Chapter 1 Introduction 1

Section 1 A Brief History of Thermal Analysis 1

Terminology of thermal analysis in the second quarter 2

I. Evolution and Development of Thermal Analysis Terminology 2

Second, the definition and classification of thermal analysis 3

Three. General terms for thermal analysis 4

Section 3 Basic Characteristics and Data Report of Thermal Analysis 4

I. Basic characteristics of thermal analysis 4

Second, the thermal analysis data report 5

Section 4 Temperature and heat standards for thermal analysis 6

I. Temperature calibration by thermogravimetry 6

2. Temperature Calibration of Differential Thermal Analyzer and Differential Scanning Calorimeter 6

Three, differential thermal analyzer and differential scanning calorimeter heat calibration 8

Four. Determination of Calibration Coefficient K of Differential Scanning Calorimeter 8

Section 5 Standard Test Method for Thermal Analysis 9

Reference 10

Chapter II Thermal Analyzer 1 1

Section 1 Overview 1 1

I. Basic composition of thermal analyzer 1 1

Second, the commodity thermal analysis instrument 1 1

Three. Computer software 12

Common thermal analysis instruments in the second quarter 13

I. Thermogravimetric Method (TG) 13

Second, differential thermal analysis (DTA) and differential scanning calorimetry (DSC) 15

Three. Thermodynamic method 20

Four. Thermal expansion method 22

Section 3 Optical, Electrical and Acoustic Thermal Analysis Methods 23

A, alternating heating method (ACC)23

Second, the thermoelectric current measurement (TSC)24

Three, thermoluminescence (TL)25

Four, thermal diffusion temperature wave analysis (TWA) measurement 26

In the fourth quarter, the combination of thermal analysis and other analysis methods 28

I. thermal microscopy 28

Second, x? Ray diffraction? DSC29

Three, escape gas analysis (EGA)29

Fourth, light? Thermal transient radiation measurement (OTTER)39

Section 5 Automatic Sampling Thermal Analysis System 40

Section 6 Installation and Use of Instruments 40

Reference 4 1

Chapter 3 Experimental factors, thermal analysis kinetics and data expression affecting thermal analysis and measurement 42

Section 1 Experimental Factors Affecting Thermal Analysis and Measurement 42

I. Influence of heating rate on experimental results of thermal analysis 42

Second, the influence of sample dosage and particle size on the experimental results of thermal analysis 42 pages

Three. Influence of atmosphere on experimental results of thermal analysis 43

Four. Influence of buoyancy, convection and turbulence on TG curve 44

Verb (abbreviation of verb) sample container and its temperature gradient and reaction degree of each part of the sample 44

Influence of the compactness of intransitive verbs on the experimental results of thermal analysis 45

In the second quarter, the discrimination method of instrument resolution 46

In the third quarter, thermal analysis kinetics 46

I. Determination of kinetic parameters of thermal analysis reaction 46

Second, the judgment of thermal analysis reaction mechanism 49

Three. Judgment of mechanism of isothermal solid-state reaction process 50

Four. Determination of non-isothermal crystallization kinetics of polymers 50

Verb (abbreviation of verb) Overview of resin curing reaction kinetics at constant temperature 53

Solution of kinetic parameters of resin curing reaction of intransitive verb 54

Seven, the new progress of thermal analysis kinetics 56

The fourth quarter thermal analysis curve and the judgment of the end point of the reaction 58

I. Thermal Analysis Curve and Its Representation Method 58

Second, the differential thermal analysis curve (DTA curve) reaction endpoint judgment 59

Three. Determination of thermal time constant RCs and minimum separation temperature l of DTA 59

Section 5 Quantitative Processing of Thermogravimetric Data of Step-by-Step Reaction 6 1

Quantitative determination of calcium oxalate hydrate 1 gradual weightlessness process

2. High resolution thermogravimetric measurement of copper sulfate pentahydrate (CuSO4 5h2o)1dehydration process.

Reference 62

The fourth chapter uses thermal analysis technology to determine various transformations.

