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).

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 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.

Thermal analysis comprises a group of techniques used to determine the physical or chemical properties of a substance as it is heated, cooled, or held at constant temperature. It is particularly important for polymer characterization, but also has major application in analysis of pharmaceuticals and foodstuffs. This comprehensive handbook presents practical and theoretical aspects of the key techniques of DSC, TGA, TMA, DMA, and related methods. It also includes separate chapters on the glass transition, polymers, polymorphism, purity determination, and method development. The large number of practical examples included should inspire readers toward new ideas for applications in their own fields of work. The chapters are independent of one another and can be read individually in any desired order. Based on years of experience in thermal analysis of users, application specialists, consultants, and course instructors, this book provides practical help to newcomers, inexperienced users, and anyone else interested in the practical aspects of thermal analysis.

The use of thermal and calorimetric methods has shown rapid growth over the past few decades, in an increasingly wide range of applications. The original text was published in 2001; since then there have been significant advances in various analytical techniques and their applications. This second edition supplies an up to date, concise and readable account of the principles, experimental apparatus and practical procedures used in thermal analysis and calorimetric methods of analysis. Written by experts in their field, brief accounts of the basic theory are reinforced with detailed technical advances and contemporary developments. Where appropriate, applications are used to highlight particular operating principles or methods of interpretation. As an important source of information for many levels of readership in a variety of areas, this book will be an aid for students and lecturers through to industrial and laboratory staff and consultants.

Handbook of Thermal Analysis Edited by T. Hatakeyama National Institute of Materials and Chemical Research, Ibaraki, Japan Zhenhai Liu Changchun Institute of Applied Chemistry, China This 425-page reference book covers a comprehensive description of the principles of thermal analysis (TA) instruments, operating conditions, and the nature of the experimental data. Presented in a compact and well-arranged style with a large number of figures and illustrations, this work is divided into two parts. Part I is designed to acquaint and orient newcomers with TA by providing a comprehensive introduction to the basic principles of instrument operation, with advice on sample preparation and optimization of operating conditions, and a guide to interpreting results. The text deals primarily with techniques such as differential scanning calorimetry (DSC), differential thermal analysis (DTA), and thermogravimetry (TG). Part II illustrates 500 TA curves covering metals, inorganic and organic minerals, polymers, construction materials, pharmaceuticals, explosives, etc. The appendices include a glossary of TA terms, a survey of reference materials, the current table of TA standards, and a TA database. This book is aimed at advanced users and specialists who utilize TA methods for practical purposes, especially in research laboratories both academic and industrial. With an emphasis on practical instruction, industrial research staff, undergraduates and postgraduate students in the relevant fields will find this work a useful introduction to principle TA techniques.