Elsevier S & T

Handbook of Thermal Analysis and Calorimetry: Recent Advances, Techniques and Applications

Brown, Michael E.

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Table of contents
  • Cover
  • Table of Contentsvii
  • Forewordv
  • Prefacevi
  • Contributorsxx
  • CHAPTER 1. INTRODUCTION TO RECENT ADVANCES, TECHNIQUES AND APPLICATIONS1
  • 1. THE HANDBOOK OF THERMAL ANALYSIS AND CALORIMETRY1
  • 2. THE LITERATURE OF THERMAL ANALYSIS AND CALORIMETRY2
  • 2.1. Books2
  • 2.2. Major conferences and their proceedings3
  • 2.3. Websites5
  • 3. NOMENCLATURE6
  • 4. RECENT ADVANCES IN TECHNIQUES6
  • 4.1. Micro-Thermal Analysis6
  • 4.2. Pulsed thermal analysis7
  • 4.3. Fast scanning calorimetry7
  • 5. ADVANCES IN APPLICATIONS7
  • 5.1. Quartz-crystal microbalances7
  • 5.2. Electrical techniques8
  • 5.3. Heating-stage spectroscopy8
  • 5.4. Rheology8
  • 5.5. Catalysis9
  • 5.6. Nanoparticles9
  • 6. KINETICS9
  • 7. ADDITIONAL TOPICS10
  • 7.1. Thermochemistry10
  • 7.2. Coordination compounds and inorganics10
  • 7.3. Thermophysical properties11
  • 7.4. Polymorphism11
  • 7.5. Medical applications11
  • 7.6. Dental materials12
  • 8. QUALITY CONTROL12
  • CHAPTER 2. DEVELOPMENTS IN NOMENCLATURE13
  • 1. INTRODUCTION13
  • 2. 2006 ICTAC NOMENCLATURE OF THERMAL ANALYSIS14
  • 2.1. Scope14
  • 2.2. Intent15
  • 2.3. Definition of the field of Thermal Analysis (TA)15
  • 2.4. Techniques15
  • 2.5. Terminology and Glossary16
  • 2.6. Experimental conditions22
  • 2.7. Symbols used specifically in Thermal Analysis22
  • 2.8. Overview and historical matters23
  • 2.9. Recent Members of the ICTAC Nomenclature Committee24
  • 3. COMMENTS ON THE 2006 ICTAC NOMENCLATURE OF THERMAL ANALYSIS24
  • 4. A CONVENIENT NOMENCLATURE FOR CALORIMETERS28
  • 4.1. Basic representation, criteria and categories28
  • 4.2. "Passive" adiabatic calorimeters30
  • 4.3. "Active" adiabatic calorimeters32
  • 4.4. "Passive" diathermal calorimeters34
  • 4.5. "Active" diathermal calorimeters35
  • 5. OTHER POSSIBLE NOMENCLATURES FOR CALORIMETERS37
  • 5.1. Nomenclature proposed by Swietoslawski in 193337
  • 5.2. Nomenclature proposed by Calvet and Prat in 195637
  • 5.3. Nomenclature proposed by Evans in 196939
  • 5.4. Nomenclature proposed by Skinner in 196939
  • 5.5. Nomenclature proposed by Rouquerol and Laffitte in 197240
  • 5.6. Nomenclature proposed by Hemminger and Höhne in 198441
  • 5.7. Nomenclature proposed by Rouquerol and Zielenkiewicz in 198644
  • 5.8. Nomenclature proposed by Tachoire and Médard in 199444
  • 5.9. Nomenclature proposed by Wadsö in 199745
  • 5.10. Nomenclature proposed by Hemminger and Särge in 199946
  • 5.11. Nomenclature proposed by Hansen in 200147
  • 5.12. Nomenclature proposed by Matsuo in 200448
  • 5.13. Nomenclature proposed by Zielenkiewicz in 200450
  • 6. CONCLUSIONS51
  • 7. REFERENCES52
  • CHAPTER 3. MICRO-THERMAL ANALYSIS AND RELATED TECHNIQUES55
