proceedings of the twenty-seventh ... conference of the north american thermal analysis society...
TRANSCRIPT
PROCEEDINGS OF THETWENTY-SEVENTH
CONFERENCE OF THENORTH AMERICAN
THERMAL ANALYSISSOCIETY
SEPTEMBER 20-22, 1999SAVANNAH, GEORGIA
UB/TIB Hannover 89121 264 211
Edited byKathryn R. WilliamsUniversity of Florida
Keith KocibaBAS Analytics
TWENTY-SEVENTH CONFERENCEOF THE
NORTH AMERICAN THERMALANALYSISSOCIETY
September 20-22,1999Savannah Marriott Riverfront, Savannah, Georgia
MONDAY MORNING
OPENING SESSIONSavannah C; Kathy Lavanga, Presiding
8:00 Opening Remarks, Kathy Lavanga
8:10 Mettler Award Presentation, Stephen Z. D. Cheng
PLENARY LECTURESavannah C; David Dollimore, Presiding
8:50 Analysis of Materials by Temperature-ModulatedCalorimetry Using Heat Capacities, GlassTransitions and First-Order Transitions, BernhardWunderlich 3
9:30 Break
CHARACTERIZATION OF POLYMERS BY TASavannah E; Bernhard Wunderlich, Presiding
10:00 Characterization of Thermoplastics and Elastomersby Modulated Temperature DSC, Alan Riga and BrianSisk 9
10:20 Measuring Equilibrium and Frequency DependentSpecific Heats of Polymers by a Pubed DSCTechnique, N. Agarwal and R. J. Farris 15
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10:40 Reversible and Irreversible Heat Capacity ofPoly(Trimethylene Terephthalate) by Temperature-Modulated Differential Scanning Calorimetry, MarekPyda and Bernhard Wunderlich 21
11:00 Thermal Properties of Gel-Spun, Ultra High MolarMass Polyethylene Fibers, Yong Ku Kwon andBernhard Wunderlich 27
11:20 StepScan DSC: An Alternative to ConventionalModulated Techniques, Bruce Cassel, Piero Scotto,and Bill Sichina 33
11:40 Thermal Analysis of Polymers Using 'VirtualInstruments', Ian R. Harrison 37
KINETIC ANALYSIS OF TA DATA FOR HAZARD ASSESSMENTSavannah D; Richard E. Lyon, Presiding
8 10:00 Invited Lecture: Thermal Analysis of PolymerFlammability, Richard E.Lyon (invited speaker) 42
9 10:40 Flammability Kinetics From TGA/DSC/GCMS,Microcalorimetry, and Computational QuantumChemistry, Phillip R. Westmoreland, TalineInguilizian, and Karin Rotem 48
10 11:00 Stabilizing Effect of Oxygen on ThermalDegradation of Poly (Methyl Methacrylate), JefferyD. Peterson, Sergey Vyazovkin, and Charles A. Wight
49
11 11:20 Concept of Variable Activation Energy (Why It JustCan't Stay Put), Sergey Vyazovkin 55
12 11:40 Hazard Evaluation of Thermally Unstable Materialsby DSC-An Overview, Roger Blaine, Pearl Chin, andPeter Whittingstall 61
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THE ANALYSIS OF THE PHYSICAL PROPERTIES OF MINERALS,METALS AND HIGH ENERGY MATERIALS USING THERMAL
TECHNIQUESOglethorpe A-B; Sergey Vyazovkin, Presiding
13 10:00 Micro-Thermal Analysis™ for Airport Detection ofEnergetic Materials, Chien-Chung Chen, William W.Bannister, Arvind Viswanathan, John Furry, and GraySlough 67
14 10:40 Thermal Analysis of High Explosives: Liquid StateDecomposition of RDX, Gregory T. Long, SergeyVyazovkin, Brittany A. Brems, and Charles A. Wight 73
15 11:00 Recognition and Temperature Assignment of Transitions inSelected Inorganic Solids by Thermomecbanical Analysis.Part I, Charles M. Earnest and Rickey J. Seyler 79
16 11:20 Recognition and Temperature Assignment ofTransitions in Selected Inorganic Solids byThermomechanical Analysis. Part H. Zirconia,Copper Sulfate Pentahydrate, and Calcium OxalateMonohydrate, Rickey J. Seyler and Charles M.Earnest 80
MONDAY AFTERNOON
CHARACTERIZATION OF POLYMERS BY TASavannah E; Bernhard Wunderlich, Presiding
17 13:30 Invited Lecture: Size Effect of Metastable States onSemicrystalline Polymer Structures andMorphologies, Stephen Z. D. Cheng (invited speaker),Jason J. Ge, Bqjie Wang, Lei Zhu, and Christopher Y.Li 81
18 14:10 A Study of the Annealing of Poly(Ethylene-co-Octene) by Standard DSC and Temperature-Modulated DSC, R. Androsch and BernhardWunderlich 87
