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Handbook of Thermal Analysis and Calorimetry
Recent Advances, Techniques and Applications
1st Edition, Volume 5 - November 7, 2007
Editors: Michael E. Brown, Patrick K. Gallagher
Language: English
Hardback ISBN:9780444531230
9 7 8 - 0 - 4 4 4 - 5 3 1 2 3 - 0
eBook ISBN:9780080556314
9 7 8 - 0 - 0 8 - 0 5 5 6 3 1 - 4
This is Volume 5 of a Handbook that has been well-received by the thermal analysis and calorimetry community. All chapters in all five volumes are written by international experts…Read more
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This is Volume 5 of a Handbook that has been well-received by the thermal analysis and calorimetry community. All chapters in all five volumes are written by international experts in the subject. The fifth volume covers recent advances in techniques and applications that complement the earlier volumes. The chapters refer wherever possible to earlier volumes, but each is complete in itself. The latest recommendations on Nomenclature are also included. Amongst the important new techniques that are covered are micro-thermal analysis, pulsed thermal analysis, fast-scanning calorimetery and the use of quartz-crystal microbalances. There are detailed reviews of heating - stage spectroscopy, the range of electrical techniques available, applications in rheology, catalysis and the study of nanoparticles. The development and application of isoconversional methods of kinetic analysis are described and there are comprehensive chapters on the many facets of thermochemistry and of measuring thermophysical properties. Applications to inorganic and coordination chemistry are reviewed, as are the latest applications in medical and dental sciences, including the importance of polymorphism. The volume concludes with a review of the use and importance of thermal analysis and calorimetry in quality control.
* Updates and complements previous volumes * Internationally recognized experts as authors * Each chapter complete in itself
Researchers in wide scientific applications, Practitioners, Libraries
CHAPTER 1. INTRODUCTION TO RECENT ADVANCES, TECHNIQUES AND APPLICATIONS (Michael E. Brown and Patrick K. Gallagher)
1. THE HANDBOOK OF THERMAL ANALYSIS AND CALORIMETRY 1
2. THE LITERATURE OF THERMAL ANALYSIS AND CALORIMETRY 2
2.1. Books 2
2.2. Major conferences and their proceedings 3
2.3. Websites 5
3. NOMENCLATURE 6
4. RECENT ADVANCES IN TECHNIQUES 6
4.1. Micro-Thermal Analysis 6
4.2. Pulsed thermal analysis 7
4.3. Fast scanning calorimetry 7
5. ADVANCES IN APPLICATIONS 7
5.1. Quartz-crystal microbalances 7
5.2. Electrical techniques 8
5.3. Heating-stage spectroscopy 8
5.4. Rheology 8
5.5. Catalysis 9
5.6. Nanoparticles 9
6. KINETICS 9
7. ADDITIONAL TOPICS 10
7.1. Thermochemistry 10
7.2. Coordination compounds and inorganics 10
7.3. Thermophysical properties 11
7.4. Polymorphism 11
7.5. Medical applications 11
7.6. Dental materials 12
8. QUALITY CONTROL 12
CHAPTER 2. DEVELOPMENTS IN NOMENCLATURE (Jean Rouquerol, I. Wadsö, T. Lever and P. Haines)
1. INTRODUCTION 13
2. 2006 ICTAC NOMENCLATURE OF THERMAL ANALYSIS 14
2.1. Scope 14
2.2. Intent 15
2.3. Definition of the field of Thermal Analysis (TA) 15
2.4. Techniques 15
2.5. Terminology and Glossary 16
2.6. Experimental conditions 22
2.7. Symbols used specifically in Thermal Analysis 22
2.8. Overview and historical matters 23
2.9. Recent Members of the ICTAC Nomenclature Committee 24
3. COMMENTS ON THE 2006 ICTAC NOMENCLATURE OF THERMAL ANALYSIS 24
4. A CONVENIENT NOMENCLATURE FOR CALORIMETERS 28
4.1. Basic representation, criteria and categories 28
4.2. “Passive” adiabatic calorimeters 30
4.3. “Active” adiabatic calorimeters 32
4.4. "Passive" diathermal calorimeters 34
4.5. “Active” diathermal calorimeters 35
5. OTHER POSSIBLE NOMENCLATURES FOR CALORIMETERS 37
5.1. Nomenclature proposed by Swietoslawski in 1933 37
5.2. Nomenclature proposed by Calvet and Prat in 1956 37
5.3. Nomenclature proposed by Evans in 1969 39
5.4. Nomenclature proposed by Skinner in 1969 39
5.5. Nomenclature proposed by Rouquerol and Laffitte in 1972 40
5.6. Nomenclature proposed by Hemminger and Höhne in 1984 41
5.7. Nomenclature proposed by Rouquerol and Zielenkiewicz in 1986 44