  • 1. INTRODUCTION55
  • 2. SCANNING THERMAL MICROSCOPY (STHM)57
  • 2.1. Introduction57
  • 2.2. Instrumentation for SThM58
  • 2.3. Probe design59
  • 2.4. Quantitative SThM61
  • 2.5. Other SThM techniques66
  • 3. LOCALISED THERMAL ANALYSIS67
  • 3.1. Principles67
  • 3.2. Calibration68
  • 3.3. Features69
  • 3.4. Terminology71
  • 3.5. Applications71
  • 4. LOCALISED CHEMICAL ANALYSIS78
  • 4.1. Introduction78
  • 4.2. Localised evolved gas analysis78
  • 4.3. Near-field photothermal spectroscopy82
  • 4.4. Therrnally-assisted rnicro-sampling83
  • 5. CONCLUSIONS84
  • 6. REFERENCES84
  • CHAPTER 4. PULSE THERMAL ANALYSIS93
  • 1. INTRODUCTION93
  • 2. EXPERIMENTAL94
  • 3. CALIBRATION OF SPECTROMETRIC SIGNALS IN HYPHENATED THERMOANALYTICAL TECHNIQUES95
  • 3.1. Calibration of gases95
  • 3.2. Verification of the calibration98
  • 3.3. Calibration of liquids99
  • 4. QUANTIFICATION OF THE SPECTROMETRIC SIGNALS IN A TA-MS-FTIR SYSTEM101
  • 4.1. Determination of the intrinsic fragmentation in a TA-MS system101
  • 4.2. Application of PulseTA® for quantification of gas-solid reactions104
  • 5. INJECTION OF A GAS WHICH REACTS WITH THE SOLID112
  • 5.1. Investigations of the reduction and oxidation of solids112
  • 5.2. Investigation of the redox behaviour of solids: reduction and re-oxidation of CeO2116
  • 5.3. Investigation of gas-solid reactions118
  • 5.4. Miscellaneous applications123
  • 6. INJECTION OF A GAS WHICH ADSORBS ON THE SOLID124
  • 6.1. Adsorption of ammonia on HZMS-5 zeolite124
  • 6.2 Investigation of the adsorption and desorption of NH3 on a titania-silica aerogel125
  • 6.3. Investigation of adsorption combined with gas-solid reaction126
  • 6.4. Miscellaneous applications129
  • 7. CONCLUSIONS129
  • 8. REFERENCES130
  • CHAPTER 5. THE QUARTZ CRYSTAL MICROBALANCE133
  • 1. HIGH SENSITIVITY BALANCES: THEIR ROLE IN THERMAL ANALYSIS AND CALORIMETRY133
  • 2. EARLY HISTORY OF THE QUARTZ CRYSTAL MICROBALANCE134
  • 3. THE LITERATURE OF THERMAL ANALYSIS AND OF THE QUARTZ CRYSTAL MICROBALANCE135
  • 4. PRINCIPLES OF OPERATION OF THE QUARTZ CRYSTAL MICROBALANCE (QCM)142
  • 5. DETECTION ELECTRONICS147
  • 5.1. Simple QCM driving circuits147
  • 5.2. Frequency and damping measurements148
  • 5.3. Impedance analysis148
  • 6. IS THE TRANSVERSE SHEAR MODE RESONATOR A TRUE MICROBALANCE?148
  • 7. PRACTICAL DETAILS150
  • 7.1. Calibration150
  • 7.2. Comparison of gravimetric and Sauerbrey masses151
  • 7.3. Sample preparation152
  • 8. CHEMICAL AND BIOLOGICAL APPLICATIONS OF THE QCM152
  • 8.1. Film-thickness monitors in vacuum deposition152
  • 8.2. The metal/solution interface in electrochemical cells153
  • 8.3. Faraday Society Discussion No. 107, 1997154
  • 8.4. Determination of shear and loss modulus at QCM frequencies154
  • 8.5. Chemical sensors and biosensors156
  • 8.6. Biological surface science158
  • 9. SENSORS159
  • 9.1. Acoustic microsensors – the challenge behind microgravimetry159
