Experimental Electrochemistry: A Laboratory Textbook / Edition 1

Experimental Electrochemistry: A Laboratory Textbook / Edition 1

by Rudolf Holze

ISBN-10: 3527310983

ISBN-13: 9783527310982

Pub. Date: 07/14/2009

Publisher: Wiley

Electrochemistry is part of our daily life: It powers our cell phones, notebook computers and many other electronic devices. It provides the power to start our cars in the morning, it is undesirably present in corrosion, but also needed in metal winning and refining. The list is seemingly endless. Similarly, electrochemical processes, methods, models, and


Electrochemistry is part of our daily life: It powers our cell phones, notebook computers and many other electronic devices. It provides the power to start our cars in the morning, it is undesirably present in corrosion, but also needed in metal winning and refining. The list is seemingly endless. Similarly, electrochemical processes, methods, models, and concepts are present in numerous fields of science and technology. Electrochemistry as a subject is an extremely interdisciplinary science, and, being an experimental science, it demands the direct hands-on testing of a model or a theory.
This textbook fills the gap for a wide-ranging collection of reproducible experiments suitable for course work at all levels, from high school to university. The careful selection presented here is based on experiments developed and installed as part of laboratory courses for students of chemistry and materials science, as well as other sciences. In addition it contains experiments developed for teachers at the various levels where pupils will encounter electrochemistry for the first time.
Following a brief overview, the book goes on to deal with electrochemistry at equilibrium and with flowing current, while further chapters cover analytical electrochemistry, non-traditional methods, electrochemical energy storage and conversion, as well as technical electrochemistry. Throughout, the author presents the obvious relationship between theory and experiment, while highlighting the practical importance of the experiments in our daily lives. The scope of electrochemistry is not only illustrated by the diversity of methods and concepts, it is also demonstrated by the range of instruments and tools employed. In all the descriptions the emphasis is placed on clear, well-defined, and lucid descriptions, including everything needed for a successful repetition of the experiment, while avoiding unnecessary details. If necessary, further references to textbooks, review articles, and research papers are given.
Complementing textbooks on electrochemistry, this is a must for lecturers as well as for students in chemistry and related fields.

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Table of Contents

Preface IX

Foreword XIII

Symbols and Acronyms XV

1 Introduction - An Overview of Practical Electrochemistry 1

Practical Hints 3

Electrodes 3

Measuring Instruments 7

Electrochemical Cells 8

Data Recording 10

2 Electrochemistry in Equilibrium 11

Experiment 2.1 The Electrochemical Series 11

Experiment 2.2 Standard Electrode Potentials and the Mean Activity Coefficient 15

Experiment 2.3 pH-Measurements and Potentiometrically Indicated Titrations 21

Experiment 2.4 Redox Titrations (Cerimetry) 26

Experiment 2.5 Differential Potentiometric Titration 28

Experiment 2.6 Potentiometric Measurement of the Kinetics of the Oxidation of Oxalic Acid 32

Experiment 2.7 Polarization and Decomposition Voltage 36

3 Electrochemistry with Flowing Current 43

Experiment 3.1 Ion Movement in an Electric Field 44

Experiment 3.2 Paper Electrophoresis 46

Experiment 3.3 Charge Transport in Electrolyte Solution 47

Experiment 3.4 Conductance Titration 52

Experiment 3.5 Chemical Constitution and Electrolytic Conductance 54

Experiment 3.6 Faraday's Law 56

Experiment 3.7 Kinetics of Ester Saponification 59

Experiment 3.8 Movement of Ions and Hittorf Transport Number 63

Experiment 3.9 Polarographic Investigation of the Electroreduction of Formaldehyde 69

Experiment 3.10 Galvanostatic Measurement of Stationary Current-Potential Curves 74

Experiment 3.11 Cyclic Voltammetry 77

Experiment 3.12 Slow Scan Cyclic Voltammetry 85

Experiment 3.13 Kinetic Investigations with Cyclic Voltammetry 88

Experiment 3.14 Numerical Simulation of Cyclic Voltammograms 93

Experiment 3.15 Cyclic Voltammetry with Microelectrodes 95

Experiment 3.16 Cyclic Voltammetry of OrganicMolecules 99

Experiment 3.17 Cyclic Voltammetry in Nonaqueous Solutions 105

Experiment 3.18 Cyclic Voltammetry with Sequential Electrode Pocesses 107

Experiment 3.19 Cyclic Voltammetry of Aromatic Hydrocarbons 110

Experiment 3.20 Cyclic Voltammetry of Aniline and Polyaniline 113

Experiment 3.21 Galvanostatic Step Measurements 118

Experiment 3.22 Chronoamperometry 122

Experiment 3.23 Chronocoulometry 124

Experiment 3.24 Rotating Disc Electrode 126

Experiment 3.25 Rotating Ring-Disc Electrode 131

Experiment 3.26 Measurement of Electrode Impedances 134

Experiment 3.27 Corrosion Cells 137

Experiment 3.28 Aeration Cell 139

Experiment 3.29 Concentration Cell 141

Experiment 3.30 Salt Water Drop Experiment According to Evans 142

Experiment 3.31 Passivation and Activation of an Iron Surface 143

Experiment 3.32 Cyclic Voltammetry with Corroding Electrodes 145

Experiment 3.33 Oscillating Reactions 147

4 Analytical Electrochemistry 151

Experiment 4.1 Ion-sensitive Electrode 152

Experiment 4.2 Potentiometrically Indicated Titrations 154

Experiment 4.3 Bipotentiometrically Indicated Titration 159

Experiment 4.4 Conductometrically Indicated Titration 161

Experiment 4.5 Electrogravimetry 163

Experiment 4.6 Coulometric Titration 166

Experiment 4.7 Amperometry 168

Experiment 4.8 Polarography (Fundamentals) 174

Experiment 4.9 Polarography (Advanced Methods) 178

Experiment 4.10 Anodic Stripping Voltammetry 180

Experiment 4.11 Abrasive Stripping Voltammetry 183

Experiment 4.12 Polarographic Analysis of Anions 185

Experiment 4.13 Tensammetry 188

5 Non-Traditional Electrochemistry 195

Experiment 5.1 UV-Vis Spectroscopy 195

Experiment 5.2 Surface Enhanced Raman Spectroscopy 199

Experiment 5.3 Infrared Spectroelectrochemistry 201

Experiment 5.4 Electrochromism 203

6 Electrochemical Energy Conversion and Storage 205

Experiment 6.1 Lead Acid Accumulator 205

Experiment 6.2 Discharge Behavior of Nickel-Cadmium Accumulators 210

Experiment 6.3 Performance Data of a Fuel Cell 213

7 Electrochemical Production 217

Experiment 7.1 Cementation Reaction 217

Experiment 7.2 Galvanic Copper Deposition 218

Experiment 7.3 Electrochemical Oxidation of Aluminum 220

Experiment 7.4 Kolbe Electrolysis of Acetic Acid 222

Experiment 7.5 Electrolysis of Acetyl Acetone 223

Experiment 7.6 Anodic Oxidation of Malonic Acid Diethylester 226

Experiment 7.7 Indirect Anodic Dimerization of Acetoacetic Ester (3-oxo-butyric acid ethyl ester) 227

Experiment 7.8 Electrochemical Bromination of Acetone 229

Experiment 7.9 Electrochemical Iodination of Ethano 231

Experiment 7.10 Electrochemical Production of Potassium Peroxodisulfate 233

Experiment 7.11 Yield of Chlor-alkali Electrolysis According to the Diaphragm Process 234

Appendix 237

Index 239

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