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Table Of Contents

1.4.9 Factors affecting calibration
1.4.10 Final comments
1.5 Interpretation of data
1.5.1 The instrumental transient
1.5.2 Melting
1.5.3 The glass transition
1.5.4 Factors affecting Tg
1.5.5 Calculating and assigning Tg
1.5.6 Enthalpic relaxation
1.5.7 Tg on cooling
1.5.8 Methods of obtaining amorphous material
1.5.9 Reactions
1.5.10 Guidelines for interpreting data
1.6 Oscillatory temperature profiles
1.6.1 Modulated temperature methods
1.6.2 Stepwise methods
1.7 DSC design
1.7.1 Power compensation DSC
1.7.2 Heat flux DSC
1.7.3 Differential thermal analysis DTA
1.7.4 Differential photocalorimetry DPC
1.7.5 High-pressure cells
Appendix: standard DSC methods
2.1 Introduction
2.2 Proof of performance
2.2.1 Effect of high scan rates on standards
2.2.2 Definition of HyperDSCTM
2.2.3 The initial transient
2.2.4 Fast cooling rates
2.3 Benefits of fast scanning rates
2.3.1 Sensitivity
2.3.3 Separate overlapping events based on different kinetics
2.3.4 Speed of analysis
2.4 Application to polymers
2.4.1 Melting and crystallisation processes
2.4.2 Comparative studies
2.4.3 Forensic studies
2.4.4 Effect of heating rate on the sensitivity of the glass transition
2.4.5 Effect of heating rate on the temperature of the glass transition
2.5 Application to pharmaceuticals
2.5.1 Purity of polymorphic form
2.5.2 Identifying polymorphs
2.5.3 Determination of amorphous content of materials
2.5.4 Measurements of solubility
2.6 Application to water-based solutions and the effect of moisture
2.6.1 Measurement of Tg in frozen solutions and suspensions
2.6.2 Material affected by moisture
2.7 Practical aspects of scanning at fast rates
2.7.1 Purge gas
2.7.2 Sample pans
2.7.3 Sample size
2.7.4 Scan rate
2.7.5 Instrumental settings
2.7.6 Cleanliness
2.7.7 Getting started
References
3.1 Introduction
3.2 Design and measuring principle
3.2.1 Buoyancy correction
3.3 Sample preparation
3.4 Performing measurements
3.4.1 Influence of heating rate
3.4.2 Influence of crucible
3.4.3 Influence of furnace atmosphere
3.4.4 Influence of residual oxygen in inert atmosphere
3.4.5 Influence of reduced pressure
3.4.6 Influence of humidity control
3.4.7 Special points in connection with automatic sample changers
3.5 Interpreting TGA curves
3.5.1 Chemical reactions
3.5.2 Gravimetric effects on melting
3.5.3 Other gravimetric effects
3.5.4 Identifying artefacts
3.5.5 Final comments on the interpretation of TGA curves
3.6 Quantitative evaluation of TGA data
3.6.1 Horizontal or tangential step evaluation
3.6.2 Determination of content
3.6.3 The empirical content
3.6.4 Reaction conversion,
3.7 Stoichiometric considerations
3.8 Typical application: rubber analysis
3.9 Analysis overview
3.10 Calibration and adjustment
3.10.1 Standard TGA methods
3.11 Evolved gas analysis
3.11.1 Brief introduction to mass spectrometry
3.11.2 Brief introduction to Fourier transform infrared spectrometry
3.11.3 Examples
Reference
4.1 Thermal analysis using mechanical property measurement
4.1.1 Introduction
4.1.2 Viscoelastic behaviour
4.1.3 The glass transition, Tg
4.1.4 Sub-Tg relaxations
4.2 Theoretical considerations
4.2.1 Principles of DMA
4.2.2 Moduli and damping factor
4.2.3 Dynamic mechanical parameters
4.3 Practical considerations
4.3.1 Usage of DMA instruments
4.3.2 Choosing the best geometry
4.3.3 Considerations for each mode of geometry
4.3.4 Static force control
4.3.5 Consideration of applied strain and strain field
4.3.6 Other important factors
4.3.7 The first experiment – what to do?
4.3.8 Thermal scanning experiments
4.3.9 Isothermal experiments
4.3.10 Strain scanning experiments
4.3.11 Frequency scanning experiments
4.3.12 Step-isotherm experiments
4.3.13 Creep – recovery tests
4.3.14 Determination of the glass transition temperature, Tg
4.4 Instrument details and calibration
4.4.1 Instrument drives and transducers
4.5.3 Example of and activation energy calculations using PMMA
4.5.4 Glass transition, Tg, measurements
4.6.3 TMA usage
Appendix: sample geometry constants
5.1 Introduction
5.2 Differential scanning calorimetry
5.2.1 Oxidation studies (OIT test)
5.2.2 Thermal history studies
5.2.3 Cross-linking processes
5.2.4 Investigation of unknowns
5.2.5 Rapid scanning with DSC
5.3 Thermomechanical analysis
5.3.1 Investigation of extrusion defects
5.3.2 Cross-linking
5.3.3 Material identification
5.3.4 Extrusion studies
5.3.5 Fire-retardant mineral insulations
5.4 Thermogravimetric analysis
5.4.1 Practical comments
5.4.2 Investigation of composition
5.4.3 Carbon content
5.4.4 Rapid scanning with TGA
5.5 Combined studies
5.6 Concluding remarks
6.1 Introduction
6.2 Thermogravimetric analysis
