Calorimetry: Fundamentals, Instrumentation and Applications

Overview

Clearly divided into three parts, this practical book begins by dealing with all fundamental aspects of calorimetry. The second part looks at the equipment used and new developments. The third and final section provides measurement guidelines in order to obtain the best results.
The result is optimized knowledge for users of this technique, supplemented with practical tips and tricks.
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Overview

Clearly divided into three parts, this practical book begins by dealing with all fundamental aspects of calorimetry. The second part looks at the equipment used and new developments. The third and final section provides measurement guidelines in order to obtain the best results.
The result is optimized knowledge for users of this technique, supplemented with practical tips and tricks.
Read More Show Less

Product Details

  • ISBN-13: 9783527327614
  • Publisher: Wiley
  • Publication date: 5/19/2014
  • Edition number: 2
  • Pages: 304
  • Product dimensions: 6.70 (w) x 9.60 (h) x 0.60 (d)

Meet the Author

Stefan M. Sarge studied chemistry at the Braunschweig University of Technology. Since 1990 he has worked for the Physikalisch-Technische Bundesanstalt (PTB) in Braunschweig, which is the National Metrology Institute of Germany providing scientific and technical services at the highest level of accuracy and reliability for the benefit of society as a whole, trade and industry, and science.
He is the Head of the Working Group on Caloric Quantities and the author of several publications in the fields of thermal analysis, calorimetry and legal metrology. In 1990 and 2004 he received the Netzsch-GEFTA award.

Günther W. H. Höhne studied chemistry, physics and mathematics at the Technical University of Berlin. In 1997 he was appointed Privatdozent (Adj. Professor) after his habilitation in experimental physics. From 1970 until his retirement in 1999 he was Head of the Section for Calorimetry of the University of Ulm, with duties including academic teaching in physics.
From 1999 to 2008 he was a visiting professor at the Eindhoven University of Technology. He has published numerous articles and two monographs on calorimetry and its applications. In 2002 he received the science award of the German Society of Thermal Analysis (GEFTA).

Wolfgang Hemminger studied physics at the University of Stuttgart and worked for a couple of years at the Braunschweig University in the field of materials science using calorimetry as one tool of research. In 1981 he joined the PTB and worked in the fields of thermal conductivity and various thermoanalytical methods.
In 1989 he was appointed Head of the PTB Division "Thermodynamics and Explosion Protection".
He was co-editor of the journal Thermochimica Acta and is the author of numerous journal articles and books. In 1981 he received the Netzsch-GEFTA award and in 2006 the GEFTA science award.

