Introduction to Thermal Analysis Techniques and applications

The aim of this book is, as its title suggests, to help sOilleone with little or no knowledge of what thermal analysis can do, to find out briefly what the subject is all about, to decide whether it will be of use to him or her, and to help in getting started on the more common techniques. Some of the less-common techniques are mentioned, but more specialized texts should be consulted before venturing into these areas. This book arose out of a set of notes prepared for courses on thermal analysis given at instrument workshops organized by'the S.A. Chemical Institute. It has also been useful for similar short courses given at various universities and technikons. I have made extensive use ofthe manufacturers' literature, and I am grateful to them for this information. A wide variety of applications has been drawn from the literature to use as examples and these are acknowledged in the text. A fuller list of the books, reviews and other literature ofthermal analysis is given towards the back of this book. The ICTA booklet 'For Better Thermal Analysis' is also a valuable source of information. I am particularly grateful to my wife, Cindy, for typing the manuscript, to Mrs Heather Wilson for the line drawings, and to Professor David Dollimore of the University of Toledo, Ohio, for many helpful suggestions.

1. Introduction.- 1.1 Definition and history.- 1.2 Thermal analysis instruments.- 1.3 Types of measurement.- 1.4 The main techniques.- 1.5 References.- 2. Thermal events.- 2.1 Reactions of solids.- 2.2 References.- 3. Thermogravimetry (TG).- 3.1 Introduction.- 3.2 The balance.- 3.3 Heating the sample.- 3.4 The atmosphere.- 3.5 The sample.- 3.6 Temperature measurement and calibration.- 3 7 Temperature programmers.- 3.8 Interpretation of TG and DTG curves.- 3.9 Applications of TG.- 3.10 References.- 4. Differential thermal analysis (DTA) and differential scanning calorimetry (DSC).- 4.1 Classical DTA.- 4.2 Calorimetric DTA or heat-flux DSC.- 4.3 Differential scanning calorimetry (DSC).- 4.4 Comparison of the principles of DTA and DSC.- 4.5 Sample containers and sampling.- 4.6 Quantitative aspects of DTA and DSC curves.- 4.7 Interpretation of DTA and DSC curves.- 4.8 Measurement of heat capacity.- 4.9 Measurement of thermal conductivity.- 4.10 Determination of phase diagrams.- 4.11 General applications of DTA and DSC.- 4.12 References.- 5. Thermoptometry (TD).- 5.1 Introduction.- 5.2 Thermomicroscopy.- 5.3 Thermophotometry.- 5.4 Thermoluminescence.- 5.5 Electron microscopy.- 5.6 References.- 6. Thermodilatometry (TD).- 6.1 Basic principles.- 6.2 Practical details.- 6.3 Interpretation of results.- 6.4 Applications of thermodilatometry.- 6.5 References.- 7. Thermomechanical analysis (TMA).- 7.1 Basic principles.- 7.2 Practical details.- 7.3 Applications of TMA.- 7.4 References.- 8. Dynamic mechanical analysis (DMA) or dynamic thermomechanometry.- 8.1 Basic principles.- 8.2 Applications of DMA.- 8.3 References.- 9. Combination of thermal analysis techniques.- 9.1 Principles.- 9.2 References.- 10. Evolved gas analysis (EGA).- 10.1 Basic principles.- 10.2 Evolved gas detection(EGD).- 10.3 Evolved gas analysis (EGA).- 10.4 Applications of EGD and EGA.- 10.5 References.- 11. Less-common techniques.- 11.1 Emanation thermal analysis (ETA).- 11.2 Thermomagnetometry (TM).- 11.3 Thermoelectrometry.- 11.4 Thermosonimetry (TS) and thermoacoustimetry.- 11.5 References.- 12. The use of microcomputers in thermal analysis.- 12.1 Introduction.- 12.2 Hardware requirements.- 12.3 Software requirements.- 12.4 Data storage.- 12.5 Data processing.- 12.6 Additional benefits.- 12.7 Automation of thermal analysis equipment.- 12.8 References.- 13. Reaction kinetics from thermal analysis.- 13.1 Introduction.- 13.2 Heterogeneous reactions.- 13.3 Formulation of the problem.- 13.4 Differential methods.- 13.5 Integral methods.- 13.6 The influences of various parameters on the shapes of theoretical thermal analysis curves.- 13.7 Conclusion.- 13.8 References.- 14. Purity determination using DSC.- 14.1 Introduction.- 14.2 Phase equilibria.- 14.3 The DSC melting curve.- 14.4 Corrections.- 14.5 Step methods.- 14.6 Conclusions.- 14.7 References.- 15. The literature and nomenclature of thermal analysis.- 15.1 Books.- 15.2 Reviews.- 15.3 Conference proceedings.- 15.4 Journals.- 15.5 Manufacturer’s literature.- 15.6 The nomenclature of thermal analysis.- 16. Thermal analysis equipment.- 16.1 Choosing thermal analysis equipment.- 16.2 Major suppliers of thermal analysis equipment.- 17. Conclusion.- Appendix A. Introductory experiments in thermal analysis.- A.1 Differential scanning calorimetry (DSC).- A.2 Thermogravimetry (TG).- Appendix B. Thermal analysis software.- B.1,2 Data capture and storage.- B.3 Display of data.- B.4 Modification of the data.- B.5 Processing of the data.- Appendix C. Explanation of the symbols used in the text.