  • 9.2. Piezoelectric sensors159
  • 10. THE QUARTZ CRYSTAL MICROBALANCE/HEAT CONDUCTION CALORIMETER161
  • 10.1. Introduction161
  • 10.2. Beginnings of QCM/HCC161
  • 10.3. Development of QCM/HCC163
  • 10.4. Biological applications164
  • 10.5. The Masscal Scientific Instruments G1 Microbalance/Calorimeter164
  • 10.6. Recent applications165
  • 10.7. Conclusion165
  • 11. REFERENCES166
  • CHAPTER 6. HEATING STAGE SPECTROSCOPY: INFRARED, RAMAN, ENERGY DISPERSIVE X-RAY AND X-RAY PHOTOELECT171
  • 1. INFRARED EMISSION SPECTROSCOPY171
  • 1.1. Introduction171
  • 1.2. The theory behind infrared emission spectroscopy (IES)173
  • 1.3. Infrared emission spectroscopy of alunite179
  • 2. HEATING STAGE RAMAN SPECTROSCOPY182
  • 2.1 Heating stage Raman spectroscopy of weddellite186
  • 3. THERMAL STUDIES OF MATERIALS USING HEATING AND COOLING STAGE SCANNING ELECTRON MICROSCOPY AND ENE188
  • 3.1. Apparatus188
  • 3.2. Thermal decomposition of weddelite by heating stage SEM and infrared emission spectroscopy (IES191
  • 3.3. Sublimation of urea CH4N2O196
  • 3.4. Wetting/drying of montmorillonite198
  • 4. HEATING STAGE PHOTOELECTRON SPECTROSCOPY (XPS)200
  • 4.1. Dehydration of calcium oxalate monohydrate CaC2O4.H2O201
  • 4.2. Calcination of titania/PVA expanded hectorite202
  • 5. CONCLUSIONS206
  • 6. ACKNOWLEDGEMENTS206
  • 7. REFERENCES206
  • CHAPTER 7. ELECTRIC TECHNIQUES209
  • 1. INTRODUCTION209
  • 1.1. Dielectric materials in the presence of static electric fields209
  • 1.2. Application of alternating electric fields211
  • 2. MEASUREMENT TECHNIQUES216
  • 2.1. Introduction216
  • 2.2. Equivalent circuits217
  • 2.3. Time-domain measurements219
  • 2.4. Cells220
  • 2.5. Temperature calibration in dielectric and electrical measurements222
  • 3. DIELECTRIC SPECTROSCOPY IN MODEL SYSTEMS AND ASSIGNMENT OF MOLECULAR MOTIONS224
  • 3.1 Sub-glass mobility225
  • 3.2. α - Relaxation231
  • 3.3. Crossover region235
  • 3.4. Low frequency processes240
  • 3.5. Dielectric response in semi-crystalline polymers247
  • 4. THERMALLY STIMULATED DEPOLARIZATION CURRENTS253
  • 5. CONCLUSIONS259
  • 6. REFERENCES260
  • CHAPTER 8. BENEFITS AND POTENTIALS OF HIGH PERFORMANCE DIFFERENTIAL SCANNING CALORIMETRY (HPer DSC)269
  • 1. INTRODUCTION269
  • 2. MAJOR CHALLENGES270
  • 2.1. Introduction270
  • 2.2. Measuring under realistic conditions271
  • 2.3. The study of metastability and reorganization271
  • 3. HIGH-SPEED CALORIMETRY276
  • 3.1. Instrumental aspects276
  • 3.2. Temperature calibration277
  • 3.3. Constancy of the scan rate282
  • 3.4. Linking experiment with practice and processing284
  • 3.5. Quantitative measurements291
  • 3.6. Higher sensitivity; working on minute amounts of material293
  • 4. CONCLUSIONS295
  • 5. REFERENCES295
  • CHAPTER 9. DYNAMIC PULSE CALORIMETRY – THERMOPHYSICAL PROPERTIES OF SOLID AND LIQUID METALS AND AL299