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Table of Contents

Preface XIII

List of Quantities and Units XV

Introduction Calorimetry: Definition, Application Fields and Units 1

Definition of Calorimetry 1

Application Fields for Calorimetry 1

First Example from Life Sciences 2

Second Example from Material Science 2

Third Example from Legal Metrology 2

Units 3

Further Reading 4

References 5

Part One Fundamentals of Calorimetry 7

1 Methods of Calorimetry 9

1.1 Compensation of the Thermal Effect 9

1.1.1 Compensation by a Phase Transition 9

1.1.2 Compensation by Electric Effects 12

1.2 Measurement of Temperature Differences 13

1.2.1 Measurement of Time-Dependent Temperature Differences 13

1.2.2 Measurement of Local Temperature Differences 15

1.2.2.1 First Example: Flow Calorimeter 15

1.2.2.2 Second Example: Heat Flow Rate Calorimeter 15

1.3 Summary of Measuring Principles 16

References 17

2 Measuring Instruments 19

2.1 Measurement of Amount of Substance 19

2.1.1 Weighing 20

2.1.2 Volume Measurement 20

2.1.3 Pressure Measurement 21

2.1.4 Flow Measurement 21

2.2 Measurement of Electric Quantities 21

2.3 Measurement of Temperatures 22

2.3.1 Thermometers 23

2.3.1.1 Liquid-in-Glass Thermometers 23

2.3.1.2 Gas Thermometers 24

2.3.1.3 Vapor Pressure Thermometers 24

2.3.1.4 Resistance Thermometers 25

2.3.1.5 Semiconductors 26

2.3.1.6 Pyrometers 26

2.3.2 Thermocouples 27

2.4 Chemical Composition 29

References 29

3 Fundamentals of Thermodynamics 31

3.1 States and Processes 31

3.1.1 Thermodynamic Variables (Functions of State) 31

3.1.2 Forms of Energy, Fundamental Form, and Thermodynamic Potential Function 34

3.1.2.1 Fundamental Form 35

3.1.2.2 Thermodynamic Potential Function 35

3.1.3 Equilibrium 38

3.1.4 Reversible and Irreversible Processes 41

3.1.5 The Laws of Thermodynamics 42

3.1.5.1 The Zeroth Law 42

3.1.5.2 The First Law 42

3.1.5.3 The Second Law 42

3.1.5.4 The Third Law 43

3.1.6 Measurement of Thermodynamic State Functions 43

3.2 Phases and Phase Transitions 47

3.2.1 Multiphase Systems 47

3.2.2 Phase Transitions 50

3.2.3 Gibbs Phase Rule 52

3.2.4 Measurement of Variables of State during Phase Transitions 56

References 59

4 Heat Transport Phenomena 61

4.1 Heat Conduction 61

4.2 Convection 64

4.3 Heat Radiation 65

4.4 Heat Transfer 67

4.5 Entropy Increase during Heat Exchange 67

4.6 Conclusions Concerning Calorimetry 68

References 71

5 Surroundings and Operating Conditions 73

5.1 The Isothermal Condition 74

5.2 The Isoperibol Condition 75

5.3 The Adiabatic Condition 75

5.4 The Scanning Condition 76

Reference 79

6 Measurements and Evaluation 81

6.1 Consequences of Temperature Relaxation within the Sample 81

6.1.1 First Example: Chemical Reaction 81

6.1.2 Second Example: Biological System 82

6.1.3 Third Example: First-Order Phase Transitions 83

6.2 Typical Results from Different Calorimeters 86

6.2.1 Adiabatic Calorimeters 86

6.2.2 Isoperibol Calorimeters 89

6.2.3 Differential Scanning Calorimeters 93

6.3 Reconstruction of the True Sample Heat Flow Rate from the Measured Function 101

6.3.1 Reconstruction of the Temperature Field for Negative Times 101

6.3.2 The Convolution Integral and Its Validity 102

6.3.3 Solution of the Convolution Integral 105

6.3.4 Obtaining the Apparatus Function 106

6.3.5 Application Limits and Estimation of Uncertainty 107

6.4 Special Evaluations 109

6.4.1 Determination of the Specific Heat Capacity 109

6.4.2 Determination of the Kinetic Parameters of a Chemical Reaction 109