The first section determination of glass transition 64

I. Glass transition temperature Tg DTA or DSC method 64

MDSC determination of glass transition of PET/ABS*** mixture 65

III. Glass transition temperatures of polymers and plasticizers 66

Four. Relationship between glass transition temperature and molecular weight of polymer 67

Verb (abbreviation for verb) Enthalpy relaxation 67

Molecular constants C 1 and C268 in the intransitive verb WLF equation

Seven. Relaxation activation energy of polymer glass transition zone 70

Eight. Transition temperature T2, free volume fraction and thermal expansion coefficient 70 of the polymer.

Section 2 Determination of Crystallization and Melting 7 1

1. Melting and crystallization temperature 7 1

Second, the determination of the equilibrium melting point of crystalline polymer 73

Three. Crystalline equilibrium melting point, interaction parameters and interaction energy density of * * * polymer and * * * mixture 74.

4. Determination of melting enthalpy and melting entropy of crystalline polymer by dilution method and equilibrium melting point method.

V. Determination of melting enthalpy and melting entropy of polymer by specific volume method 75

Interfacial free energy during crystallization of intransitive verbs.

Seven. Crystal region transition of polymer 77

Eight, the determination of molecular chain migration activation energy in the process of polymer crystallization 78

Nine. Isothermal crystallization of polymers 79

X. determination of isothermal crystallization rate 80

XI。 The radial growth rate of spherulites during isothermal crystallization of supercooled polymer melt was measured by polarizing microscope (8 1).

Twelve. Determination of isothermal crystallization heat 82

Thirteen. Determination of heat of melting and crystallization of polymers 83

Fourteen Determination of crystallinity of polymer 84

15. MDSC determination of crystallinity of original sample of crystalline polymer 85

Sixteen. The crystallinity of PET under different molding conditions is 86.

Density, melting and crystallinity of polyethylene 87

18. Multiple melting peaks of polyethylene 87

Nineteen. Heat of conversion of lipids 87

20. Polymorphism of tridecane 88

Twenty-one, thermotropic liquid crystal 88

22. Thermotropic polymer liquid crystal 90

23. The wax content of lubricating oil is 9 1

XXIV. Determination of Solid Fat Index of Oils and Fats 9 1

Twenty-five, draw a binary system phase diagram 92

Section 3 Determination of Composition and Compatibility of Polymer Mixtures 93

I. Determination of composition of polymer mixture 93

Second, the glass transition temperature of random * * * polymer and the composition of * * * polymer 93

Three. Compatibility of partially compatible polymer mixtures 94

Four, compatible polymer * * * mixed system 95

The verb (abbreviation for verb) contains a compatible mixed system of crystalline polymers 96

6. Liquid of polymer * * * mixed system? Liquid phase behavior 97

Seven, the upper and lower critical compatibility temperature 98

VIII. Compatibility of Polyimide/Polythioimide * * * DMA Determination 99

The fourth quarter thermodynamic analysis (TMA) and dynamic thermodynamic analysis (DMA) 100

1. Determination of Anisotropy of Polymer Materials by TMA 100

Secondly, the reinforcing agent inhibits the deformation of polyethylene film 10 1

Three. Determination of permeability and tensile strength of polymer films TMA 10 1

4. The apparent activation energy of polymer transition determined by dynamic viscoelasticity is 102.

Drawing of dynamic viscoelastic measurement combination curve of verb (abbreviation of verb) 102

The fifth water-saving measurement 104

First, water? Determination of ethanol mixture by DSC 104

Second, the thermal analysis of free water and bound water 105

Three. Determination of moisture in manganese dioxide 105

Four. Pressurized dehydration process of hydrated alumina 106

Section 6 Thermal Analysis of Metals and Alloys 107

I. Determination of thermodynamic parameters of phase transition between metals and alloys 107

Second, the determination of kinetic parameters of phase transformation between metal and alloy 1 1 1

Determination of specific heat capacity of metals and alloys 1 14

Four. Oxidation resistance of metals and alloys 1 16

Verb (abbreviation of verb) Measurement of thermal expansion coefficient of amorphous alloy and DMA measurement 1 16

Section 7 Other determinations related to transformation 1 16

1.DSC determination of frozen cells in suspension 1 16

Second, the polymer transition and its thermal history 1 17

III. Thermal Analysis of Silicone Rubber 1 18

Four. Thermal analysis of mixed oil 1 19

V. DSC determination of edible meat 1 19

Dielectric analysis of intransitive verb polymethyl methacrylate 120

Reference 12 1

Chapter 5 Determination of various reactions by thermal analysis technology 124

Section 1 Determination of Thermal Stability 124

I. Relative thermal stability of polymer materials 124

II. Toop Method for Evaluating Temperature Index of Insulating Materials 126

Three. Thermal Secant Method for Evaluating Temperature Index of Electrical Insulating Materials 127

