_STP_1466-2007.pdf

STP 1466Techniques in Thermal Analysis:Hyphenated Techniques,ThermalAnalysis of the Surface,and FastRate AnalysisWei-Ping Pan and Lawrence Judovits,editorsASTM Stock Number:STP1466ASTM100 Barr Harbor DrivePO Box C700West Conshohocken,PA 19428-2959Printed in the U.S.A.Library of Congress Cataloging-in-Publication DataTechniques in thermal analysis:hyphenated techniques,thermal analysis of the surface,and fast rateanalysis/Wei-Ping Pan and Lawrence Judovits,editor.p.cm.“STP1466.”ISBN 978-0-8031-5616-61.Thermal analysisCongresses.2.ThermogravimetryCongresses.I.Pan,Wei-Ping,1954-II.Judovits,Lawrence,1955-QD79.T38T384 2007543.26dc222007004395Copyright 2007 AMERICAN SOCIETY FOR TESTING AND MATERIALS INTERNATIONAL,WestConshohocken,PA.All rights reserved.This material may not be reproduced or copied,in whole orin part,in any printed,mechanical,electronic,film,or other distribution and storage media,without thewritten consent of the publisher.Photocopy RightsAuthorization to photocopy items for internal,personal,or educational classroom use,orthe internal,personal,or educational classroom use of specific clients,is granted by theAmerican Society for Testing and Materials International(ASTM)provided that the appropri-ate fee is paid to the Copyright Clearance Center,222 Rosewood Drive,Danvers,MA 01923;Tel:978-750-8400;online:http:/ Review PolicyEach paper published in this volume was evaluated by two peer reviewers and at least one editor.The authors addressed all of the reviewers comments to the satisfaction of both the technicaleditor(s)and the ASTM International Committee on Publications.The quality of the papers in this publication reflects not only the obvious efforts of the authors andthe technical editor(s),but also the work of the peer reviewers.In keeping with long-standing publica-tion practices,ASTM International maintains the anonymity of the peer reviewers.The ASTMInternational Committee on Publications acknowledges with appreciation their dedication and contri-bution of time and effort on behalf of ASTM International.Printed in Mayfield,PAJuly,2007iiiForewordThis publication,Techniques in Thermal Analysis:Hyphenated Techniques,ThermalAnalysis of the Surface,and Fast Rate Analysis,contains papers presented at the sympo-sium of the same name held at ASTM International Headquarters,W.Conshohocken,PA,on 24-25 May 2004,sponsored by the ASTM International Committee E37 on ThermalMeasurements.The symposium chairmen were Prof.Wei-Ping Pan,Western KentuckyUniversity,Bowling Green,KY and Dr.Lawrence Judovits,Arkema Inc.,King of Prussia,PA.vContentsOVERVIEWVIIHYPHENATEDTECHNIQUESAn Application of Thermal Analysis to Household Waste Z.CHENG,H.CHEN,Y.ZHANG,P.HACK,ANDW.PAN3Development and Evaluation of a TG/DTA/Raman SystemW.J.COLLINS,C.DUBOIS,R.T.CAMBRON,N.L.REDMAN-FUREY,ANDA.S.BIGALOWKERN13The Role of TGA-DTA in the Initial Evaluation of the Solid State Forms for Pharmaceutical New Chemical Entities,Part 1:Evaluation of Pure FormsN.L.REDMAN-FUREY,M.L.DICKS,J.GODLEWSKI,D.C.VAUGHN,ANDW.J.COLLINS23The Role of TGA-DTA in the Initial Evaluation of the Solid State Forms for Pharmaceutical New Chemical Entities,Part 2:Evaluation of Mixed FormsN.L.REDMAN-FUREY,M.L.DICKS,J.GODLEWSKI,D.C.VAUGHN,ANDW.J.COLLINS33Use of a TG/DTA/Raman System to Monitor Dehydration and Phase ConversionsA.S.BIGALOWKERN,W.J.COLLINS,R.T.CAMBRON,ANDN.L.REDMAN-FUREY42Quantitative Mass Measurements from Mass Spectrometer Trend Data in a TG/MS SystemC.G.SLOUGH52Separation of Overlapping Processes from TGA Data and Verification EGAR.ARTIAGA,R.CAO,S.NAYA,B.GONZLEZ-MARTIN,J.L.MIER,ANDA.GARCIA60Characterization of Modified Carbon Nanotubes by TG-MS and Pyrolysis-GC/MSQ.LINEBERRY,T.BUTHELEZI,ANDW.PAN72FASTRATEANALYSISCharacterization of Epoxy Curing Using High Heating Rate DSCB.BILYEU,W.BROSTOW,ANDK.P.MENARD83THERMALANALYSIS OF THESURFACEPhoto Thermal Micro-Spectroscopy A New Method for Infared Analysis of MaterialsC.G.SLOUGH,A.HAMMICHE,M.READING,ANDH.M.POLLOCK95A Thermal Analysis Method for Measuring Polymer Flammability R.E.LYON,R.N.WALTERS,ANDS.I.STOLIAROV101Fast Scan Differential Scanning Calorimetry Distinguishes Melting,MeltingDegradation/Sublimation and Thermal Stability of DrugsA.RIGA,M.GOLINAR,ANDK.ALEXANDER119Thermal and Oxidative Properties of Physiologically Relevant Free Fatty Acids By Dielectric Analysis Differential Scanning CalorimetryA.RIGA,K.ALEXANDER,ANDK.WILLIAMS127viCONTENTSviiOverview(updated 1/12/2007)In May 2004 a two day symposium titled“Techniques in Thermal Analysis:Hyphenated Techniques,Thermal Analysis of the Surface,and Fast Rate Analysis”was held at the ASTM Headquarters inWest Conshohocken,PA.Twenty-two presentations were given at the symposium.Additionally,thepresenters were given the opportunity to submit to the Journal of ASTM International and for theirpapers to be included into a special technical publication(STP),thirteen papers were received.The symposium itself was timely and reflected leading edge research in thermal