6.4.3 Determination of Phase Transition Temperatures 111

6.4.4 Determination of Heats of Transition 112

6.4.5 Determination of the Purity of a Substance 114

6.5 Determination of the Measurement Uncertainty 115

References 121

Part Two Practice of Calorimetry 123

7 Calorimeters 125

7.1 Functional Components and Accessories 125

7.2 Heating Methods 126

7.3 Cooling Methods 126

7.4 Comments on Control Systems 128

7.5 Thermostats 131

7.6 On the Classification of Calorimeters 131

7.7 On the Characterization of Calorimeters 132

7.8 Isothermal Calorimeters 134

7.8.1 Phase Transition Calorimeters 134

7.8.1.1 First Example: Ice Calorimeter 135

7.8.1.2 Second Example: Calorimeter with Liquid–Gas Phase Transition 137

7.8.2 Isothermal Calorimeters with Electrical Compensation 141

7.8.2.1 First Example: Calorimeter according to Tian 142

7.8.2.2 Second Example: Isothermal Titration Calorimeter 143

7.8.2.3 Third Example: Isothermal Flow Calorimeter 144

7.9 Calorimeters with Heat Exchange between the Sample and Surroundings 144

7.9.1 Isoperibol Calorimeters with Uncontrolled Heat Exchange 145

7.9.1.1 First Example: Classic Liquid (or Mixing) Calorimeter 145

7.9.1.2 Second Example: Combustion Calorimeter 148

7.9.1.3 Third Example: Drop Calorimeter 151

7.9.2 Isoperibol Calorimeter with Controlled Heat Exchange 154

7.9.2.1 First Example: Activity Monitor 159

7.9.2.2 Second Example: Large-Volume Battery Calorimeter 160

7.9.2.3 Third Example: Calvet Calorimeter 161

7.9.2.4 Fourth Example: Whole-Body Calorimeter 169

7.9.3 Isoperibol Flow Calorimeter 170

7.9.3.1 First Example: The Picker Calorimeter 175

7.9.3.2 Second Example: Flow Calorimeter for High-Pressure and High-Temperature Measurements 176

7.9.3.3 Third Example: Gas Combustion Calorimeter 177

7.9.3.4 Fourth Example: Microchip Flow Calorimeter 177

7.9.4 Calorimeters with Linear Temperature Change of the Surroundings 178

7.9.4.1 First Example: Heat Flow Differential Scanning Calorimeter 179

7.9.4.2 Second Example: Power-Compensated Differential Scanning Calorimeter 183

7.9.4.3 Third Example: Privalov Calorimeter 185

7.9.5 Calorimeters with Nonlinear Temperature Change of the Surroundings 186

7.9.5.1 First Example: Temperature-Modulated DSC 187

7.9.5.2 Second Example: Stepscan Differential Scanning Calorimetry 189

7.9.5.3 Third Example: Advanced Multifrequency TMDSC 189

7.10 Adiabatic Calorimeters 190

7.10.1 Calorimeters with a Thermally Isolated Sample 190

7.10.1.1 First Example: Nernst Calorimeter 191

7.10.1.2 Second Example: Low-Temperature Calorimeter 192

7.10.1.3 Third Example: AC Calorimeter 194

7.10.1.4 Fourth Example: 3v Technique 195

7.10.1.5 Nernst’s Method with a Contactless Energy Supply 196

7.10.2 Calorimeters with Zero Temperature Difference against the Surroundings 197

7.10.2.1 First Example: Adiabatic Reaction Calorimeter 198

7.10.2.2 Second Example: Adiabatic Flow Calorimeter 199

7.10.2.3 Third Example: Adiabatic Whole-Body Calorimeter 199

7.10.2.4 Fourth Example: Adiabatic Scanning Calorimeter 200

7.10.3 Quasi-adiabatic Calorimetry by Sudden Heat Events 201

7.10.3.1 Example: Pulse Heating Calorimeter 201

7.11 Other Calorimeters 202

7.11.1 Reaction Calorimeters 202

7.11.1.1 First Example: Reaction Calorimeter 203

7.11.1.2 Second Example: Accelerating Rate Calorimeter (ARC) 204

7.11.2 Special Calorimeters 206

7.11.2.1 Photocalorimeters 206

7.11.2.2 Pressure Calorimeters 206

7.11.2.3 Pressure Perturbation Calorimeter 206