Four. Determination of oxidation induction period of organic materials 127

Section 2 Crosslinking and Polymerization 128

I. Curing Reaction of Epoxy Resin and Its Glass Transition 128

II. Contents, Fabrication and Significance of Isothermal Curing "Three T" Diagram 129

III. Thermometry of Photopolymerization 130

Four. Determination of post-polymerization reaction of photosensitive resin monomer 13 1

Section III Evaluation of Solid Catalysts 132

I. Evaluation of Metal Catalysts 132

Second, the catalyst phase analysis (DTA? EGD method) 132

Three. Selection of oxidation activity of automobile exhaust purification catalyst 133

Iv. Selection of catalyst preparation methods 134

Verb (abbreviation of verb) Determination of surface acidity of solid catalyst 135

Study on poisoning effect and regeneration of intransitive verb 136 catalyst

Seven, catalyst carbon deposition and charring 137

The fourth quarter wood thermal analysis 138

1. TG of cellulose thermal decomposition? DTA？ Determination of 138 by infrared spectroscopy

Second, the determination method of cellulose acid hydrolysis 139

Three. Determination of Oxidation Stability of Rosin 139

Four. Determination of combustion characteristics of flame retardant wood 140

Section 5 Thermal Analysis of Energetic Materials and Coal 140

I. Tracking of Transient Reaction of High Energy Materials 140

Second, the self-reactive substance 14 1

Three. Industrial analysis of coal and coke 142

IV. Determination of calorific value of coal 143

Section 6 Thermogravimetric Determination of Mineral Quantification and Homomorphism 143

I quantitative thermogravimetric analysis of minerals 143

II. Determination of Isomorphic Component Content of Substances 144

Section 7 Other Determination Related to Reaction 145

I. Determination of Thermal Decomposition of Heat Transfer Oil 145

Second, the determination of oil oxidation reaction 146

Three. Determination of carbon black content in rubber 146

4. DSC determination of gypsum converted into plaster of Paris 147.

Verb (abbreviation of verb) Determination of reaction between metal and gas 148

TG determination of the reaction between intransitive verb CaO and SO2 148

Reference 149

Chapter VI Thermal Analysis and Determination of Material Characteristic Parameters 150

The first section determination of thermodynamic parameters 150

1. DSC determination of specific heat capacity 150

Second, the determination method of linear expansion coefficient TMA 15 1

Iii. Determination of thermal diffusivity 15 1

Four. Determination of thermal conductivity 153

Determination of purity in the second quarter 154

Section 3 Determination of Porosity by Calorimetry 155

Reference 156

Second thermal analysis curve and data set

Chapter VII Thermal Analysis Curve of Polymer Materials 157

Section 1 Thermal Analysis Curve of Ordinary Polymer 157

I. Thermal Analysis Curve of Polyolefin and Its Polymer 157

2. Thermal analysis curves of elastomers such as polystyrene, polyvinyl chloride, styrene-butadiene polymer and polyisoprene 162.

3. Thermal analysis curves of epoxy resin, polyacetal, polyacrylonitrile, polyamide, polyester and cotton yarn 168.

Section 2 Special polymers (PTFE, polyarylate, polyphenylene sulfide, polysulfone, polyimide, polyetheretherketone and

Thermal analysis curve of conductive polymer 175)

In the third quarter, other polymer materials (polyurethane, cellulose, polymer aqueous system and several * * * polymers, * * mixtures,

Interpenetrating polymer networks, etc. ) 182.

Section IV Diagram of Relationship between Polymer Transition Temperature and Frequency 190

Reference 195

Chapter VIII Thermal analysis curves of food additives and food. 196

Section 1 Thermal Analysis Curve of Food Additives 196

In the second quarter, thermal analysis curves of wine, chocolate, edible solid fat, cream and hydrogenated soybean oil 206

Section III Thermal Analysis Curve of Palm Oil and Coconut Oil 208

Section IV Thermal Analysis Curve of Alkanes in Rice, Starch, Gelatin, protein, Animal Organs and Cornus officinalis 209.

