Experimental Electrochemistry A Laboratory

Showing how to apply the theoretical knowledge in practice, the one and only compilation of electrochemical experiments on the market now in a new edition.
Maintaining its didactic approach, this successful textbook provides clear and easy-to-follow instructions for carrying out the experiments, illustrating the most important principles and applications in modern electrochemistry, while pointing out the potential dangers and risks involved.
This second edition contains 84 experiments, many of which cover electrochemical energy conversion and storage as well as electrochemical equilibrium.

Rudolf Holze is Full Professor of Physical Chemistry and Electrochemistry at the Institute of Chemistry at Chemnitz University of Technology. He finished his studies of chemistry at Bonn University with a diploma thesis on new cathode materials for lithium batteries. His doctoral thesis focused on impedance measurements at porous electrodes for energy conversion systems. As a postdoctoral fellow with E.B. Yeager at Case Western Reserve University, Cleveland, Ohio, USA, he studied transition metal complexes as electrocatalysts for fuel cells. Research interests include spectroelectrochemistry, electrochemical materials science (intrinsically conducting polymers, corrosion, functionalized electrode surfaces) and corrosion. He has published several books and more than 280 research papers and reviews. In editorial boards of various journals and as editor he is actively involved in scientific communication, including the organization of conferences and workshops.

Preface to the Second Edition ix

Preface to the First Edition xi

Foreword to the Second Edition xv

Symbols and Acronyms xvii

1 Introduction: An Overview of Practical Electrochemistry 1

Practical Hints 2

Electrodes 3

Measuring Instruments 6

Electrochemical Cells 7

Data Recording 9

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 20

Experiment 2.4: Redox Titrations (Cerimetry) 25

Experiment 2.5: Differential Potentiometric Titration 27

Experiment 2.6: Potentiometric Measurement of the Kinetics of the Oxidation of Oxalic Acid 30

Experiment 2.7: Polarization and Decomposition Voltage 34

Experiment 2.8: A Simple Relative Hydrogen Electrode 39

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 51

Experiment 3.5: Chemical Constitution and Electrolytic Conductance 54

Experiment 3.6: Faraday’s Law 56

Experiment 3.7: Kinetics of Ester Saponification 58

Experiment 3.8: Movement of Ions and Hittorf Transport Number 62

Experiment 3.9: Polarographic Investigation of the Electroreduction of Formaldehyde 68

Experiment 3.10: Galvanostatic Measurement of Stationary Current–Potential Curves 72

Experiment 3.11: Cyclic Voltammetry 75

Experiment 3.12: Slow Scan Cyclic Voltammetry 82

Experiment 3.13: Kinetic Investigations with Cyclic Voltammetry 86

Experiment 3.14: Numerical Simulation of Cyclic Voltammograms 90

Experiment 3.15: Cyclic Voltammetry with Microelectrodes 92

Experiment 3.16: Cyclic Voltammetry of Organic Molecules 96

Experiment 3.17: Cyclic Voltammetry in Nonaqueous Solutions 102

Experiment 3.18: Cyclic Voltammetry with Sequential Electrode Processes 104

Experiment 3.19: Cyclic Voltammetry of Aromatic Hydrocarbons 107

Experiment 3.20: Cyclic Voltammetry of Aniline and Polyaniline 110

Experiment 3.21: Galvanostatic Step Measurements 115

Experiment 3.22: Cyclic Voltammetry of a Supercapacitor Electrode 118

Experiment 3.23: Chronoamperometry 121

Experiment 3.24: Chronocoulometry 122

Experiment 3.25: Rotating Disk Electrode 124

Experiment 3.26: Rotating Ring-Disk Electrode 130

Experiment 3.27: Measurement of Electrode Impedances 133

Experiment 3.28: Corrosion Cells 136

Experiment 3.29: Aeration Cell 138

Experiment 3.30: Concentration Cell 139

Experiment 3.31: Salt Water Drop Experiment According to Evans 141

Experiment 3.32: Passivation and Activation of an Iron Surface 142

Experiment 3.33: Cyclic Voltammetry with Corroding Electrodes 143

Experiment 3.34: Tafel Plot of a Corroding Electrode 145

Experiment 3.35: Impedance of a Corroding Electrode 148

Experiment 3.36: Linear Polarization Resistance of a Corroding Electrode 150

Experiment 3.37: Oscillating Reactions 152

4 Analytical Electrochemistry 155

Experiment 4.1: Ion-Sensitive Electrode 156

Experiment 4.2: Potentiometrically Indicated Titrations 158

Experiment 4.3: Bipotentiometrically Indicated Titration 163

Experiment 4.4: Conductometrically Indicated Titration 165

Experiment 4.5: Electrogravimetry 167

Experiment 4.6: Coulometric Titration 170

Experiment 4.7: Amperometry 172

Experiment 4.8: Polarography (Fundamentals) 178

Experiment 4.9: Polarography (Advanced Methods) 182

Experiment 4.10: Anodic Stripping Voltammetry 183

Experiment 4.11: Abrasive Stripping Voltammetry 186

Experiment 4.12: Polarographic Analysis of Anions 189

Experiment 4.13: Tensammetry 191

5 Nontraditional Electrochemistry 197

Experiment 5.1: UV-Vis Spectroscopy 197

Experiment 5.2: Surface-Enhanced Raman Spectroscopy 200

Experiment 5.3: Surface-Enhanced Raman Spectroscopy of a

Self-Assembled Monolayer 203

Experiment 5.4: Infrared Spectroelectrochemistry 205

Experiment 5.5: Electrochromism 207

Experiment 5.6: Raman Spectroscopic Monitoring of Charge/Discharge of an Intrinsically Conducting Polyaniline Supercapacitor Electrode Material 209

6 Electrochemical Energy Conversion and Storage 211

Experiment 6.1: Lead–Acid Accumulator 211

Experiment 6.2: Discharge Behavior of Nickel–Cadmium Accumulators 216

Experiment 6.3: Performance Data of a Fuel Cell 218

Experiment 6.4: Charging Supercapacitors 221

Experiment 6.5: Discharging Supercapacitors 224

Experiment 6.6: Zinc–Air Cell 227

Experiment 6.7: Lithium-Ion Battery 228

Experiment 6.8: Low-Temperature Discharge Behavior of Nickel–Cadmium Accumulators 230

Experiment 6.9: Discharge Behavior of Nickel–Cadmium Accumulators at Constant Load 233

Experiment 6.10: Impedance of a Button Cell 234

Experiment 6.11: Potentiostatic Polarization Curves 236

Experiment 6.12: Galvanostatic Polarization Curves 237

7 Electrochemical Production 241

Experiment 7.1: Cementation Reaction 241

Experiment 7.2: Galvanic Copper Deposition 242

Experiment 7.3: Electrochemical Oxidation of Aluminum 244

Experiment 7.4: Kolbe Electrolysis of Acetic Acid 245

Experiment 7.5: Electrolysis of Acetyl Acetone 247

Experiment 7.6: Anodic Oxidation of Malonic Acid Diethylester 250

Experiment 7.7: Indirect Anodic Dimerization of Acetoacetic Ester (3-Oxo-Butyric Acid Ethyl Ester) 251

Experiment 7.8: Electrochemical Bromination of Acetone 253

Experiment 7.9: Electrochemical Iodination of Ethanol 255

Experiment 7.10: Electrochemical Production of Potassium Peroxodisulfate 257

Experiment 7.11: Yield of Chlor-Alkali Electrolysis According to the Diaphragm Process 258

Appendix 261

Index 263

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Experimental Electrochemistry A Laboratory Textbook

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