Thermal Analysis and Calorimetry: Versatile Techniques

✍ Scribed by Auroux A., Damjanović-Vasilić L. (ed.)

• Publisher: Walter de Gruyter
• Year: 2023
• Tongue: English
• Leaves: 412
• Series: De Gruyter STEM
• Category: Library

✦ Synopsis

This book summarizes the application of thermal analysis tools in different research areas. Areas covered include characterization of catalytic materials, plastics and polymers, analysis of salts, minerals and oxides. The reader is provided with an overview of experimental strategy, methodology, usage of complementary thermoanalytical methods and the type of information which could be drawn depending on the research field.
Covers characterization of catalytic materials, plastics and polymers, analysis of salts, minerals, oxides, and energy materials.
Discusses experimental strategy, methodology, and usage of complementary thermoanalytical methods.

✦ Table of Contents

Cover
Half Title
Also of interest
Thermal Analysis and Calorimetry: Versatile Techniques
Copyright
Abstract
Preface
Contents
List of contributors
1. Thermal analysis: a guide through catalyst’s synthesis and reaction process
1.1 Prologue
1.2 Concerning thermal analysis in catalysis
1.2.1 Acknowledgments
1.3 Cu-based catalyst for industrial methanol synthesis
1.3.1 Calcination
1.3.1.1 Cu/Zn hydroxocarbonates as precursors for active catalyst
1.3.1.2 Nature of carbonate-modified oxide, decomposition kinetics
1.3.1.3 Effect of high-temperature carbonate on catalytic methanol synthesis
1.3.2 Activation
1.3.2.1 Effect of calcination temperature on the reduction profile
1.3.2.2 The course of reduction
1.3.2.3 The impact of reduction temperature on catalytic activity
1.3.3 Characterization of metal–support interaction in a Cu-based catalyst
1.3.4 Reaction
1.3.5 Final remarks
1.4 Ni-based catalyst for industrial application
1.4.1 Calcination
1.4.1.1 Decomposition of NiMgAl and NiMg hydroxocarbonates
1.4.2 Activation
1.4.2.1 Reducibility
1.4.2.2 Redox dynamics
1.4.3 Surface characterization
1.4.3.1 Metal dispersion and pulse TA
1.4.4 Reaction studies
1.4.4.1 Coking behavior in dry reforming of methane
1.4.5 Conclusive summary
1.5 In situ perspective
References
2. Contribution of isothermal titration calorimetry to elucidate the mechanism of adsorption from dilute aqueous solutions on solid surfaces: data processing, analysis, and interpretation
2.1 Introduction
2.2 Typical ITC operating principles and implementation of the ITC adsorption experiment
2.2.1 General operating mode
2.2.2 Individual adsorption isotherms and adsorption kinetics
2.2.3 Incremental titration procedure, the resulting thermal effects, and mass balance
2.2.4 Designing ITC adsorption experiment: operating conditions and baseline stability
2.3 Analysis of enthalpy balance in ITC experiments and correlation between dilution and adsorption calorimetry runs
2.3.1 Enthalpy quantities adequate for the implementation of incremental titration model
2.3.2 Enthalpy changes accompanying adsorption from single-solute solutions
2.3.3 Correlation between dilution and adsorption experiments in single-solute systems
2.3.4 Enthalpy changes accompanying adsorption from two-solute solutions
2.3.5 Correlation between dilution and adsorption experiments in two-solute systems
2.4 Possible interpretation of the results of ITC adsorption measurements with a view to improving the understanding of adsorption mechanism
2.4.1 Example of competitive ion adsorption
2.4.2 Example of cooperative ion adsorption from dilute aqueous solutions
2.4.3 Main limitation of ITC technique in adsorption studies
2.5 Concluding remarks
References
3. Thermal analysis and solid-state hydrogen storage: Mg/MgH2 system case study
3.1 Introduction
3.2 Hydrogen storage in magnesium: mechanisms, interests, and limits
3.3 Thermal analysis to perform screening processes: TPD and TGA
3.4 Thermal analysis to study in detail the dehydrogenation properties of MgH2: DSC
3.5 Volumetric techniques to study the hydrogenation of Mg: Sieverts apparatus
3.6 Conclusion
References
4. Using calorimetry to study catalytic surfaces and processes for biomass valorization
4.1 Introduction
4.2 The calorimetry technique
4.2.1 Gas-phase calorimetry and “intrinsic” acidity and basicity
4.2.2 Liquid-phase calorimetry and “effective” acidity and basicity
4.3 Production of 5-HMF from biomass: case studies
4.3.1 Fructose dehydration
4.3.2 Hydrolysis of cellobiose
4.4 Guerbet reaction of methanol and ethanol to higher R-OH: a case study
4.5 Acrolein production from biomass: case studies
4.5.1 Glycerol dehydration
4.5.2 Oxidative coupling of alcohols
4.6 Conclusions
References
