junction Potentials л :
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2.3 Liquid Junction Potentials < 65
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2.3 Liquid Junction Potentials 67 T
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2.3 Liquid Junction Potentials 69 W
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2.3 Liquid Junction Potentials «I
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2.3 Liquid Junction Potentials : 73
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2.4 Selective Electrodes \ 75 Ag wi
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2.4 Selective Electrodes 77 The fir
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Other Ion-Selective Electrodes 2.4
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2.4 Selective Electrodes •« 81 (
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2.5 References 83 8. M. W. Chase, J
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2.3 Devise a cell in which the foll
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3 KINETICS OF ELECTRODE REACTIONS I
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3.1 Review of Homogeneous Kinetics
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3.2 Essentials of Electrode Reactio
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3.3 Butler-Volmer Model of Electrod
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3.4 Implications of the Butler-Volm
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Г " т - ') = e f(E-E«) ( 3 A 2 7
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3.5 Multistep Mechanisms 107 -200 -
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3.5 Multistep Mechanisms 109 one-st
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3.5 Multistep Mechanisms 111 which
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3.5 Multistep Mechanisms 113 dent o
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3.6 Microscopic Theories of Charge
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3.7 References 133 17. J. A. V. But
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3.8 Problems 135 Use a spreadsheet
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CHAPTER 4 MASS TRANSFER BY MIGRATIO
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4.2 Migration 139 component at any
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4.3 Mixed Migration and Diffusion N
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4.4 Diffusion i 147 -5/ -41 -31 -21
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4.4 Diffusion 149 net mass-transfer
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4.4 Diffusion 151 X IТ i i i \ \\
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4.5 References i 153 4.4.4 Solution
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4.6 Problems 155 4.4 The mobility,
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5.1 Overview of Step Experiments 15
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5.1 Overview of Step Experiments 15
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5.2 Potential Step Under Diffusion
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and inversion produces the current-
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5.3 Diffusion-Controlled Currents a
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Responses to a Large-Amplitude Pote
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5.4 Sampled-Current Voltammetry for
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5.6 Multicomponent Systems and Mult
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5.7 Chronoamperometric Reversal Tec
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5.7 Chronoamperometric Reversal Tec
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5.8 Chronocoulometry 211 nal-to-noi
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5.8 Chronocoulometry 213 100 200 30
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5.8 Chronocoulometry «i 215 The ap
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5.9 Special Applications of Ultrami
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5.9 Special Applications of Ultrami
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5.10 References « 221 would diffus
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5.11 Problems 223 0.2, 0.5, 1, 2, 3
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5.11 Problems < 225 5.19 G. Denault
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6.1 Introduction -I 227 0 t E t E°
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6.2 Nemstian (Reversible) Systems 2
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6.2 Nemstian (Reversible) Systems <
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6.2 Nernstian (Reversible) Systems
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where Introducing E(t) from (6.2.1)
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6.4 Quasireversible Systems *4 237
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6.5 Cyclic Voltammetry 239 Figure 6
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6.5 Cyclic Voltammetry 241 0.5 -0.3
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6.7 Convolutive or Semi-Integral Te
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6.8 Cyclic Voltammetry of the Liqui
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6.9 References 255 100 I -100 I I I
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6.10 Problems 257 20 r- 15 /, цА
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6.10 Problems *« 259 -0.8 -1.0 -1.