  • 1. INTRODUCTION - THERMOPHYSICAL PROPERTIES299
  • 2. DYNAMIC PULSE CALORIMETRY (PULSE-HEATING)301
  • 2.1. Historical development and brief description of pulse-heating301
  • 2.2. Classification of pulse-heating systems and existing systems302
  • 3. EXPERIMENTAL DESCRIPTION304
  • 3.1. General information about pulse-heating304
  • 3.2. Experiment - Basic electrical quantities308
  • 3.3. Experiment – Derived thermophysical properties310
  • 3.4. Experiment - Levitation324
  • 4. EXPERIMENTAL DATA - IRIDIUM325
  • 5. RECENTLY DEVELOPED (SPECIAL) APPLICATIONS OF PULSE CALORIMETRY329
  • 5.1. Extended temperature range by a pulse-calorimeter/DSC combination329
  • 5.2. Mechanical properties with a Kolsky bar apparatus330
  • 5.3. Pulse-heating/ laser flash combination331
  • 5.4. Pulse-heating microcalorimetry332
  • 6. UNCERTAINTIES333
  • 6. FURTHER READING333
  • 7. CONCLUSIONS334
  • 8. ACKNOWLEDGEMENTS334
  • 9. REFERENCES335
  • CHAPTER 10. SURFACE PROPERTIES OF NANOPARTICLES343
  • 1. INTRODUCTION343
  • 1.1. Nanotechnology and nanostructures343
  • 1.2. Total (energetic and structural) heterogeneity of surfaces345
  • 1.3. Fractal dimensions of nanoparticles348
  • 2. PHYSICOCHEMICAL PROPERTIES OF SELECTED NANOMATERIALS349
  • 2.1. Carbon nanotubes349
  • 2.2. Montmorillonites349
  • 2.3. Zeolites350
  • 2.4. Superconductor materials350
  • 3. TECHNIQUES USED351
  • 3.1. Q-TG thermogravimetry351
  • 3.2. Surface adsorption356
  • 3.3. Porosimetry356
  • 3.4. Calculation of fractal dimensions from sorptometry and porosimetry data357
  • 3.5. Atomic force microscopy, (AFM), Scanning electron microscopy (SEM) and Energy dispersive X-ray358
  • 4. EXAMPLES OF STUDIES ON SELECTED MATERIALS359
  • 4.1. Carbon nanotubes359
  • 4.2. Montmorillonites370
  • 4.3. Aluminas371
  • 4.4. Fractal dimensions381
  • 5. SUMMARY382
  • 6. REFERENCES384
  • CHAPTER 11. HETEROGENEOUS CATALYSIS ON SOLIDS387
  • 1. INTRODUCTION387
  • 2. EXPERIMENTAL388
  • 2.1. Some limitations of the technique for characterizing catalytic sites394
  • 2.2. Probe molecules most commonly used to characterize catalytic surfaces396
  • 2.3. The role and the influence of the probe molecule in determining adsorption heats398
  • 3. ACID-BASE PROPERTIES OF CATALYST SURFACES401
  • 3.1. Zeolites and related materials401
  • 3.2. Bulk, doped, supported and mixed oxides408
  • 4. REDOX PROPERTIES OF CATALYST SURFACES421
  • 4.1. Metals and supported metals421
  • 4.2. Oxides and supported oxides424
  • 5. CORRELATION WITH CATALYTIC ACTIVITY426
  • 6. CONCLUSIONS430
  • 7. REFERENCES431
  • CHAPTER 12. COORDINATION COMPOUNDS AND INORGANICS439
  • 1. INTRODUCTION439
  • 2. REVIEWS440
  • 3. USE OF COORDINATION COMPOUNDS AND INORGANICS TO DEVELOP NEW METHODS441
  • 4. INORGANICS445
  • 4.1. Alloys445
  • 4.2. Arsenates449
  • 4.3. Borates450
  • 4.4. Carbonates451
  • 4.5. Chromates453
  • 4.6. Iodides453
  • 4.7. Nitrates and Nitrites454
