| |
| |
| |
Introduction | |
| |
| |
| |
Materials, Heat and Changes | |
| |
| |
Definitions of Thermal and Calorimetric Methods | |
| |
| |
The Family of Thermal Methods | |
| |
| |
Instrumentation for Thermal Analysis and Calorimetry | |
| |
| |
The Reasons for Using Thermal and Calorimetric Methods | |
| |
| |
The Need for Proper Practice | |
| |
| |
Further Reading | |
| |
| |
References | |
| |
| |
| |
Thermogravimetry and Derivative Thermogravimetry | |
| |
| |
| |
Introduction and Definitions | |
| |
| |
Instrumentation | |
| |
| |
Balance | |
| |
| |
Furnace | |
| |
| |
Atmosphere Control | |
| |
| |
Crucibles | |
| |
| |
Thermocouples | |
| |
| |
Temperature Control | |
| |
| |
Data Collection | |
| |
| |
Isothermal Experiments | |
| |
| |
Calibration for Mass and Temperature | |
| |
| |
Effect of Experimental Variables | |
| |
| |
Reporting Thermogravimetry Results | |
| |
| |
| |
Properties of the Sample | |
| |
| |
| |
Experimental Conditions | |
| |
| |
| |
Data Acquisition and Manipulation Methods | |
| |
| |
| |
Results | |
| |
| |
| |
Typical Thermogravimetric Experiment | |
| |
| |
Preliminary Steps | |
| |
| |
Crucible Treatment | |
| |
| |
Zero Setting | |
| |
| |
Adding the Sample | |
| |
| |
Starting the Run | |
| |
| |
Ending the Run | |
| |
| |
Example Experiment | |
| |
| |
Results | |
| |
| |
Applications | |
| |
| |
Oxysalt Decomposition | |
| |
| |
Polymer Stability and Charcoal Production | |
| |
| |
Metal Oxidation | |
| |
| |
Compositional Analysis | |
| |
| |
Glass-making Reactions | |
| |
| |
Kinetics of Solid-state Reactions | |
| |
| |
Ancillary Techniques | |
| |
| |
Residue Analysis | |
| |
| |
Other Temperature Regimes | |
| |
| |
High Resolution Thermogravimetry | |
| |
| |
Further Reading | |
| |
| |
References | |
| |
| |
| |
Differential Thermal Analysis and Differential Scanning Calorimetry | |
| |
| |
| |
Introduction | |
| |
| |
Definitions and Nomenclature | |
| |
| |
Applications | |
| |
| |
Theoretical Considerations | |
| |
| |
Instrumentation | |
| |
| |
Specification | |
| |
| |
Temperature Sensors | |
| |
| |
Crucibles | |
| |
| |
Temperature and Atmosphere Control | |
| |
| |
Cooling Systems and Accessories | |
| |
| |
Calvet-type Equipment | |
| |
| |
Experimental Considerations | |
| |
| |
Variables | |
| |
| |
Do's and Do not's | |
| |
| |
Reference | |
| |
| |
Calibration | |
| |
| |
Preliminaries | |
| |
| |
Temperature Calibration | |
| |
| |
Energy Calibration | |
| |
| |
Measurements | |
| |
| |
Measurement of Heat Capacity | |
| |
| |
Measurement of Energy | |
| |
| |
Measurement of Purity | |
| |
| |
Kinetics | |
| |
| |
Final Thoughts on Measurement | |
| |
| |
Further Reading | |
| |
| |
References | |
| |
| |
| |
Thermomechanical, Dynamic Mechanical and Dielectric Methods | |
| |
| |
| |
Introduction and Principles | |
| |
| |
Thermomechanical Analysis and Thermodilatometry | |
| |
| |
Dynamic Mechanical Analysis | |
| |
| |
Dielectric Techniques | |
| |
| |
Instrumentation | |
| |
| |
Thermomechanical Analysis | |