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CHAPTER 7 POLAROGRAPHY AND PULSE VO
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7.1 Behavior at Polarographic Elect
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7.2 Polarographic Waves 273 Kouteck
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7.3 PULSE VOLTAMMETRY 7.3 Pulse Vol
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7.3 Pulse Voltammetry 277 -0.4 -0.6
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7.3 Pulse Voltammetry < 279 • Dro
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7.3 Pulse Voltammetry 281 Potential
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7.3 Pulse Voltammetry 283 duration
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7.3 Pulse Voltammetry \. 285 cant c
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7.3 Pulse Voltammetry < 287 Second
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7.3 Pulse Voltammetry 289 The shape
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7.3 Pulse Voltammetry I 291 one ref
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7.3 Pulse Voltammetry 293 effects o
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7.3 Pulse Voltammetry 295 In genera
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7.3 Pulse Voltammetry < 297 1.0 i
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7.3 Pulse Voltammetry 299 (d) Appli
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7.4 References 301 Therefore, the b
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7.5 Problems < 303 49. L. Ramaley a
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8 CONTROLLED-CURRENT TECHNIQUES 8.1
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8.2 General Theory of Controlled-Cu
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8.2 General Theory of Controlled-Cu
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8.2.3 Programmed Current Chronopote
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8.3 Potential-Time Curves in Consta
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8.3 Potential-Time Curves in Consta
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8.4 Reversal Techniques 317 connect
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8.6 The Galvanostatic Double Pulse
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8.7 Charge Step (Coulostatic) Metho
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8.9 Problems 329 electrolysis time
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CHAPTER 9 METHODS INVOLVING FORCED
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9.2 Theoretical Treatment of Convec
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9.3 Rotating Disk Electrode 335 9.3
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9.3 Rotating Disk Electrode 337 Fig
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9.3 Rotating Disk Electrode i 339 T
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9.3 Rotating Disk Electrode 341 For
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9.3 Rotating Disk Electrode 343 1 0
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9.3 Rotating Disk Electrode 345 to
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7iim» o f j lim =l№l(i u /A)s l/
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9.4 Rotating Ring and Ring-Disk Ele
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9.4 Rotating Ring and Ring-Disk Ele
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9.5 Transients at the RDE and RRDE
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9.5.2 Transients at the RRDE 9.5 Tr
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9.6 Modulated RDE «1 357 600 400 -
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9.6 Modulated RDE < 359 Full-wave r
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9.7 Convection at Ultramicroelectro
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9.8 Electrohydrodynamics and Relate
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9.10 Problems 365 40. D. A. Saville
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9.10 Problems 367 +1.0 -0.2 Figure
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ЮЛ Introduction 369 Potentiometer
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10.1 Introduction 371 Figure 10.1.3
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10.1 Introduction 373 In this way w
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10.1 Introduction 375 *I_L -3 -2 -1
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10.2 Interpretation of the Faradaic
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10.2 Interpretation of the Faradaic
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10.3 Kinetic Parameters from Impeda
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10.4 Electrochemical Impedance Spec
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10.5 ас Voltammetry < 389 voltamm
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10.5 ас Voltammetry «I 391 exper
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10.5 ас Voltammetry 393 heterogen
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10.5 ас Voltammetry 395 This maxi
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10.5 ас Voltammetry < 397 The str
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10.5 ас Voltammetry -Щ 399 peak
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10.6 Higher Harmonics -m 401 f В R
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10.6 Higher Harmonics 403 Output H
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10.7 Chemical Analysis by ac Voltam
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10.8 Instrumentation for Electroche
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10.8 Instrumentation for Electroche
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10.9 Analysis of Data in the Laplac
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10.9 Analysis of Data in the Laplac
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10.11 Problems « 415 22. J. Vareec
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CHAPTER 11 BULK ELECTROLYSIS METHOD
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General Considerations in Bulk Elec
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General Considerations in Bulk Elec
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Controlled-Potential Methods < 423
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Controlled-Potential Methods 425 lo
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11.3.3 Electroseparations Controlle
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Controlled-Potential Methods 429 ur
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Controlled-Current Methods ^ 431 Ba
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Controlled-Current Methods i 433 Th
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Electrometric End-Point Detection 4
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Electrometric End-Point Detection i
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Electrometric End-Point Detection <
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Flow Electrolysis 441 11.6 FLOW ELE
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Flow Electrolysis ) = nFv dC o (x)
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Flow Electrolysis 445 This allows t
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Flow Electrolysis ^ 447 I Solution
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Flow Electrolysis 449 Spacer Auxili
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Flow Electrolysis 451 are much high
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Thin-Layer Electrochemistry 453 Mic
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Thin-Layer Electrochemistry 455 thr
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Thin-Layer Electrochemistry 457 -0.
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Stripping Analysis 459 Deposition (
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Stripping Analysis 461 -0.6 Figure
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Stripping Analysis 463 0 -0.2 1 1 1
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References 465 7. N. Tanaka, op. ci
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Problems 467 1.0 +0.8 +0.6 +0.4 +0.
