ELECTROCHEMICAL METHODS Fundamentals and Applications - Allen.J.Bard

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Major Symbols xxi Abbreviation QRE RDE RDS RPP RPV RRDE SAM SCE SECM SERS SHE SHG SMDE SNIFTIRS SPE SPR SSCE STM swv TBABF4 TBAI TBAP TEAP THF UHV UME UPD XPS VB Meaning quasi-reference electrode rotating disk electrode rate-determining step reverse pulse polarography reverse pulse voltammetry rotating ring-disk electrode self-assembled monolayer saturated calomel electrode scanning electrochemical microscopy surface enhanced Raman spectroscopy standard hydrogen electrode = NHE second harmonic generation static mercury drop electrode subtractively normalized interfacial Fourier transform infrared spectroscopy solid polymer electrolyte surface plasmon resonance sodium saturated calomel electrode, Hg/Hg 2 Cl2/NaCl (sat'd) scanning tunneling microscopy square wave voltammetry tetra-/2-butylammonium fluoborate tetra-ft-butylammonium iodide tetra-w-butylammoniumperchlorate tetraethylammonium perchlorate tetrahydrofuran ultrahigh vacuum ultramicroelectrode underpotential deposition X-ray photoelectron spectrometry valence band Section Reference 2.1.7 9.3 3.5 7.3.4 7.3.4 9.4.2 14.2.2 1.1.1 16.4 17.2.2 1.1.1 17.1.5 7.1.1 17.2.1 14.2.6 17.1.3 16.2 7.3.5 17.3 5.3 11.2.1 17.3.2 18.2.2
CHAPTER 1 INTRODUCTION AND OVERVIEW OF ELECTRODE PROCESSES 1.1 INTRODUCTION Electrochemistry is the branch of chemistry concerned with the interrelation of electrical and chemical effects. A large part of this field deals with the study of chemical changes caused by the passage of an electric current and the production of electrical energy by chemical reactions. In fact, the field of electrochemistry encompasses a huge array of different phenomena (e.g., electrophoresis and corrosion), devices (electrochromic displays, electro analytical sensors, batteries, and fuel cells), and technologies (the electroplating of metals and the large-scale production of aluminum and chlorine). While the basic principles of electrochemistry discussed in this text apply to all of these, the main emphasis here is on the application of electrochemical methods to the study of chemical systems. Scientists make electrochemical measurements on chemical systems for a variety of reasons. They may be interested in obtaining thermodynamic data about a reaction. They may want to generate an unstable intermediate such as a radical ion and study its rate of decay or its spectroscopic properties. They may seek to analyze a solution for trace amounts of metal ions or organic species. In these examples, electrochemical methods are employed as tools in the study of chemical systems in just the way that spectroscopic methods are frequently applied. There are also investigations in which the electrochemical properties of the systems themselves are of primary interest, for example, in the design of a new power source or for the electrosynthesis of some product. Many electrochemical methods have been devised. Their application requires an understanding of the fundamental principles of electrode reactions and the electrical properties of electrode-solution interfaces. In this chapter, the terms and concepts employed in describing electrode reactions are introduced. In addition, before embarking on a detailed consideration of methods for studying electrode processes and the rigorous solutions of the mathematical equations that govern them, we will consider approximate treatments of several different types of electrode reactions to illustrate their main features. The concepts and treatments described here will be considered in a more complete and rigorous way in later chapters.
Page 1 and 2: SECOND EDITION ELECTROCHEMICAL METH
Page 3 and 4: PREFACE In the twenty years since t
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: xx Major Symbols Abbreviation Meani
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
Page 55 and 56: 1.5 Semiempirical Treatment of Nems
Page 57 and 58: 1.6 The Literature of Electrochemis
Page 59 and 60: 1.6 The Literature of Electrochemis
Page 61 and 62: 1.8 Problems 43 1.6 For the electro
Page 63 and 64: Thus the net cell reaction is 1 Zn
Page 65 and 66: 2.1 Basic Electrochemical Thermodyn
Page 67 and 68: 2.1 Basic Electrochemical Thermodyn
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2.1 Basic Electrochemical Thermodyn
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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
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TABLE C.I (continued) Reaction 2H +
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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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ELECTROCHEMICAL METHODS Fundamentals and Applications - Allen.J.Bard

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