5. The correspondence of calorimetric studies with DFT simulations in heterogeneous catalysis
5.1 DFT Studies for prediction of adsorption energetics and activated complexes
5.1.1 Exchange correlation functionals
5.1.1.1 Local spin-density approximation (LSDA)
5.1.1.2 Generalized gradient approximation (GGA)
5.1.1.3 Meta-GGA
5.1.1.4 Hybrid GGA/meta-GGA
5.1.1.5 Van der Waals interactions
5.1.1.6 Random phase approximation (RPA)
5.1.2 Databases for benchmarking
5.1.3 Other aspects to consider
5.2 Adsorption microcalorimetry in catalysis
5.3 Benchmarking DFT methods through comparisons with heat of adsorption data
5.3.1 CO adsorption on metal surfaces
5.3.2 Benzene adsorption on metal surfaces
5.3.3 Acid site characterization in zeolites
5.3.4 Energetics of the active site in real catalysts at two operating conditions
5.4 Concluding remarks
References
6. Major concern regarding thermophysical parameters’ measurement techniques of thermochemical storage materials
6.1 Introduction
6.2 Principles of sorption-based THS
6.3 Closed and open system for sorption-based THS
6.4 Sorption storage materials
6.5 Thermophysical material characterization
6.5.1 Enthalpy of hydration reaction-ΔHh
6.5.2 Specific heat capacity, Cp
6.5.3 Thermal conductivity, λ
6.5.3.1 Steady-state methods
6.5.3.1.1 Guarded hot plate method-GHP
6.5.3.1.2 Method known as radial flow or coaxial cylinder cell
6.5.3.2 Transient methods
6.5.3.2.1 Hot-wire method
6.5.3.2.2 Transient plane source (TPS) method “hot disk”
6.5.3.2.3 Laser flash method
6.5.3.3 Selection of a method
6.6 General overview and summary
References
7. Calorimetric methods for key properties in refrigeration cycles
7.1 Cold production
7.1.1 Electric heat pump (EHP)
7.1.2 Absorption heat pump (AHP)
7.1.3 Working fluids
7.2 Thermodynamic properties and calorimetric measurements for refrigeration systems
7.2.1 Measurement of heat of vaporization and phase diagrams
7.2.2 Heat capacity measurements
7.2.2.1 Adiabatic calorimeters
7.2.2.2 Differential scanning calorimetry
References
8. Calorimetry and thermal analysis for the study of polymer properties
8.1 Introduction
8.2 Polymer classification
8.3 Calorimetry for the study of polymers
8.3.1 Differential scanning calorimetry
8.3.1.1 Examples
8.3.2 Calvet calorimetry
8.3.2.1 Example
8.4 TGA and polymers
8.4.1 Principle
8.4.1.1 Examples of TGA analyses
8.5 Thermomechanical analyses (TMA) for the study of polymers
8.5.1 Principle
8.5.1.1 Examples of TMA analyses
8.6 Evolved gas analysis, to know more about the polymer decomposition mechanism
8.6.1 Principle
8.6.2 Techniques used in EGA
8.6.2.1 TGA-MS coupling
8.6.2.2 TGA-FTIR coupling
8.6.2.3 TGA-GC-MS coupling
8.6.2.4 TGA–micro-GC-MS coupling (TGA-μGC-MS)
8.6.3 EGA conclusion
8.7 Conclusion
References
9. Role of calorimetry in clathrate hydrate research
9.1 Introduction
9.1.1 Introduction to gas hydrates and their calorimetric analysis
9.1.2 Introduction to differential scanning calorimetry
9.1.3 Calorimetry-based key measurements
9.1.4 Differential scanning calorimetry setup
9.1.5 Key influencing factors
9.2 Calorimetric assessment of clathrate hydrate thermodynamics
9.3 Assessment of hydrate inhibitors using calorimetric methods
9.4 Quantification of hydrate-in-oil stability using DSC
9.5 Role of calorimetry in hydrate structure elucidation
9.5.1 How to distinguish the different hydrate structures using DSC thermograms
9.5.2 CH4–CO2 replacement process using a differential scanning calorimeter
9.6 Thermal properties of gas hydrates
9.7 Recent research trend calorimetry applications
9.8 Challenges and recent advancements in calorimetry
References
10. Thermal methods as a tool for studying cultural heritage
10.1 Introduction
10.2 Characterization of materials that constitute ancient artworks by thermal methods
10.2.1 Mortars
10.2.2 Stones
10.2.3 Ceramics
10.2.4 Leathers and parchments
10.2.5 Wood
10.2.6 Paper
10.2.7 Painting materials
10.3 Conclusion
References
11. The application of calorimetry and thermal methods of analysis in the investigation of food
11.1 Introduction
11.2 Temperature-dependent properties of foods
11.3 Experimental techniques available to monitor temperature-dependent properties of food: the acquired data
11.4 Thermal analysis of food components
11.4.1 Thermal analysis of proteins
11.4.2 Thermal analysis of fats and oils
11.4.3 Thermal analysis of carbohydrates
11.5 Interactions between food components
11.6 Complementary application of thermal methods of analysis with other techniques
11.6.1 Case study 1: chocolate
11.6.2 Case study 2: encapsulation
11.7 The role of thermal methods in the newest food technology trends
11.8 Conclusions
References
Index