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to Thermal Analysis Techniques and Applications Edited by Michael E. Brown Chemistry Department, Rhodes University, Grahamstown, South Africa KLUWER ACADEMIC PUBLISHERS NEW YORK, BOSTON, DORDRECHT, LONDON, MOSCOW eBook ISBN: 0-306-48404-8 Print ISBN: 1-4020-0472-9 ©2004 Kluwer Academic Publishers New York, Boston, Dordrecht, London, Moscow Print ©2001 Kluwer Academic Publishers Dordrecht All rights reserved No part of this eBook may be reproduced or transmitted in any form or by any means, electronic, mechanical, recording, or otherwise, without written consent from the Publisher Created in the United States of America Visit Kluwer Online at: http://kluweronline. com and Kluwer's eBookstore at: http://ebooks. kluweronline. com CONTENTS Preface to the First Edition, Chapman & Hall, London, 1988 ix About the First Edition of this Book x Preface to the Second Edition xi 1. INTRODUCTION 1. 1 Definition and History 1 1. 2 Thermal Analysis Instruments 4 References 11 2. THERMAL EVENTS 2. 1 Introduction 13 2. 2 The Solid State 13 2. 3 Reactions of Solids 14 2. 4 Decomposition of Solids 15 2. 5 Reaction with the Surrounding Atmosphere 16 2. 6 Solid-Solid Interactions 16 References 17 3. THERMOGRAVIMETRY (TG) Introduction 3. 1 19 3. 2 The Balance 19 3. 3 Heating the Sample 21 3. 4 The Atmosphere 24 3. 5 The Sample 26 3. 6 Temperature Measurement 26 3. 7 Temperature Control 28 Sample Controlled Thermal Analysis (SCTA) 29 3. 8 3. 9 Calibration 36 3. 10 Presentation of TG Data 37 3.
Thermal Analysis and Thermodynamic Properties of Solids, Second Edition covers foundational principles and recent updates in the field, presenting an authoritative overview of theoretical knowledge and practical applications across several fields. Since the first edition of this book was published, large developments have occurred in the theoretical understanding of—and subsequent ability to assess and apply—principles of thermal analysis. Drawing on the knowledge of its expert author, this second edition provides fascinating insight for both new and experienced students, researchers, and industry professionals whose work is influenced or impacted by thermo analysis principles and tools. Part 1 provides a detailed introduction and guide to theoretical aspects of thermal analysis and the related impact of thermodynamics. Key terminology and concepts, the fundamentals of thermophysical examinations, thermostatics, equilibrium background, thermotics, reaction kinetics and models, thermokinetics and the exploitation of fractals are all discussed. Part 2 then goes on to discuss practical applications of this theoretical information to topics such as crystallization kinetics and glass states, thermodynamics in superconductor models, and climate change. - Includes fully updated as well as new chapters on kinetic phase diagrams, thermokinetics in DTA experiments, and crystallization kinetics - Discusses the influence of key derivatives such as thermostatics, thermodynamics, thermotics, and thermokinetics - Helps readers understand and describe reaction kinetics in solids, both in terms of simplified descriptions of the reaction mechanism models and averaged descriptions using fractals
Handbook of Thermal Analysis and Calorimetry, Volume 1: Principles and Practice describes the basic background information common to thermal analysis and calorimetry in general. Thermodynamic and kinetic principles are discussed along with the instrumentation and methodology associated with thermoanalytical and calorimetric techniques. The purpose is to collect the discussion of these general principles and minimize redundancies in the subsequent volumes that are concerned with the applications of these principles and methods. More unique methods, which pertain to specific processes or materials, are covered in later volumes.
The use of thermal and calorimetric methods has shown rapid growth over the last two decades, in an increasingly wide range of applications. In addition, a number of powerful new techniques have been developed. This book supplies a concise and readable account of the principles, experimental apparatus and practical procedures used in thermal analysis and calorimetric methods of analysis. Brief accounts of the basic theory are reinforced with detailed applications of the methods and contemporary developments. Also included is information on standard test methods and manufacturers. Written by acknowledged experts, Principles of Thermal Analysis and Calorimetry is up-to-date, wide-ranging and practical. It will be an important source of information for many levels of readership in a variety of areas, from students and lecturers through to industrial and laboratory staff and consultants.