19 14:30 Tf and Cp Measurements on Perfluoropolyethers,Richard L. Siemens and T.E. Karis 93
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20 14:50 New TMA Method for the Measurement ofPolymerization-Induced Shrinkage inPhotopolymers, Harvey E. Bair, Marcia L. Schilling,Vicki L. Colvin, Arturo Hale, and Nicholas J. Levinos 99
15:10 Break
21 15:30 Analysis of Nanophase Structure of SemicrystallinePolymers with Atomic Force Microscopy,Microcalorimetry, and Temperature-ModulatedCalorimetryfTMQ, Bernhard Wunderlich and I.Moon 105
22 15:50 Investigation of Entangled Chains in Semi-Crystalline Polyethylenes by A Novel CalorimetryTechnique and by Turbidity at a Lower CriticalSolution Temperature, H. Phuong Nguyen, PaulBernazzani, and Genevieve Delmas 111
23 16:10 New Enhancements in the Area of High ResolutionDifferential Scanning Calorimetery (DSC), Vijay N.Reddy, Nobutaka Nakamura, and Randy Byrne 117
KINETIC ANALYSIS OF TA DATA FOR HAZARD ASSESSMENTSavannah D; Richard E. Lyon, Presiding
24 13:30 Safe Process Development for Reaction HazardsTesting, David J. Leggett 118
25 13:50 Application of Reaction Calorimetry TowardUnderstanding the Large Scale Chemistry of EthylDiazpacetate, Jerry Clark H 9
26 14:10 Phenomenon of Autocatalysis in Decomposition ofEnergetic Chemicals, Sima Chervin and Glenn T.Bodman I2 5
27 14:30 Multivariate Non-Linear-Regression Kinetics andThermal Simulation of Reactions with ExothermalDecomposition Potential, E. Kaisersberger and J.Opfermann 131
28 14:50 Kinetics of Thermal Degradation of EPDM UsingAdvanced Thermal Analysis, Clint D. Gamlin, NabaK. Dutta, Namita Roy-Choudhury, Jani G. Matisons,and D. Kehoe 132
15:10 Break
THE ANALYSIS OF MECHANICAL PROPERTIES OF MATERIALSUSING DYNAMIC MECHANICAL AND DIELECTRIC TA
Savannah D; Lin Li, Presiding
29 15:30 The Torsion of Solids in a Rotational Rheometerand Its Comparison to DMA, Peter R. Whittingstalland Louis E. Waguespack 138
30 15:50 Characterization of Core-Shell Polymers andGrafted Lattices by Combined DynamicMechanical/Electrical Analysis, R. D. Sanderson andJ. Vermeulen 144
31 16:10 Dynamic Mechanical Properties of an Epoxy-BasedUnderfill Material, Yi He 145
32 16:30 Introduction to the Environment ControlledDynamic Viscoelasticity Measurement System, VijayN. Reddy, Hideteka Kato, Toshihiko Nakamura, andNick Ohkubo 151
33 16:50 DMA-FTK Study of Polymer Rheology andMolecular Dynamics, Haochuan Wang, Richard A.Palmer, and Steven R. Aubuchon 157
THE ANALYSIS OF THE PHYSICAL PROPERTDZS OF MINERALS,METALS AND HIGH ENERGY MATERIALS USING THERMAL
TECHNIQUEOglethorpe A-B; Sergey Vyazovkin, Presiding
34 13:30 Thermal Analytical Investigation of DifferentialSurface Weathering on Indiana Limestone: A Studyof the Michael Lantz Sculptures: Federal TradeCommission, Washington, DC, James E. Adams,David Dollimore, and John G. Lee 163
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35 13:50 An Examination of Recylced Portland CementConcrete Rich in Dolomite and Low in CalciteObtained from Various Locations in Ohio, S.Lerdkanchanaporn, S. Nippani, J. D. Gupta, andDavid Dollimore 170
36 14:10 The Local Industries of Savannah and Georgia andWhat Can Be Learned About Them from ThermalAnalysis, David Dollimore 171
37 14:30 Thermal Analysis of Floyd Shale, Charles M. Earnestand Erin Rudzinski 172
38 14:50 High Accuracy Specific Heat Measurement hiComplex Metal Alloys, J. B. Henderson 173
39 15:10 Thermoanalytical Studies on the Sintering of Bi2O3,Blaine J. Weddle, J. A. Foreman, and P. K. Gallagher
174
40 15:30 Lead-Tin Solder Characterization by DifferentialScanning Calorimetry, Mark F. Fleszar 175
15:50 Break
APPLICATION OF THERMAL ANALYSIS IN INDUSTRY PRODUCTDEVELOPMENT
Oglethorpe A-B; John Rose, Presiding