5.8. Nomenclature proposed by Tachoire and Médard in 1994 44
5.9. Nomenclature proposed by Wadsö in 1997 45
5.10. Nomenclature proposed by Hemminger and Särge in 1999 46
5.11. Nomenclature proposed by Hansen in 2001 47
5.12. Nomenclature proposed by Matsuo in 2004 48
5.13. Nomenclature proposed by Zielenkiewicz in 2004 50
6. CONCLUSIONS 51
7. REFERENCES 52 - 54
CHAPTER 3. MICRO-THERMAL ANALYSIS AND RELATED TECHNIQUES (Duncan M. Price)
1. INTRODUCTION 55
2. SCANNING THERMAL MICROSCOPY (STHM) 57
2.1. Introduction 57
2.2. Instrumentation for SThM 58
2.3. Probe design 59
2.4. Quantitative SThM 61
2.5. Other SThM techniques 66
3. LOCALISED THERMAL ANALYSIS 67
3.1. Principles 67
3.2. Calibration 68
3.3. Features 69
3.4. Terminology 71
3.5. Applications 71
4. LOCALISED CHEMICAL ANALYSIS 78
4.1. Introduction 78
4.2. Localised evolved gas analysis 78
4.3. Near-field photothermal spectroscopy 82
4.4. Thermally-assisted micro-sampling 83
5. CONCLUSIONS 84
6. REFERENCES 84 - 92
CHAPTER 4. PULSE THERMAL ANALYSIS (M. Maciejewski and A. Baiker)
1. INTRODUCTION 93
2. EXPERIMENTAL 94
3. CALIBRATION OF SPECTROMETRIC SIGNALS IN HYPHENATED THERMOANALYTICAL TECHNIQUES 95
3.1. Calibration of gases 95
3.2. Verification of the calibration 98
3.3. Calibration of liquids 99
4. QUANTIFICATION OF THE SPECTROMETRIC SIGNALS IN A TA-MS-FTIR SYSTEM 101
4.1. Determination of the intrinsic fragmentation in a TA-MS system 101
4.2. Application of PulseTA® for quantification of gas-solid reactions 104
5. INJECTION OF A GAS WHICH REACTS WITH THE SOLID 112
5.1. Investigations of the reduction and oxidation of solids 112
5.2. Investigation of the redox behaviour of solids: reduction and re-oxidation of CeO2 116
5.3. Investigation of gas-solid reactions 118
5.4. Miscellaneous applications 123
6. INJECTION OF A GAS WHICH ADSORBS ON THE SOLID 124
6.1. Adsorption of ammonia on HZMS-5 zeolite 124
6.2. Investigation of the adsorption and desorption of NH3 on a titania-silica aerogel 125
6.3. Investigation of adsorption combined with gas-solid reaction 126
6.4. Miscellaneous applications 129
7. CONCLUSIONS 129
8. REFERENCES 130 - 132
CHAPTER 5. THE QUARTZ CRYSTAL MICROBALANCE (Allan L. Smith)
1. HIGH SENSITIVITY BALANCES: THEIR ROLE IN THERMAL ANALYSIS AND CALORIMETRY 133
2. EARLY HISTORY OF THE QUARTZ CRYSTAL MICROBALANCE 134
3. THE LITERATURE OF THERMAL ANALYSIS AND OF THE QUARTZ CRYSTAL MICROBALANCE 135
4. PRINCIPLES OF OPERATION OF THE QUARTZ CRYSTAL MICROBALANCE (QCM) 142
5. DETECTION ELECTRONICS 147
5.1. Simple QCM driving circuits 147
5.2. Frequency and damping measurements 148
5.3. Impedance analysis 148
6. IS THE TRANSVERSE SHEAR MODE RESONATOR A TRUE MICROBALANCE? 148
7. PRACTICAL DETAILS 150
7.1. Calibration 150 7.2. Comparison of gravimetric and Sauerbrey masses 151
7.3. Sample Preparation 152
8. CHEMICAL AND BIOLOGICAL APPLICATIONS OF THE QCM 152
8.1. Film-thickness monitors in vacuum deposition 152
8.2. The metal/solution interface in electrochemical cells 153
8.3. Faraday Society Discussion No. 107, 1997 154
8.4. Determination of shear and loss modulus at QCM frequencies 155
8.5. Chemical sensors and biosensors 156
8.6. Biological surface science 158
9. SENSORS 159
9.1. Acoustic microsensors – the challenge behind microgravimetry 159
9.2. Piezoelectric sensors 159
10. THE QUARTZ CRYSTAL MICROBALANCE/HEAT CONDUCTION CALORIMETER 161
10.1. Introduction 161
10.2. Beginnings of QCM/HCC 161
10.3. Development of QCM/HCC 163
10.4. Biological applications 164
10.5. The Masscal Scientific Instruments G1 Microbalance/Calorimeter 164
10.6. Recent applications 165
10.7. Conclusion 165
11. REFERENCES 166 - 170
CHAPTER 6. HEATING STAGE SPECTROSCOPY: INFRARED, RAMAN, ENERGY DISPERSIVE X-RAY AND X-RAY PHOTOELECTRON SPECTROSCOPY (Ray L. Frost and J. Theo Kloprogge)
1. INFRARED EMISSION SPECTROSCOPY 171
1.1. Introduction 171
1.2. The theory behind infrared emission spectroscopy (IES) 173
1.3. Infrared emission spectroscopy of alunite 179
2. HEATING STAGE RAMAN SPECTROSCOPY 182
2.1 Heating stage Raman spectroscopy of weddellite 186
3. THERMAL STUDIES OF MATERIALS USING HEATING AND COOLING STAGE SCANNING ELECTRON MICROSCOPY AND ENERGY DISPERSIVE X-RAY ANALYSIS 188
3.1. Apparatus 188
3.2. Thermal decomposition of weddelite by heating stage SEM and infrared emission spectroscopy (IES) 191