The wide range of applications of thermal methods of analysis in measuring physical properties, studying chemical reactions and determining the thermal behaviour of samples is of interest to academics and to industry. These applications prompted the writing of this book, in the hope that the descriptions, explanations and examples given would be of help to the analyst and would stimulate the investigation of other thermal techniques. Thermal studies are a fascinating means of examining the samples and the problems brought to us by colleagues, students and clients. If time allows, watching crystals change on a hot-stage microscope, or measuring the properties and changes on a DSC or TG or any thermal instrument can be a rewarding activity, besides providing valuable analytical information. This book started from a series of lectures delivered at Kingston University and at meetings of the Thermal Methods Group of the United Kingdom. The collaboration and information supplied to all the contribu tors by colleagues and instrument manufacturers is most gratefully ack nowledged, as are the valuable contributions made at meetings of the International Confederation for Thermal Analysis and Calorimetry (ICT AC) and at the European Symposia on Thermal Analysis and Calorimetry (ESTAC).
Thermal Analysis: From Introductory Fundamentals to Advanced Applications presents an easy-to-understand introduction to Thermal Analysis (TA) principles alongside in-depth coverage of the wide variety of techniques currently in use across several industries. It covers differential scanning calorimetry (DSC), temperature modulated DSC (TMDSC), differential thermal analysis (DTA), thermogravimetry (TG) or thermogravimetric analysis (TGA), thermomechanical analysis (TMA), differential photo-calorimetry (DPC), dynamic mechanical analysis (DMA), thermodilatometry (TD), dielectric thermal analysis (DEA), thermally-stimulated current (TSC), emanation thermal analysis (ETA), thermoluminescence (TL), fast scanning calorimetry (FSC), and microcalorimetry. Chapters define the various TA techniques, report the Temperature-Modulated DSC (TMDSC) method and its applications, especially its use for studying the thermodynamic properties of polymers and pharmaceuticals, focus on the potential of TA in materials science with applications in chemistry and engineering, demonstrate, in detail, the various applications of TA in food, electronic industries, solid-state reactions, chemistry of polymers and large directing agents, kinetic studies, demonstrate the crystal structure and phase changes occurring upon heating by TA, and the potential of TA in recycling and waste management. - Gives a solid introduction to the scientific principles of TA for those who are new to these techniques or need a deeper understanding - Illustrates concepts with more than 100 schematic and analysis curves, several flow charts, process diagrams and photographs - Contains chapters that cover the user of TA in materials science and crystal structures
This is an expanded and revised second edition, presenting accurate and comprehensive information about our leading thermal scientists to current and future generations. In our globalized world, most researchers in thermal analysis do not know each other in person and are not familiar with each other’s achievements. This volume provides the reader with an up-to-date list of the prominent members in this community. The publication contains only living scientists. The selection is based partly on several decades of the editors' personal professional experience and also partly on the opinion of the Regional Editors of the Journal of Thermal Analysis and Calorimetry.
Thermal Analysis techniques are used in a wide range of disciplines, from pharmacy and foods to polymer science, materials and glasses; in fact any field where changes in sample behaviour are observed under controlled heating or controlled cooling conditions. The wide range of measurements possible provide fundamental information on the material properties of the system under test, so thermal analysis has found increasing use both in basic characterisation of materials and in a wide range of applications in research, development and quality control in industry and academia. Principles and Applications of Thermal Analysis is written by manufacturers and experienced users of thermal techniques. It provides the reader with sound practical instruction on how to use the techniques and gives an up to date account of the principle industrial applications. By covering basic thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) including the new approach of Fast Scanning DSC, together with dynamic mechanical analysis (DMA /TMA) methods, then developing the discussion to encompass industrial applications, the book serves as an ideal introduction to the technology for new users. With a strong focus on practical issues and relating the measurements to the physical behaviour of the materials under test, the book will also serve as an important reference for experienced analysts.
Table of Contents Table of Contents 1 Atoms, small, and large molecules 2 Basics of thermal analysis 3 Dynamics of chemical and phase changes 4 Thermal analysis tools 5 Structure and properties of materials 6 Single component materials 7 Multiple component materials App. A.1 Table of thermal properties of linear macromolecules and related small molecules - the ATHAS data bank App. A.2 Radiation scattering App. A.3 Derivation of the Rayleigh ratio App. A.4 Neural network predictions App. A.5 Legendre transformations, Maxwell relations, linking of entropy and probability, and derivation of (dS/dT) App. A.6 Boltzmann distribution, harmonic vibration, complex numbers, and normal modes App. A.7 Summary of the basic kinetics of chemical reactions App. A.8 The ITS 1990 and the Krypton-86 length standard App. A.9 Development of classical DTA to DSC App. A.10 Examples of DTA and DSC under extreme conditions App. A.11 Description of an online correction of the heat-flow rate App. A.12 Derivation of the heat-flow equations App. A.13 Description of sawtooth-modulation response App. A.14 An introduction to group theory, definitions of configurations and conformations, and a summary of rational and irrational numbers App. A.15 Summary of birefringence and polarizing microscopy App. A.16 Summary of X-ray diffraction and interference effects App. A.17 Optical analog of electron double diffraction to produce Moire patterns.