7.11.2.4 Cement Calorimeter 207

References 207

8 Recent Developments 213

8.1 Microchip Calorimetry 214

8.1.1 First Example: Thin-Film Differential Scanning Calorimeter 216

8.1.2 Second Example: Low-Temperature AC Nanocalorimeter 217

8.2 Ultrafast Calorimetry 217

8.2.1 First Example: Ultrafast Nanocalorimeter 218

8.2.2 Second Example: Flash Differential Scanning Calorimeter 220

8.3 Extreme Ranges of State 220

8.3.1 High Pressure 221

8.3.1.1 Example: Power-Compensated High-Pressure DSC 222

8.3.2 High Temperature 222

8.3.2.1 Example: Levitation Calorimetry on Nickel, Iron, Vanadium, and Niobium 223

8.3.3 Strong Magnetic Fields 224

8.3.3.1 Example: Influence of Magnetic Fields on Point Defects 224

8.3.4 Plasma Surroundings 224

8.3.4.1 Example: Calibration Using a Laser Beam 224

8.4 Calorimetry as an Analytical and Diagnostic Tool 225

8.4.1 First Example: “Artificial Nose” 225

8.4.2 Second Example: Infection Diagnostics 225

References 226

9 Calorimetric Measurements: Guidelines and Applications 229

9.1 General Considerations 229

9.1.1 Sensitivity (DX/Q or DX/DF) 230

9.1.2 Noise (dQ or dF) 230

9.1.3 Linearity (Xout¼K Xin) and Linearity Error (dK/K) 232

9.1.4 Apparatus Function (fapp(t)) 232

9.1.5 Accuracy and Total Error ({Qmeasured – Qtrue}/Qtrue) 233

9.1.6 Repeatability and Random Uncertainty (DQ/Q) 235

Conclusion 235

9.2 Guidelines to Calorimetric Experiments 235

9.2.1 Definition of the Problem to be Investigated 236

9.2.2 Selection of the Proper Calorimeter 237

9.2.2.1 Calorimeter Requirements 237

9.2.2.2 Selection of the Calorimeter 238

9.2.3 Testing of the Calorimeter 239

9.2.3.1 Calibration 239

9.2.3.2 Other Testing 242

9.2.4 Performing the Experiment 243

9.2.4.1 Preparation of the Sample 243

9.2.4.2 Calorimetric Measurement 244

9.2.4.3 Evaluation of the Measurement 245

9.2.5 Interpretation of the Results 245

9.2.6 Uncertainty Estimation 246

9.3 Calorimetric Applications 246

9.3.1 Example from Material Science 247

9.3.1.1 Definition of the Problem to be Investigated 247

9.3.1.2 Selection of the Calorimeter 247

9.3.1.3 Calorimetric Experiments 248

9.3.1.4 Evaluation of the Measurements 248

9.3.1.5 Interpretation of the Results 251

9.3.1.6 Uncertainty Estimation 252

9.3.2 Examples from Biology 256

9.3.2.1 Definition of the Problem to be Investigated 256

9.3.2.2 Selection of the Proper Calorimeter 256

9.3.2.3 Calorimetric Experiments 257

9.3.2.4 Evaluation of the Results 258

9.3.2.5 Calorimetry on Hornets 258

9.3.2.6 Uncertainty Estimation 259

9.3.3 Example from Medicine 259

9.3.3.1 Definition of the Problem to be Investigated 259

9.3.3.2 Selection of the Proper Calorimeter 259

9.3.3.3 Calorimetric Experiment 260

9.3.3.4 Evaluation of the Measurements 260

9.3.3.5 Interpretation of the Results 260

9.3.3.6 Uncertainty Estimation 261

9.3.4 Example from Chemistry 261

9.3.4.1 Definition of the Problem to be Investigated 262

9.3.4.2 Selection of the Proper Calorimeter 262

9.3.4.3 Calorimetric Experiment 263

9.3.4.4 Evaluation of the Measurements 263

9.3.4.5 Interpretation of the Results 264

9.3.4.6 Uncertainty Estimation 265

9.3.5 Example from Combustion Calorimetry 265

9.3.5.1 Definition of the Problem to be Investigated 265

9.3.5.2 Selection of the Proper Calorimeter 265

9.3.5.3 Calorimetric Experiment 267

9.3.5.4 Evaluation of the Measurements 267

9.3.5.5 Interpretation of the Results 268

9.3.5.6 Uncertainty Estimation 268

References 269

Index 271

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