  • 4.8. Oxalates456
  • 4.9. Oxides460
  • 4.10. Perchlorates463
  • 4.11. Phosphates464
  • 4.12. Stannates465
  • 4.13. Sulfides, Sulfites and Sulfates466
  • 5. METAL-ORGANIC FRAMEWORKS: COORDINATION POLYMERS469
  • 5.1. Introduction469
  • 5.2. Bismuth469
  • 5.3. Cadmium469
  • 5.4. Cobalt470
  • 5.5. Copper472
  • 5.6. Iron477
  • 5.7. Lanthanides478
  • 5.8. Lead482
  • 5.9. Lithium483
  • 5.10. Magnesium484
  • 5.11. Manganese485
  • 5.12. Nickel486
  • 5.13. Palladium488
  • 5.14. Silver488
  • 5.15. Sodium490
  • 5.16. Strontium490
  • 5.17. Zinc491
  • 6. REFERENCES493
  • CHAPTER 13. ISOCONVERSIONAL KINETICS503
  • 1. INTRODUCTION503
  • 2. ISOCONVERSIONAL METHODS504
  • 3. CONCEPT OF VARIABLE ACTIVATION ENERGY508
  • 4. KINETICS OF PHYSICAL PROCESSES512
  • 4.1. Crystallization512
  • 4.2. Melt and glass crystallization of polymers516
  • 4.3. Second-order transitions518
  • 4.4. Glass transition519
  • 5. KINETICS OF CHEMICAL PROCESSES522
  • 5.1. Reversible decompositions522
  • 5.2. Thermal and thermo-oxidative degradation of polymers525
  • 5.3. Crosslinking526
  • 6. ISOCONVERSIONAL METHODS AND THE KINETIC TRIPLET529
  • 6.1. Is it really needed?529
  • 6.2. Isoconversional kinetic predictions529
  • 6.3. Evaluating the pre-exponential factor and the reaction model532
  • 7. CONCLUSIONS534
  • 8. REFERENCES535
  • CHAPTER 14. THERMOCHEMISTRY539
  • 1. INTRODUCTION539
  • 1.1. The objectives of thermochemistry539
  • 1.2. Short historical introduction541
  • 2. EXPERIMENTAL DETERMINATION OF THE ENTHALPIES OF FORMATION OF ORGANIC COMPOUNDS542
  • 2.1. Introduction542
  • 2.2. Combustion calorimetry542
  • 2.3. Reaction calorimetry550
  • 2.4. Thermochemistry of phase changes551
  • 2.5. Additional techniques554
  • 3. REFERENCE MATERIALS557
  • 4. THERMOCHEMICAL DATA BASES FOR ORGANIC COMPOUNDS558
  • 5. RECENT DEVELOPMENTS IN EXPERIMENTAL TECHNIQUES559
  • 5.1. Combustion calorimetry559
  • 5.2. Enthalpies of sublimation and vaporization560
  • 6. COMPUTATIONAL THERMOCHEMISTRY561
  • 7. THERMOCHEMISTRY AS A POWERFUL TOOL TO SOLVE ACTUAL CHEMICAL PROBLEMS562
  • 7.1. Thermochemistry of cyclobutadiene: Enthalpy of formation, ring strain, and anti-aromaticity562
  • 7.2. Thermochemistry of cubane and cuneane563
  • 7.3. Enthalpy of formation of Buckminsterfullerene, C60563
  • 7.4. Steric, estereolectronic and electrostatic interactions in oxanes, thianes and sulfone and sulf564
  • 7.5. Keto-enol tautomerism and the enthalpy of mixing between tautomers of acetylacetone565
  • 7.6. Radical generation by using organometallic complexes of Group 6 metals566
  • 7.7. Application to biochemical systems566
  • 7.8. Thermochemistry of reactions in gas phase for compounds with important implications as catalyst566
  • 8. CONCLUSIONS567
  • 9. REFERENCES567
  • CHAPTER 15. THERMAL ANALYSIS AND RHEOLOGY579
  • 1. INTRODUCTION579
  • 2. PARAFFIN WAXES580
  • 3. EXPERIMENTAL TECHNIQUES581
