Thermal Analysis
Fundamentals and Applications to Polymer Science
Second Edition
T. Hatakeyama
Otsuma Women's University, Faculty of Home Economics, Tokyo, Japan
F.X. Quinn
L'Oréal Recherche Avancée, Aulnay-sous-Bois, France

Contents
Preface ix
Preface to the Second Edition x
1
Thermal Analysis
1
1.1 Definition 1
1.2 Characteristics of Thermal Analysis 2
1.3 Conformation of Thermal Analysis Instruments 3
1.4 Book Outline 4
2
Differential Thermal Analysis and Differential Scanning
Calorimetry
5
2.1 Differential Thermal Analysis (DTA) 5
2.1.1 Custom DTA 7
2.2 Quantitative DTA (Heat-Flux DSC) 8
2.3 Triple-Cell Quantitative DTA 10
2.4 Power Compensation Differential Scanning
Calorimetry (DSC)
11
2.5 Temperature Modulated DSC (TMDSC) 12
2.5.1 General Principles of Temperature
Modulated DSC
13
2.5.2 TMDSC Calibration 18
2.5.3 TMDSC Experimental Conditions 18
2.6 High-Sensitivity DSC (HS-DSC) 20
2.7 Data Analysis and Computer Software 21
2.8 Automated TA Systems 22
2.9 Simultaneous TA 22
2.10 Installation and Maintenance 22
2.11 References 24
3
Calibration and Sample Preparation
25
3.1 Baseline 25
3.1.1 Baseline Curvature and Noise 25
3.1.2 Baseline Subtraction 27
3.1.3 Baseline Correction 28
3.2 Temperature and Enthalpy Calibration 28
3.3 Sample Vessel 29
3.4 Sample Preparation 32
3.4.1 Films, Sheets and Membranes 33
3.4.2 Granules and Blocks 34
3.4.3 Powders 34
3.4.4 Fibres and Fabrics 34
3.4.5 Biomaterials and Gels 35
3.4.6 Storing Samples 35
3.5 Temperature Gradient in Sample 36
3.5.1 Mass of Sample 37
3.5.2 Solutions 39
3.6 Sample Packing 39
3.6.1 Hydrophilic Sample 40
3.6.2 Liquid Sample 40
3.7 Purge Gas 41
3.8 Scanning Rate 41
3.9 Sub-ambient Operation 43
4
Thermogravimetry
45
4.1 Introduction 45
4.2 Thermobalance 46
4.2.1 Installation and Maintenance 46
4.2.2 Microbalance and Crucible 47
4.2.3 Furnace and Temperature Programmer 50
4.2.4 Data Recording Unit 54
4.3 Temperature Calibration 55
4.4 Sample 58
4.5 Atmosphere 61
4.6 Heating Rate 63
4.7 Classification of TG Curves 65
4.8 Calculation of Mass Change Rates 66
4.9 Derivative Thermogravimetry (DTG) 68
4.10 Intercomparison of TG and DTA 68
4.11 TG Reports 70
4.12 References 71
5
Applications of Thermal Analysis
72
5.1 Temperature Measurement 72
5.2 Enthalpy Measurement 74
5.2.1 Polymer Melting (Initial Crystallinity) 75
5.3 Reaction Rate Kinetics 77
5.3.1 Differential Methods 80
5.3.2 Integral Methods 82
5.3.3 Jump Method 84
5.3.4 Isothermal Crystallization of Polymers 85
5.3.5 General Comment on Reaction Rate
Kinetics
88
5.4 Glass Transition of Polymers 90
5.4.1 Enthalpy Relaxation of Glassy Polymers 91
5.4.2 Enthalpy Relaxation Measurement by
TMDSC
95
5.4.3 Glass Transition Measurement by TMDSC 95
5.4.4 Glass Transition in the Presence of Water 96
5.5 Heat Capacity Measurement by DSC 97
5.6 Heat Capacity Measurement by TMDSC 100
5.7 Purity Determination by DSC 102
5.7.1 Thermal Lag 103
5.7.2 Undetected Premelting 103
5.7.3 General Comment on Purity Determination
by DSC
104
5.8 Crystallinity Determination by DSC 105
5.9 Molecular Rearrangement during Scanning 106
5.10 Polymorphism 107
5.11 Annealing 109
5.12 Bound Water Content 109
5.12.1 Experimental Procedure 112
5.13 Phase Diagram 113
5.14 Gel-Sol Transition 115
5.14.1 Other Applications of HS-DSC 117
5.15 References 118
6
Other Thermal Analysis Methods
119
6.1 Evolved Gas Analysis 119
6.1.1 Mass Spectrometry (MS) 119
6.1.2 Fourier Transform Infrared (FTIR)
Spectroscopy
120
6.1.3 Gas Chromatography (GC) 121
6.1.4 TG-EGA Report 123
6.2 Mechanical Analysis 125
6.2.1 Thermomechanical Analysis (TMA) 126
6.2.2 Dynamic Mechanical Analysis (DMA) 130
6.2.3 TMA and DMA Reports 133
6.3 Dilatometry 133
6.3.1 Dilatometer Assembly 133
6.3.2 Definition of Expansion Coefficients 135
6.4 Thermomicroscopy 136
6.4.1 Observation by Reflected Light 137
6.4.2 Observation by Transmitted Light 137
6.5 Simultaneous DSC-X-Ray Analysis 139
6.6 Thermoluminescence (TL) 139
6.7 Alternating Current Calorimetry (ACC) 142
6.8 Thermal Diffusivity (TD) Measurement by
Temperature Wave Method
145
6.9 Thermally Stimulated Current (TSC) 148
6.10 Thermal Conductivity 152
6.11 Micro-thermal Analysis (μTA) 153
6.12 Optothermal Transient Emission Radiometry
(OTTER)
154
6.13 Specific Heat Spectroscopy 155
6.14 References 156
Appendix 1
Glossary of TA Terms
158
Appendix 2
Standard Reference Materials
164
Appendix 3
Physical Constants and Conversion Tables
167
Chemical Formula Index 172
Subject Index 175

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