41 16:00 Invited Lecture: Thermal Analysis for IndustrialProduct Development: Things You Really Shouldn'tDo, Kevin P. Menard (invited speaker) 1 8 1
42 16:40 Thermal Decomposition Granite and MarbleIndustry Reject By TG/DTG/DTA, Heitor FernandesMoth6 Filho, Cheila Goncalves Mothe" I 8 2
MONDAY EVENING
POSTER SESSION, 5:00-6:30Savannah C; Wei-Ping Pan, Presiding
PI Thermal Decomposition Analysis of MagnesiumHydroxide, R. Malhotra, K. Alexander, and D. Dollimore 187
P2 An Investigation into the Thermal Decomposition ofMagnesium Carbonate Samples, N. Khan, K. Alexander,and D. Dollimore 191
P3 The Thermal Decomposition Behaviors of Stearic Acid,Paraffin Wax, and Polyvinyl Acetate, Chung-King Hsu,Jinn-Shing Lee, and Wenjea Tseng 196
P4 Binder Decomposition from a Sample of Ceramic InjectionMolding, Chung-King Hsu, Jinn-Shing Lee, and Wenjea J.Tseng 202
P5 A Study on the Devitrification of Calcium PhosphateGlasses with Various Ca/P Molar Ratios, Chung-King Hsu,Jinn-Shing Lee, and Kuo-Chung Dong 208
P6 The Thermal Properties of KCIO4 with Different ParticleSize, Jinn-Shing Lee and Chung-King Hsu 215
P7 Thermal Decomposition Behaviors of PETN, RDX, andHMX, Jinn-Shing Lee and Chung-King Hsu 221
P8 The Thermal Behaviors and Safety Characteristics ofComposition B Explosive, Jinn-Shing Lee and Chung-KingHsu 226
P9 DSC Studies on the Phase Transition, Decomposition andMelting of Potassium Perchlorate with Additives, Jinn-Shing Lee and Chung-King Hsu 232
P10 The Effect of Different Zirconium on Thermal Behaviorsfor Zr/KCIO4 Priming Composition, Jinn-Shing Lee andChung-King Hsu 237
P l l Kinetic Studies on Devitrification of Calcium PhosphateGlass with TiO2, A12O3, and SiO2 Additions, Jinn-ShingLee, Chung-King Hsu, and Kuo-Chung Dong 243
P12 The Thermal Degradation of Corn Starch in the Presenceof Preservatives, Carolyn A. O'Connell and David Dollimore 251
P13 Thermal Investigation of Amylose Phase Composition:Correlation of DSC and FTIR Techniques, Paul Bernazzani,Camille Chapados, and Genevieve Delmas 252
P14 Optimization of Percent Carbon Black by TGA, Roger E.Moody 258
P15 Use of Several Thermal Analysis Techniques to Study theCracking of a Nitrile Butadiene Rubber (NBR) Insulatoron the Booster Separation Motor (BSM) of the SpaceShuttle, Charles D. Wingard 259
P16 Thermal Characterization of TNT and HNIW Mixtures,Tsao-Fa Yeh 260
P17 Kinetics of Thermal Decomposition of PropellantsContaining GAP as Binder, Tsao-Fa Yeh 266
P18 Thermal Behavior of Propellants Containing GAP asBinder, Tsao-Fa Yeh 267
P19 The Influence of Stress Changes on the Kinetics ofCrystallization of FejgNijSigBuCj Amorphous Alloy, JelenaA. Maricic, Zorica V. Marinkovic, Aleksa M. Maricic andMomcilo M. Ristic 268
P20 A Cure Kinetic Model of Polyester Resins, Marco A. M.Menezes, and Verdnica M. A. Cal^jo 269
P21 Thermal Analysis of NTO: Com^titive Sublimation andCondensed Phase Decomposition of a High Explosive,Gregory T. Long, Brittany A. B r e i ^ ^ d Charles A. Wight 270
P22 Center for Thermal Analysis, Se r g e y Vyazovkin and CharlesA. Wight 276
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P23 The Characterization of Ascorbic Acid by Kinetic Analysisof Thermogravimetric Data, Chunhong Gu, K. S.Alexander, and David Dollimore 277
P24 Using Simultaneous TGA-DSC to More EffectivelyCharacterize Metals, Minerals, and Polymers, E. Post andB. Fidler 283
P25 Cooling Rate Study Between Heat Flux and PowerCompensation Differential Scanning Calorimeters, SeverineBarrau and Lawrence Judovits 284
P26 Thermal Characterization of Polycarbonate/Granite andMarble Reject Composites, Cheila Goncalves Mothe", LeilaIna'cio Passos, and Luci D.B. Machado 289
P27 An Investigation of Maleic Acid Using Simultaneous TG-DTA, Shontell F. Wright, Kenneth S. Alexander, and DavidDollimore 295