  • 3.1. Introduction581
  • 3.2. Differential scanning calorimetry (DSC)582
  • 3.3. Thermomicroscopy and rheology584
  • 4. APPLICATIONS584
  • 5. CONCLUSIONS595
  • 6. REFERENCES595
  • CHAPTER 16. POLYMORPHISM597
  • 1. INTRODUCTION597
  • 2. RECENT DEVELOPMENTS IN POLYMORPHIC RESEARCH599
  • 2.1. Introduction599
  • 3. THERMAL ANALYSIS IN STUDIES OF CRYSTAL POLYMORPHISM603
  • 3.1. Introduction603
  • 4. RECENT STUDIES611
  • 4.1. Characterization of polymorphs and polymorphic transformations611
  • 4.2. Characterization of solvates and desolvation processes621
  • 5. CONCLUSIONS626
  • 6. ACKNOWLEDGEMENTS626
  • 7. REFERENCES626
  • CHAPTER 17. DENTAL MATERIALS631
  • 1. INTRODUCTION631
  • 2. NICKEL-TITANIUM ALLOYS IN DENTISTRY631
  • 2.1. Metallurgy background631
  • 2.2. Nickel-titanium endodontic instruments632
  • 2.3. Nickel-titanium orthodontic wires641
  • 3. DENTAL POLYMER MATERIALS647
  • 3.1. Silicone maxillofacial materials647
  • 3.2. Elastomeric impression materials650
  • 3.3. Orthodontic elastomeric modules654
  • 3.4. Resin composites and other dental polymers656
  • 4. ACKNOWLEDGMENTS658
  • 5. REFERENCES658
  • CHAPTER 18. MEDICAL APPLICATIONS OF THERMAL METHODS663
  • 1. INTRODUCTION663
  • 2. APPLICATION TO PENETRATION OF DRUGS INTO THE SKIN664
  • 2.1. Introduction664
  • 2.2. Thermoanalytical techniques and the skin665
  • 2.3. Thermoanalytical techniques and drug penetration (penetration enhancers) into the skin668
  • 3. APPLICATION TO DRUG DELIVERY675
  • 3.1. Introduction675
  • 3.2. Thermoanalytical techniques used in drug delivery675
  • 4. APPLICATION TO IMPLANTS677
  • 4.1. Introduction677
  • 4.2. Thermoanalytical techniques used in implants677
  • 5. APPLICATIONS TO PROSTHETICS685
  • 5.1. Introduction685
  • 5.2. Bioprostheses used in heart valves685
  • 5.3. Bioprostheses used in aortic valves686
  • 6. MISCELLANEOUS APPLICATIONS687
  • 6.1. DSC studies on albumins687
  • 6.2. DSC studies on the human intervertebral disc688
  • 6.3. DSC studies of human skin from patients with diabetes mellitus (DM)689
  • 6.4. DSC studies on cartilage destruction by septic arthritis689
  • 6.5. DSC studies on the effect of tetracaine on erythrocyte membranes689
  • 6.6. DSC studies on modified poly(urethaneurea) blood sacs690
  • 7. CONCLUSIONS690
  • 8. REFERENCES691
  • CHAPTER 19. QUALITY CONTROL695
  • 1. INTRODUCTION695
  • 2. GENERAL CONSIDERATIONS696
  • 3. POLYMERS698
  • 4. ORGANIC CHEMICALS704
  • 5. PHARMACEUTICALS709
  • 6. FOODS715
  • 7. INORGANIC CHEMICALS722
  • 8. METALS724
  • 9. OTHER REFERENCES728
  • 10. FUTURE OPPORTUNITIES729
  • 11. REFERENCES729
  • INDEX733
Book details
  • Vendor Elsevier S & T
  • SKU 9780444531230
  • ISBN-13 9780080556314
  • Author Brown, Michael E.
  • Category Science
  • Subject Physical & Theoretical

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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