Reference 2 14

Chapter 9 Thermal Analysis Curve of Drugs, Biology, Wood and Their Components 2 15

The first section drug thermal analysis curve 2 15

In the second quarter, the thermal analysis curve of organisms 235

In the third quarter, the thermal analysis curve of wood and its components 239

Reference 245

Chapter 10 Thermal analysis curve of minerals 246

The first section thermal characteristics of natural elements 246

In the second quarter, the thermal characteristics of halide, sulfide and oxide minerals 249

I. Thermal characteristics of halides 249

2. Thermal characteristics of sulfide minerals 25 1

Three. Thermal characteristics of oxide minerals 263

In the third quarter, the thermal characteristics of inorganic minerals 27 1

I. Thermal characteristics of sulfate minerals 27 1

Second, the thermal characteristics of carbonate minerals 28 1

Third, the thermal characteristics of borate minerals 286

Four, the thermal characteristics of phosphate minerals 290

Verb (abbreviation of verb) Thermal characteristics of arsenate mineral 293

Thermal characteristics of silicate minerals in intransitive verbs 295

Reference 3 10

Chapter XI Thermal Analysis Curve of Energetic Materials 3 1 1

Section 1 Thermal Analysis Curve of Simple Explosive 3 1 1

Thermal analysis curve of mixed explosives in the second quarter 339

1. Thermal analysis curves of two kinds of mixed explosives

Second, the thermal analysis curve of binary single explosive mixing system 340

In the third quarter, thermal analysis curves of mononitrotoluene, nitrochlorobenzene and m-nitroaniline 347

In the fourth quarter, thermal analysis curves of primary explosive and molybdenum-barium chromate-potassium perchlorate delay explosive 349

Section 5 Thermal Analysis Curve of Powder and Black Powder 356

Section VI Thermal Analysis Curve of Solid Rocket Propellant 363

Section 7 Thermal analysis curve of gunpowder-related substances 365

Reference 368

Chapter 12 Thermal analysis curve of inorganic compounds 372

Section 1 Thermal Analysis Curve of Rare Earth Bromide Complexes with Glycine/Alanine 372

Section II Thermal Analysis Curve of Transition Metal Schiff Base Complexes 38 1

In the third quarter, thermal analysis curves of other rare earth complexes 386

Reference document 396

Chapter XIII DTA? EGD？ GC combination curve and data 397

The first section solid catalyst evaluation 397

In the second quarter, the thermal (oxidation) stability of petroleum antioxidant additives 407

Thermal characteristics evaluation of the third coal saving 4 10

The fourth quarter mineral identification 427

Section 5 Identification of various compounds 440

Reference document 460

Appendix 462

A. Calibrate the specific heat capacity of material 462.

(a) calibration material α? Specific heat capacity of alumina 462

(2) Calibrating the specific heat capacity of benzoic acid 462

(3) Calibrating the specific heat capacity of copper 463.

(4) Calibrating the specific heat capacity of material water 463

(5) Calibrating the specific heat capacity of potassium chloride 463.

Second, the thermal conductivity of the solid element 464.

Thirdly, the melting point Tm and heat of fusion Δ Δ HM465 of the calibration substance are calibrated.

Iv. ICTA calibration temperature calibration material 465

V. fundamental constants of physics value 465

Six, thermocouple temperature thermoelectric electromotive force (millivolts) comparison table 466

(a) platinum rhodium 10? Platinum thermocouple graduation table 466

(2) platinum rhodium 30? Platinum rhodium 6 thermocouple graduation table 470

(3) Nickel chromium? Nickel silicon (nickel chromium? Nickel aluminum) thermocouple graduation table 474

(4) copper? Kangtong thermocouple graduation table 478

(5) platinum rhodium 13? Platinum thermocouple graduation table 480

(6) Nickel chromium? Copper thermocouple graduation table 484

Seven, commonly used thermal analysis glossary 486

Eight, common minerals and other inorganic melting point table 488

Nine. Melting point table of common organic compounds 502

Reference 509

Thermal analysis curve index 5 10

Composite index 524

List of symbols and abbreviations in this book 536