Principles of Thermal Analysis and Calorimetry

By: Peter Haines (Editor)

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Paperback | 3 April 2002

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280 Pages

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The use of thermal and calorimetric methods has shown rapid growth over the last two decades, in an increasingly wide range of applications. In addition, a number of powerful new techniques have been developed. This book supplies a concise and readable account of the principles, experimental apparatus and practical procedures used in thermal analysis and calorimetric methods of analysis. Brief accounts of the basic theory are reinforced with detailed applications of the methods and contemporary developments. Also included is information on standard test methods and manufacturers. Written by acknowledged experts, Principles of Thermal Analysis and Calorimetry is up-to-date, wide-ranging and practical. It will be an important source of information for many levels of readership in a variety of areas, from students and lecturers through to industrial and laboratory staff and consultants.

Industry Reviews

"... should certainly be recommended reading for all students who are concerned with analytical chemistry at degree level."

* Chromatographia, 2002, Vol 56, p 521 *

"... a first-class book."

* Chemistry & Industry, Issue 3, 3 February 2003 *

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Non-Fiction Science Chemistry Analytical Chemistry Science in General Physical Chemistry Thermochemistry & Chemical Thermodynamics

Introduction	p. 1
Materials, Heat and Changes	p. 1
Definitions of Thermal and Calorimetric Methods	p. 3
The Family of Thermal Methods	p. 4
Instrumentation for Thermal Analysis and Calorimetry	p. 4
The Reasons for Using Thermal and Calorimetric Methods	p. 6
The Need for Proper Practice	p. 6
Further Reading	p. 8
References	p. 8
Thermogravimetry and Derivative Thermogravimetry	p. 10
Introduction and Definitions	p. 10
Instrumentation	p. 12
Balance	p. 12
Furnace	p. 14
Atmosphere Control	p. 15
Crucibles	p. 15
Thermocouples	p. 16
Temperature Control	p. 16
Data Collection	p. 17
Isothermal Experiments	p. 18
Calibration for Mass and Temperature	p. 19
Effect of Experimental Variables	p. 20
Reporting Thermogravimetry Results	p. 24
Properties of the Sample	p. 24
Experimental Conditions	p. 24
Data Acquisition and Manipulation Methods	p. 24
Results	p. 25
Typical Thermogravimetric Experiment	p. 26
Preliminary Steps	p. 26
Crucible Treatment	p. 26
Zero Setting	p. 27
Adding the Sample	p. 28
Starting the Run	p. 28
Ending the Run	p. 28
Example Experiment	p. 29
Results	p. 29
Applications	p. 31
Oxysalt Decomposition	p. 31
Polymer Stability and Charcoal Production	p. 33
Metal Oxidation	p. 37
Compositional Analysis	p. 38
Glass-making Reactions	p. 40
Kinetics of Solid-state Reactions	p. 42
Ancillary Techniques	p. 50
Residue Analysis	p. 50
Other Temperature Regimes	p. 51
High Resolution Thermogravimetry	p. 51
Further Reading	p. 52
References	p. 53
Differential Thermal Analysis and Differential Scanning Calorimetry	p. 55
Introduction	p. 55
Definitions and Nomenclature	p. 57
Applications	p. 60
Theoretical Considerations	p. 65
Instrumentation	p. 69
Specification	p. 69
Temperature Sensors	p. 69
Crucibles	p. 70
Temperature and Atmosphere Control	p. 70
Cooling Systems and Accessories	p. 71
Calvet-type Equipment	p. 71
Experimental Considerations	p. 72
Variables	p. 72
Do's and Do not's	p. 73
Reference	p. 75
Calibration	p. 76
Preliminaries	p. 76
Temperature Calibration	p. 77
Energy Calibration	p. 79
Measurements	p. 82
Measurement of Heat Capacity	p. 82
Measurement of Energy	p. 85
Measurement of Purity	p. 87
Kinetics	p. 89
Final Thoughts on Measurement	p. 91
Further Reading	p. 91
References	p. 92
Thermomechanical, Dynamic Mechanical and Dielectric Methods	p. 94
Introduction and Principles	p. 94
Thermomechanical Analysis and Thermodilatometry	p. 94
Dynamic Mechanical Analysis	p. 96
Dielectric Techniques	p. 99
Instrumentation	p. 101
Thermomechanical Analysis	p. 101
Dynamic Mechanical Analysis	p. 103
Dielectric Techniques	p. 105
Typical Experiments	p. 106
Thermomechanical Analysis	p. 107
Dynamic Mechanical Analysis	p. 109
Dielectric Techniques	p. 113
Applications	p. 117
Thermomechanical Analysis	p. 117
Dynamic Mechanical Analysis	p. 120
Dielectric Thermal Analysis	p. 123
Modulated Temperature Thermomechanical and Dielectric Techniques	p. 126
Concluding Remarks	p. 126
Acknowledgements	p. 127
Further Reading	p. 127
References	p. 127
Calorimetry	p. 129
Introduction	p. 129
Definition of Calorimetry	p. 130
Thermochemistry and Thermodynamics	p. 131
The First law of Thermodynamics	p. 132
The Second Law of Thermodynamics	p. 133
The Third Law of Thermodynamics	p. 133
Calorimeters	p. 136
Classification of Calorimeters	p. 137
Calibration	p. 138
Instrumentation: Calorimeters for Special Purposes	p. 139
Solution Calorimeters	p. 139
Combustion Calorimeters	p. 141
Reaction Hazard Calorimeters	p. 144
Isothermal Calorimeters	p. 145
Applications of Isothermal Calorimetry	p. 146
Calorimetric Information	p. 148
The Calorimetric Signal	p. 148
Reaction Mechanism	p. 150
Kinetic Information	p. 152
Examples of Calorimetric Applications	p. 153
Chemical Reactions	p. 153
Physical Changes	p. 156
Summary	p. 160
Acknowledgements	p. 161
References	p. 161
Simultaneous Thermal Analysis Techniques	p. 166
Introduction: The Rationale behind the Simultaneous Approach	p. 166
Simultaneous Thermogravimetry--Differential Thermal Analysis (TG-DTA)	p. 167
Istrumentation	p. 167
Applications of TG-DTA	p. 170
Simultaneous Thermogravimetry--Differential Scanning Calorimetry (TG-DSC)	p. 172
Instrumentation	p. 172
Applications of TG-DSC	p. 173
Evolved Gas Analysis (EGA)	p. 174
Introduction	p. 174
Instrumentation for EGA	p. 175
Applications of EGA	p. 177
Less Common Techniques	p. 181
Optical Techniques	p. 181
Spectroscopic Techniques	p. 183
X-Ray Techniques	p. 183
DTA--Rheometry	p. 185
Micro-thermal Analysis ([mu]-TA)	p. 185
Summary	p. 187
References	p. 187
Appendices	p. 190
Symbols for Physical Quantities and Units	p. 190
Nomenclature for Thermal Analysis and Calorimetry	p. 191
Sources of Information	p. 191
Journals	p. 191
Major Textbooks on Thermal Analysis and Calorimetry	p. 192
Videos, CD-Roms etc.	p. 197
Conference Proceedings	p. 197
ICTAC and Its Affiliated Societies in Europe and the USA	p. 199
American and Other Standard Test Methods	p. 200
American Society for Testing and Materials (ASTM) Methods	p. 201
British Standards	p. 205
Manufacturers, Consultants and Other Suppliers	p. 207
Consultancies and Other Groups	p. 214
Subject Index	p. 216
Table of Contents provided by Syndetics. All Rights Reserved.

Principles of Thermal Analysis and Calorimetry

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