Thermal Analysis Fundamentals and Applications to Polymer Science 2d Ed - T. Hatakeyama,
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Thermal Analysis
Fundamentals and Applications to Polymer Science
Second Edition
T. Hatakeyama
Otsuma Women's University, Faculty of Home Economics, Tokyo, Japan
F.X. Quinn
L'Oréal Recherche Avancée, Aulnay-sous-Bois, France
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Library of Congress Cataloging-in-Publication Data
Hatakeyama, T.
Thermal analysis: fundamentals and applications to polymer
science/ T. Hatakeyama, F.X. Quinn. —2nd ed.
p. cm.
Includes bibliographical references and indexes.
ISBN 0-471-98362-4 (hb)
1. Thermal analysis. 2. Polymers—Analysis. I. Quinn, F.X.
II. Title.
QD79.T38H38 1999
543'.086—dc21 98-49129
CIP
British Library Cataloguing in Publication Data
A catalogue record for this book is available from the British Library
ISBN 0 471 98362 4
Typeset in 10/12pt Times New Roman by Pure Tech India Ltd, Pondicherry
Printed and bound in Great Britain by Biddles Limited, Guildford, Surrey
This book is printed on acid-free paper responsibly manufactured from sustainable forestry, in which at
least two trees are planted for each one used for paper production.
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Contents
Preface
ix
Preface to the Second Edition
x
1
Thermal Analysis
1
1.1 Definition
1
1.2 Characteristics of Thermal Analysis
2
1.3 Conformation of Thermal Analysis Instruments
3
1.4 Book Outline
4
2
Differential Thermal Analysis and Differential Scanning Calorimetry
5
2.1 Differential Thermal Analysis (DTA)
5
2.1.1 Custom DTA
7
2.2 Quantitative DTA (Heat-Flux DSC)
8
2.3 Triple-Cell Quantitative DTA
2.4 Power Compensation Differential Scanning Calorimetry (DSC)
2.5 Temperature Modulated DSC (TMDSC)
2.5.1 General Principles of Temperature Modulated DSC
2.5.2 TMDSC Calibration
2.5.3 TMDSC Experimental Conditions
2.6 High-Sensitivity DSC (HS-DSC)
2.7 Data Analysis and Computer Software
2.8 Automated TA Systems
2.9 Simultaneous TA
2.10 Installation and Maintenance
2.11 References
3
Calibration and Sample Preparation
3.1 Baseline
3.1.1 Baseline Curvature and Noise
3.1.2 Baseline Subtraction
3.1.3 Baseline Correction
3.2 Temperature and Enthalpy Calibration
3.3 Sample Vessel
3.4 Sample Preparation
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3.4.1 Films, Sheets and Membranes
3.4.2 Granules and Blocks
3.4.3 Powders
3.4.4 Fibres and Fabrics
3.4.5 Biomaterials and Gels
3.4.6 Storing Samples
3.5 Temperature Gradient in Sample
3.5.1 Mass of Sample
3.5.2 Solutions
3.6 Sample Packing
3.6.1 Hydrophilic Sample
3.6.2 Liquid Sample
3.7 Purge Gas
3.8 Scanning Rate
3.9 Sub-ambient Operation
4
Thermogravimetry
4.1 Introduction
4.2 Thermobalance
4.2.1 Installation and Maintenance
4.2.2 Microbalance and Crucible
4.2.3 Furnace and Temperature Programmer
4.2.4 Data Recording Unit
4.3 Temperature Calibration
4.4 Sample
4.5 Atmosphere
4.6 Heating Rate
4.7 Classification of TG Curves
4.8 Calculation of Mass Change Rates
4.9 Derivative Thermogravimetry (DTG)
4.10 Intercomparison of TG and DTA
4.11 TG Reports
4.12 References
5
Applications of Thermal Analysis
5.1 Temperature Measurement
5.2 Enthalpy Measurement
5.2.1 Polymer Melting (Initial Crystallinity)
5.3 Reaction Rate Kinetics
5.3.1 Differential Methods
5.3.2 Integral Methods
5.3.3 Jump Method
5.3.4 Isothermal Crystallization of Polymers
5.3.5 General Comment on Reaction Rate Kinetics
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