Handbook of Differential Scanning Calorimetry

Techniques, Instrumentation, Inorganic, Organic and Pharmaceutical Substances

1st Edition - February 22, 2023
Imprint: Butterworth-Heinemann
Editors: Joseph D Menczel, Janusz Grebowicz
Language: English
Hardback ISBN:
9 7 8 - 0 - 1 2 - 8 1 1 3 4 7 - 9
eBook ISBN:
9 7 8 - 0 - 1 2 - 8 1 1 3 4 8 - 6

Differential scanning calorimetry (DSC) is the most important thermal analysis technique used today and the most common thermal analysis instrument found in chemical ch… Read more

Handbook of Differential Scanning Calorimetry

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Differential scanning calorimetry (DSC) is the most important thermal analysis technique used today and the most common thermal analysis instrument found in chemical characterization laboratories. DSC has become an everyday tool in characterization laboratories, but many researchers using this technique have a limited understanding of the true breadth of its capabilities. Up to now, there has been no book that would describe the application of DSC in all the various areas of materials chemistry. The Handbook of Differential Scanning Calorimetry has been written to fill that void. This book is designed to summarize the knowledge of differential scanning calorimetry so that materials researchers and application chemists are given both a better understanding of techniques , as well as a review of the full scope of its capabilities. It also discusses how to properly interpret the DSC thermograms data obtained. Included in this work is the most up-to-date information written by some of the leaders in the field. It is written not only to help users get the most out of their equipment, After reading this book, people in all chemical and biological areas will have a broad overview of this measuring technique, and will be able to utilize this analytical technique more efficiently.

Cover image
Title page
Table of Contents
Copyright
Dedication
Contributors
Preface
Chapter 1: Fundamentals of DSC
Abstract
1.1: Introduction
1.2: Overview of DSC
1.3: Elements of Thermodynamics in Differential Scanning Calorimetry
1.4: PerkinElmer’s Power Compensation DSC
1.5: Heat-Flux DSC
1.6: Tian-Calvet Calorimeters
1.7: Modulated Temperature DSC
1.8: Fast Scanning Calorimetry
1.9: Photocalorimetry
1.10: High Temperature DSC
1.11: Calibration of DSCs
1.12: Measurement of Heat Capacity by DSC
1.13: Thermal Transitions in DSC
1.14: Baseline
1.15: Accessories for DSC Measurements
References
Further reading
Chapter 2: The Theory of Modulated Temperature Differential Scanning Calorimetry
Abstract
Acknowledgements
2.1: Introduction
2.2: Notes on Heat Capacity and the Deconvolution Procedure
2.3: Chemical Reactions
2.4: The Phase Lag and Kinetic Effects
2.5: Notes on Nomenclature
2.6: Notes on Correcting for Baseline Deviations
2.7: Notes on Selecting Experimental Parameters
2.8: Notes on Calibration
2.9: Crystallization Behaviour (Without Rearrangement)
2.10: Glass Transitions
2.11: Melting (With Rearrangement)
2.12: Modulation Functions Other Than Sinusoidal
2.13: Overview
References
Further reading
Chapter 3: Chip-Based Fast Scanning Calorimetry
Abstract
Acknowledgments
3.1: Preamble
3.2: Chips and Sensors for Fast Scanning Calorimetry
3.3: Ultra-Fast Scanning Calorimetry
References
Chapter 4: DSC of Inorganic Materials
Abstract
4.1: Introduction
4.2: Principles of Application of DSC to Inorganic Compounds and Elements
4.3: Experimental Conditions in DSC Measurements
4.4: Application of DSC to Elements and Alloys
4.5: Application of DSC to Oxides and Sulfides
4.6: Application of DSC to Inorganic Salts
References
Chapter 5: DSC of Low Molecular Mass Organic Materials and Pharmaceuticals
Abstract
5.1: Introduction
5.2: Purity Evaluation
5.3: Polymorphism
5.4: Compatibility of Tablet Ingredients
5.5: Chemical Kinetics for Characterization of Thermal Stability and Shelf Life of APIs
5.6: Thermal Behavior and Thermal Stability
5.7: Thermal and Thermooxidative Degradation
5.8: Conclusions
References
Chapter 6: Simultaneous DSC Techniques
Abstract
6.1: Introduction
6.2: Commercial Simultaneous Thermal Analyzers
6.3: Simultaneous DSC/DTA-TGA Measurements
6.4: Simultaneous DSC-Electromagnetic Radiation Techniques
6.5: DSC-DEA
6.6: DSC-TMA
6.7: DSC-Rheology (Rheo-DSC)
6.8: Conclusions
References
Chapter 7: Instrumentation
Abstract
7.1: Introduction
7.2: DSC Instruments of PerkinElmer
7.3: DSCs of TA Instruments
7.4: DSCs of Mettler-Toledo
7.5: DSC Instruments of Netzsch
7.6: DSCs of Hitachi High-Tech Science
7.7: DSC Instruments of Setaram
7.8: Other Manufacturers of DSCs
7.9: High Temperature DSC Instruments
7.10: Differential Photocalorimetry Instrumentation
7.11: Fast Scanning Calorimeters
7.12: Simultaneous Thermal Analyzers
References
Index

Joseph D Menczel

Dr. Menczel is a recognized expert in thermal analysis of polymers with some thirty years of industrial and academic experience. He has researched more than 120 polymeric systems in which he studied calibration of DSCs, glass transition, nucleation, crystallization, melting, stability, mechanical and micromechanical properties of polymers, and polymer-water interactions. Dr. Menczel holds six patents and is the author of seventy scholarly papers. He is the author of two chapters in the book Thermal Characterization of Polymeric Materials. Dr. Menczel is an elected NATAS fellow and was the 2010 recipient of the Mettler-Toledo Award in Thermal Analysis.

Affiliations and expertise

Former president, North American Thermal Analysis Society

Janusz Grebowicz

Dr. Grebowicz is a Professor of Chemistry and Physics at the University of Houston-Downtown and a 2014/15 Fulbright Scholar at AGH UST. His areas of expertise are thermal analysis, polymer physical chemistry, phase structure and phase transitions in materials, such as low molecular weight chemicals, polymers and geological materials. He has several significant contributions to science including: design of first ever schematic of all phases and mesophases (with his recognition of new mesophase: conformationally disordered crystals - Condis Crystals), recognition of Rigid Amorphous phase and first ever demonstration of capillary breakup of liquid threads in molten polymer systems - polymer blends (high viscosity). He has authored over 70 papers in these areas. A native of Poland, he received his MS degree in physics from the University of Łódź. His MS project was on polymer physics: development of experimental methods of characterization morphology of semi-crystalline polymers. Soon after, he was appointed a researcher at the Center of Molecular and Macromolecular Studies, Polish Academy of Sciences. There he received his PhD in research on polymer blends followed by a series of post-doctoral studies at Rensselaer Polytechnic Institute, Max Planck Institute (Mainz, Germany), and the University of Massachusetts, Amherst. He became a world-class specialist in thermal analysis, as recognized by his colleagues in the field. For over a decade he worked for Shell Oil, Westhollow Technology Center in Houston, as the head of the Thermal Analysis laboratory (global reach).

Affiliations and expertise

Professor of Chemistry and Physics at the University of Houston-Downtown and a 2014/15 Fulbright Scholar at AGH UST

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