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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.

The aim of this book is, as its title suggests, to help sOilleone with little or no knowledge of what thermal analysis can do, to find out briefly what the subject is all about, to decide whether it will be of use to him or her, and to help in getting started on the more common techniques. Some of the less-common techniques are mentioned, but more specialized texts should be consulted before venturing into these areas. This book arose out of a set of notes prepared for courses on thermal analysis given at instrument workshops organized by'the S.A. Chemical Institute. It has also been useful for similar short courses given at various universities and technikons. I have made extensive use ofthe manufacturers'literature, and I am grateful to them for this information. A wide variety of applications has been drawn from the literature to use as examples and these are acknowledged in the text. A fuller list of the books, reviews and other literature ofthermal analysis is given towards the back of this book. The ICTA booklet'For Better Thermal Analysis'is also a valuable source of information. I am particularly grateful to my wife, Cindy, for typing the manuscript, to Mrs Heather Wilson for the line drawings, and to Professor David Dollimore of the University of Toledo, Ohio, for many helpful suggestions.