| |
| |
Dynamic Mechanical Analysis | |
| |
| |
Dielectric Techniques | |
| |
| |
Typical Experiments | |
| |
| |
Thermomechanical Analysis | |
| |
| |
Dynamic Mechanical Analysis | |
| |
| |
Dielectric Techniques | |
| |
| |
Applications | |
| |
| |
Thermomechanical Analysis | |
| |
| |
Dynamic Mechanical Analysis | |
| |
| |
Dielectric Thermal Analysis | |
| |
| |
Modulated Temperature Thermomechanical and Dielectric Techniques | |
| |
| |
Concluding Remarks | |
| |
| |
Acknowledgements | |
| |
| |
Further Reading | |
| |
| |
References | |
| |
| |
| |
Calorimetry | |
| |
| |
| |
Introduction | |
| |
| |
Definition of Calorimetry | |
| |
| |
Thermochemistry and Thermodynamics | |
| |
| |
The First law of Thermodynamics | |
| |
| |
The Second Law of Thermodynamics | |
| |
| |
The Third Law of Thermodynamics | |
| |
| |
Calorimeters | |
| |
| |
Classification of Calorimeters | |
| |
| |
Calibration | |
| |
| |
Instrumentation: Calorimeters for Special Purposes | |
| |
| |
Solution Calorimeters | |
| |
| |
Combustion Calorimeters | |
| |
| |
Reaction Hazard Calorimeters | |
| |
| |
Isothermal Calorimeters | |
| |
| |
Applications of Isothermal Calorimetry | |
| |
| |
Calorimetric Information | |
| |
| |
The Calorimetric Signal | |
| |
| |
Reaction Mechanism | |
| |
| |
Kinetic Information | |
| |
| |
Examples of Calorimetric Applications | |
| |
| |
Chemical Reactions | |
| |
| |
Physical Changes | |
| |
| |
Summary | |
| |
| |
Acknowledgements | |
| |
| |
References | |
| |
| |
| |
Simultaneous Thermal Analysis Techniques | |
| |
| |
| |
Introduction: The Rationale behind the Simultaneous Approach | |
| |
| |
Simultaneous Thermogravimetry--Differential Thermal Analysis (TG-DTA) | |
| |
| |
Istrumentation | |
| |
| |
Applications of TG-DTA | |
| |
| |
Simultaneous Thermogravimetry--Differential Scanning Calorimetry (TG-DSC) | |
| |
| |
Instrumentation | |
| |
| |
Applications of TG-DSC | |
| |
| |
Evolved Gas Analysis (EGA) | |
| |
| |
Introduction | |
| |
| |
Instrumentation for EGA | |
| |
| |
Applications of EGA | |
| |
| |
Less Common Techniques | |
| |
| |
Optical Techniques | |
| |
| |
Spectroscopic Techniques | |
| |
| |
X-Ray Techniques | |
| |
| |
DTA--Rheometry | |
| |
| |
Micro-thermal Analysis ([mu]-TA) | |
| |
| |
Summary | |
| |
| |
References | |
| |
| |
Appendices | |
| |
| |
| |
Symbols for Physical Quantities and Units | |
| |
| |
Nomenclature for Thermal Analysis and Calorimetry | |
| |
| |
| |
Sources of Information | |
| |
| |
| |
Journals | |
| |
| |
| |
Major Textbooks on Thermal Analysis and Calorimetry | |
| |
| |
| |
Videos, CD-Roms etc. | |
| |
| |
| |
Conference Proceedings | |
| |
| |
| |
ICTAC and Its Affiliated Societies in Europe and the USA | |
| |
| |
| |
American and Other Standard Test Methods | |
| |
| |
| |
American Society for Testing and Materials (ASTM) Methods | |
| |
| |
| |
British Standards | |
| |
| |
| |
Manufacturers, Consultants and Other Suppliers | |
| |
| |
| |
Consultancies and Other Groups | |
| |
| |
Subject Index | |