Analytical Calorimetry. Volume 5

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1 Analytical Calorimetry Volume 5

2 A Continuation Order Plan is available for this series. A continuation order will bring delivery of each new volume immediately upon publication. Volumes are billed only upon actual shipment. For further information please contact the publisher.

3 Analytical Calorimetry Volume 5 Edited by Julian F. Johnson Institute of Materials Science University of Connecticut Storrs, Connecticut and Philip S. Gill Du Pont Company Wilmington, Delaware PLENUM PRESS NEW YORK AND LONDON

4 The Library of Congress cataloged the first volume of this title as follows: Analytical calorimetry. v New York. Plenum Press. v. ill. 26 cm. Editors: R. S. Porter and J. F. Johnson. Vols for contain the proceedings of the American Chemical Society Symposium on Analytical Calorimetry. ISSN Thermal analysis - Congresses - Collected works. 2. Calorimeters and calorimetry-congress-collected works. I. Porter, Roger Stephen ed. II. Johnson, Julian Frank, ed. III. American Chemical Society Symposium on Analytical Calorimetry. QD79.T38A5 547'.308' Library of Congress Catalog Card Number ISBN-13: DOl: / e-lsbn-13: Proceedings of an International Symposium on Analytical Calorimetry, a part of the 185th National Meeting of the American Chemical Society, held March 20-25, 1983, in Seattle, Washington 1984 Plenum Press, New York Softcover reprint of the hardcover I st edition 1984 A Division of Plenum Publishing Corporation 233 Spring Street, New York, N.Y All rights reserved No part of this book may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, mechanical, photocopying, microfilming, recording, or otherwise, without written permission from the Publisher

5 PREFACE This Volume 5 in a continuing series represents the compilation of papers presented at the International Symposium on Analytical Calorimetry as part of the 185th National Meeting of the American Chemical Society, Seattle, Washington, March 20-25th A much broader variety of topics are covered than in previous volumes, due to the growth in the field of Thermal Analysis. Specific topics covering such techniques as differential scanning calorimetry, combined thermogravimetric procedures, dynamic mechanical analysis and a variety of novel kinetic analyses are covered. A wide range of material types are included in this volume such as polymers (alloys, blends and composites), fossil fuels, biological products, liquid crystals and inorganic materials. The co-editors of this volume would like to thank all the contributors for their efforts in conforming to the manuscript requirements, and for being prompt in the preparation. We would also like to thank those who presided over sessions during the course of the symposium; Professor Anselm C. Griffin, Professor Roger S. Porter and Dr. Edith A. Turi. Philip S. Gill Julian F. Johnson

6 CONTENTS Coupling of DSC and Dynamic Mechanical Experiments for Probing Processing-Structure-Property Relationships of Catalyst Modified High Performance Epoxy Matrices... 1 Thomas E. Munns and James C. Seferis On the Glass Transition of Polyacrylamide H. K. Yuen, E. P. Tam and J. W. Bulock The Binary Blends, Transreaction and Copolymers of Bisphenol-A Polycarbonate and a Polyarylate 25 Masao Kimura and Roger S. Porter Curie Temperatures of the lcta Certified Reference Materials... 1# Paul D. Gam and Ali-Asghar Alamolhoda Thermal Analysis of Acrylamide-Based Polymers 43 J. J. Maurer, D. N. Schulz, D. B. Siano, and J. Bock Defining B-Stage and Total Cure for a Dicy Based Epoxy Resin by DSC Bernd K. Appelt and Pamela J. Cook Differential Scanning Calorimetry: Simultaneous Temperature and Calorimetric Calibration 67 W. Eysel and K.-H. Breuer Dynamic Mechanical Analysis Application to Dynamic Thermomechanometry Takayuki Murayama Applications of Differential Rheometry 95 P. H. Foss and M. T. Shaw Materials Characterization Using Thermogravimetry Coupled to Triple Quadrupole Tandem Mass Spectrometry (MS/MS) 105 Bori Shushan, Bill Davidson, and R. Bruce Prime vii

7 viii CONTENTS Calorimetric Response of Fossil Fuel Systems: Prospects and Problems.. " Krishnan Rajeshwar Multiple Sample Differential Scanning Calorimetry Robert C. Johnson and Valdis Ivansons 133 Quantitative Evaluation of the Gibbs-DiMarzio Theory of the Glass Transition for Polystyrene 143 A. R. Greenberg and R. P. Kusy Study on Adhesives Performance by Dynamic Mechanical Techniques Lecon Woo 1 Effect of Molecular Structure of Mesomorphism. 15. Thermal and X-ray Diffraction Analysis of a "Siamese Twin" Series: The 4,4'-Dicarboxy-a,w-Diphenoxya1kanes 169 Anselm C. Griffin, Sharon Gorman, and William E. Hughes Reversibility and Capacity of Different Energy Storage Reactions by Calorimetry 179 Pierre Le Par10uer Power Scanning Calorimetry (PSC) 191 Joeseph Hakl A Combined TG-GC-MS System for Materials Characterization 197 Jen Chiu A New Approach for Determining Mechanical Properties of Thermoset Resins Charles Grame1t The Melting Temperature of Polymers: Theoretical and Experimental L. Mande1kern, G. M. Stack and P. J. M. Mathieu Nonequi1ibrium Thermodynamics and Modern Dynamic Thermal Analysis.Techniques Paul H. Lindenmeyer and Genia Paul Integral-Differential Relationships in Thermal Analysis 255 John P. Elder The Characterization of Water in Treed Crosslinked Polyethylene Films... "." R. A. Weiss, S. H. Shaw, and M. T. Shaw

8 CONTENTS Application of Combined Thermogravimetry Atmospheric Pressure Chemical Ionization Mass Spectrometry to,c.opolymer Analysis Susan M. Dyszel Semi-Automated Measurement of Composites Flexural Stress Relaxation P. S. Gill and J. D. Lear Some Uses of Differential Scanning Calorimetry in Biomembrane Research Donald L. Melchior The Effect of Sample Temperature Gradients on DSC Thermograms at the Glass Transition Temperature 325 Edward Donoghue, Thomas S. Ellis, and Frank E. Karasz Characterization of Coal Liquefaction Residues by Thermal Methods of Analysis Charles M. Earnest Computer Automation of the Dynamic Mechanical Analyzer and its Application to Cure Kinetics Studies and Dynamic Mechanical Property Analysis of Organic Coatings 361 M. E. Koehler, A. F. Kah, C. M. Neag, T. F. Niemann, F. B. Malihi and T. Provder Cure Reaction Kinetics Characterization of Some Model Organic Coatings Systems by FT-IR and Thermal Mechanical Analysis T. Provder, C. M. Neag, G. Carlson. C. Kuo and R. M. Holsworth Contributors 395 Index ix

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