6.2.1 Background
6.2.2 Determination of additives
6.2.3 Compositional analysis
6.2.4 Thermal stability determinations
6.2.5 High resolution TGA and modulated TGA
6.2.6 Hyphenated TGA techniques and evolved gas analysis
6.3 Dynamic mechanical analysis
6.3.1 Background
6.3.3 Characterisation of curing and cure state studies
6.3.5 Ageing, degradation and creep studies
6.3.6 Thermal mechanical analysis
6.4 Differential scanning calorimetry
6.4.1 Background
6.4.2 Crystallinity studies and the characterisation of polymer blends
6.4.3 Glass transition and the factors that influence it
6.4.4 Ageing and degradation
6.4.5 Curing and cross-linking
6.4.6 Blowing agents
6.4.8 HyperDSCTM
6.4.9 Microthermal analysis
6.5.1 Dielectric analysis
6.5.2 Differential photocalorimetry (DPC)
6.5.3 Thermally stimulated current (TSC)
6.5.4 Thermal conductivity analysis (TCA)
6.6 Conclusion
Abbreviations
7.1 Biomaterials
7.1.1 Introduction
7.2 Material classes of biomaterials
7.2.1 Metals and alloys
7.2.2 Ceramics and glasses
7.2.3 Polymers
7.2.4 Composites
7.3 The significance of thermal analysis in biomaterials
7.4.3 Porous foams for tissue engineering scaffolds
7.5.2 Plasticisation effect of solvents
7.5.3 Thermal stability and degradation
7.5.4 Setting behaviour of inorganic cements
7.6.1 Bioactive glasses
7.6.2 Thermal stability of bioactive composites
7.7 Summary
8.1 Introduction
8.2 Determining the melting behaviour of crystalline solids
8.2.1 Evaluating the melting point transition
8.3 Polymorphism
8.3.1 Significance of pharmaceutical polymorphism
8.3.3 Characterisation of polymorphs by DSC
8.3.4 Determining polymorphic purity by DSC
8.4 Solvates and hydrates (pseudo-polymorphism)
8.4.1 Factors influencing DSC curves of hydrates and solvates
8.4.2 Types of desolvation/dehydration
8.5 Evolved gas analysis
8.6 Amorphous content
8.6.1 Introduction
8.6.3 Quantification of amorphous content using DSC
8.7 Purity determination using DSC
8.7.1 Types of impurities
8.7.2 DSC purity method
8.7.3 Practical issues and potential interferences
8.9.3 High-sensitivity DSC
Bill MacNaughtan, Imad A. Farhat
9.1 Introduction
9.2 Starch
9.2.1 Starch structure
9.2.2 Order in the granule
9.2.3 The glass transition
9.2.4 Extrusion and expansion
9.2.5 Mechanical properties
9.2.6 Starch retrogradation
9.2.7 Effect of sugars
9.2.8 Lipid–amylose complexes
9.2.9 Multiple amorphous phases: polyamorphism
9.2.10 Foods
9.3 Sugars
9.3.1 Physical properties
9.3.2 Sugar glasses
9.3.3 Sugar crystallisation
9.3.4 Effect of ions on crystallisation
9.3.5 Effect of ions on the glass transition temperature
9.3.6 Ageing
9.3.7 The Maillard reaction
9.3.8 Mechanical properties
9.3.9 Foods
9.4 Fats
9.4.1 Solid/liquid ratio
9.4.2 Phase diagrams
9.4.3 Polymorphic forms and structure
9.4.4 Kinetic information
9.4.5 Non-isothermal methods
9.4.6 DSC at high scanning rates
9.4.7 Mechanical measurements
9.4.9 Foods
9.5 Proteins
9.5.1 Protein denaturation and gelation
9.5.2 Differential scanning microcalorimetry
9.5.3 Aggregation
9.5.4 Glass transition in proteins
9.5.5 Ageing in proteins
9.5.6 Gelatin in a high-sugar environment
9.5.7 Mechanical properties of proteins
9.5.8 Foods
9.5.9 TA applied to other areas
9.5.10 Interactions with polysaccharides and other materials
9.6 Hydrocolloids
9.6.1 Definitions
9.6.2 Structures in solution
9.6.3 Solvent effects
9.6.4 The rheological Tg
9.6.5 Glassy behaviour in hydrocolloid/high-sugar systems
9.6.6 Foods
9.7 Frozen systems
9.7.1 Bound water?
9.7.2 State diagram
9.7.3 Mechanical properties of frozen sugar solutions
9.7.5 Foods
9.7.6 Cryopreservation
9.8 Thermodynamics and reaction rates
9.8.1 Studies on mixing
9.8.2 Isothermal titration calorimetry
9.8.3 Reaction rates
9.8.4 Thermogravimetric analysis
9.8.5 Sample controlled TA
David Furniss, Angela B. Seddon
10.1 Introduction
10.2 Background glass science
10.2.1 Nature of glasses
10.2.2 Crystallisation of glasses
10.2.3 Liquid–liquid phase separation
10.2.4 Viscosity of the supercooled, glass-forming liquid
10.3 Differential thermal analysis
10.3.1 General comments
10.3.2 Experimental issues
10.3.3 DTA case studies
10.4 Differential scanning calorimetry
10.4.1 General comments
10.4.2 Experimental issues
10.4.3 DSC case studies
10.4.4 Modulated Differential scanning calorimetry case studies
10.5 Thermomechanical analysis
10.5.1 General comments
10.5.2 Experimental issues
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Principles and Applications of Thermal Analysis - 1405131713

Principles and Applications of Thermal Analysis - 1405131713

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Published by: Ashwini Kumar on Sep 23, 2010
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