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Problems 469 are equal and (b) thos
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CHAPTER 12 ELECTRODE REACTIONS WITH
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12.1 Classification of Reactions i
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12.1 Classification of Reactions 47
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12.2 Fundamentals of Theory for Vol
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(as above) дС т д2 С т С О2
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12.2 Fundamentals of Theory for Vol
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12.3 Theory for Transient Voltammet
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Catalytic Reaction—E r Cj 12.3 Th
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Icurr< 12.3 Theory for Transient Vo
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12.4 Rotating Disk and Ring-Disk Me
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12.7 Controlled-Potential Coulometr
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12.8 References « 529 12.8 REFEREN
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12.9 Problems =4 531 92. G. Denuaul
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12.9 Problems 533 12.11 Consider cu
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13.1 Thermodynamics of the Double L
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13.1 Thermodynamics of the Double L
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13.2 Experimental Evaluation of Sur
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13.2 Experimental Evaluation of Sur
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13.2.3 Relative Surface Excesses 13
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13.3 Models for Double-Layer Struct
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The total charge per unit volume in
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13.4 Studies at Solid Electrodes 55
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13.5 Extent and Rate of Specific Ad
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13.6 Effect of Adsorption of Electr
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13.7 Double-Layer Effects on Electr
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13.7.2 Double-Layer Effects in the
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13.8 Referencess 575 / / / 4 —% -
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13.9 Problems 577 64. D. M. Mohilne
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13.9 Problems 579 13.13 Aramata and
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14.2 Types, Preparation, and Proper
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14.3 Electrochemical Responses of A
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14.4 Overview of Processes at Modif
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where the permeation current, ip, i
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14.5 Blocking Layers 619 One can al
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14.5 Blocking Layers 621 current at
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14.5 Blocking Layers 623 The parame
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14.5 Blocking Layers 625 at the ele
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14.6 Other Methods of Characterizat
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14.7 References . 629 (b) H. S. Whi
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14.8 Problems 631 15 20 25 [ВГ],
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15.1 Operational Amplifiers 633 +15
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15.2 Current Feedback 635 (f) Other
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15.2 Current Feedback < 637 i Figur
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15.3 Voltage Feedback * 639 This ki
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15.4 Potentiostats 641 Counter Work
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15.4 Potentiostats -4 643 I Potenti
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15.6 Difficulties with Potential Co
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15.7 Measurement of Low Currents
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15.8 Computer-Controlled Instrument
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15.9 Troubleshooting Electrochemica
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15.11 Problems 657 25. P. He, J. P.
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CHAPTER 16 SCANNING PROBE TECHNIQUE
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16.2 Scanning Tunneling Microscopy
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16.3 Atomic Force Microscopy 667 no
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16.4 Scanning Electrochemical Micro
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16.6 Problems 679 tip and the subst
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17.1 Ultraviolet and Visible Spectr
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17.2 Vibrational Spectroscopy 701 R
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17.2 Vibrational Spectroscopy ; 703
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17.2 Vibrational Spectroscopy 705 h
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17.2 Vibrational Spectroscopy 707 0
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17.3 Electron and Ion Spectrometry
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17.4 Magnetic Resonance Methods 723
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17.5 Quartz Crystal Microbalance 72
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17.5 Quartz Crystal Microbalance ;
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17.6 X-Ray Methods 729 few millimet
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17.7 References 731 17.7 REFERENCES
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17.7 References =- 733 87. D. M. Ko
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17.8 Problems 735 17.2 Given D = 6.
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18.1 ElectrogeneratedChemiluminesce
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18.2 Photoelectrochemistry at Semic
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18.3 Electrochemical Detection of P
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18.3 Electrochemical Detection of P
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18.4 References ! 765 41. L. L. Shu
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18.5 Problems 767 18.4 The transien
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А Р Р #Й D IX А MATHEMATICAL M
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АЛ Solving Differential Equations
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А. 1 Solving Differential Equation
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А. 1 Solving Differential Equation
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А.2 Taylor Expansions 777 10 Figur
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А.З The Error Function and the Ga
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А.5 Complex Notation «i 781 A val
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А.8 Problems 783 In most applicati
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APPENDIX В DIGITAL SIMULATIONS OF
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ut the definition of a derivative a
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B.I Setting Up the Model 789 1. C*
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B.I Setting Up the Model 791 could
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В.2 An Example < 793 and imax « 6
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В.2 An Example « 795 mensionless
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В.З Incorporating Homogeneous Kin
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В.4 Boundary Conditions for Variou
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В.4 Boundary Conditions for Variou
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В.6 Miscellaneous Digital Simulati
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В.6 Miscellaneous Digital Simulati
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В.8 Problems 807 / B vs. x f° r t
Page 827 and 828:
TABLE C.I (continued) Reaction 2H +
Page 829 and 830:
Reference Tables 811 TABLE C.3 Esti
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Referem TABLE C.4 Selected Diffusio
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816 • Index Blocking polymers, 58
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818 Index Convective-diffusion equa
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820 Index Dropping mercury electrod
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822 ; Index Ellipsometry, described
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824 Index Instrumentation (continue
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826 Index Multicomponent systems: m
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828 Index Potential step methods (c
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830 • Index Sampled-current volta
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832 Index Thin-layer electrochemist
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