P28 Dynamic Mechanical Analysis and MorphologicalCharacterization of Polystyrene-Polyisobutylene-Polystyrene Copolymers, Dawn M. Crawford, EugeneNapadensky, Nora C. Beck Tan, Kenneth S. Laverdure,Samuel P. Gido, David A. Reuschle, David A. Mountz, andKenneth A. Mauritz 296
P29 Thermal Properties of Elastic Fibers and Yarns, GajananBhat, Subhash Chand, and Simon Yakopson 302
P30 Thermal Degradation of Vinylidene Chloride/VinylChloride Copolymers hi the Presence of N-SubstitutedMaleimides, Bob A. Howell and J. Zhang 308
P31 Thermal Analysis of Ground Dolomite, M. Samtani, K.Alexander, and David Dollimore 309
P32 Isothermal and Non-Isothermal Cure Kinetics ofPolynaphthalene Networks from Bis-o/tAo-diynylarene(BODA) Monomers, Hiren V. Shah, David A. Babb, andDennis W. Smith, Jr. 315
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P33 Validation of DSC and TGA for Pharmaceutical Analysisunder Current Good Manufacturing Practices, Robert P.Weissburg, Fred E. Burris, Theodora K. Ferrell, and EdaRoss-Montgomery 321
P34 Effect of Plasticizers on the Glass Transition Temperatureof Cellulose Acetate Polymeric Membrane, A. S. Tatavarti,K. S. Alexander, and David Dollimore 322
P35 Characterization of Glass Pastes for Sensor Applications,Indira S. Adhihetty, Dianne L. White, and DaXue Xu 323
P36 Dynamic-Mechanical Properties of Frozen Doughs: Effectsof Sugar, NaCl and Sugar-NaCl Mixture, Tommi J.Laaksonen and Yrjo H. Roos 329
P37 Reproducibility Analysis of pTA Measurements as aFunction of the Molecular Size of Polymer Specimens,Matthew W. Tillman, Brian S. Hayes, and James C. Seferis
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TUESDAY MORNING
PLENARY LECTURESavannah C; David Dollimore, Presiding
43 8:00 Review of Coupling Techniques for TG-MS andTG-FTCR, Erwin W. Kaisersberger 330
8:40 Break
CHARACTERIZATION OF POLYMERS BY TASavannah E; Bernhard Wunderlich, Presiding
44 9:00 Changes in Structure and Properties of PP FibersDuring Thermal Bonding, Subhash Chand, GajananS. Bhat, Joseph E. Spruiell, and Sanjiv R. Malkan 333
45 9:20 The Determination of Heat Capacities by Saw-ToothModulated TMDSC with Multiple Frequencies,Jeongihm Pak and Bernhard Wunderlich 339
46 9:40 Heat Capacities by Multi-Frequencies Saw-ToothModulation by Standard DSC, Marek Pyda andBernhard Wunderlich 345
47 10:00 Successive Self-Nucleation and Annealing (SSA): ANovel DSC Thermal Fractionation Technique forPolymer Characterization, Alejandro J. Muller,Maria L. Arnal, Angelica S&ichez, and VittoriaBalsamo 351
48 10:20 Use of Several Thermal Analysis Techniques on aHypalon Paint Coating for the Solid Rocket Booster(SRB) of the Space Shuttle, Charles D. Wingard 357
10:40 Break
49 11:00 Thermal Characterization of High-Strain,Electrostrictive Poly(Vinylidene Fluoride-Trifluoroethylene) Copolymers, ThomasRamotowski, Kenneth Hamilton, George Kavarnos, Q.Zhang, and V. Bharli 366
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50 11:20 Polymer Durability Estimates Based on ActivationEnergies of Thermal Oxidative Degradation, SamuelY. Ding, Atul R. Khare, Michael T. K. Ling, andLecon Woo 372
51 11:40 Heats of Immersion of PANI hi NMP, K. Strobach,N. Luce, H. Phuong Nguyen, Sandrine Amrani, andGenevieve Delmas 378
MATERIALS CHARACTERIZATION USING SIMULTANEOUSAND COMBINED TECHNIQUES
Savannah D; Michael Reading, Presiding
52 9:00 Evaluation of Curing and Thermal Stability of anEpoxy Resin by Means of Simultaneous ThermalAnalysis (STA), John H. Suwardie, Ramon Artiaga,and Laura Garcia 383
53 9:20 DSC by the TGA/SDTA 851E Considering MassChanges, Rudolf Riesen, Markus Schubnell, andJonathon Foreman 389
54 9:40 Expanding the Capabilities of TGA-FTIR: The Useof Reduced Pressure, Richard S. Jackson andAlbrecht Rager 395
55 10:00 Characterization of Thermal Stability Behavior byMeans of TGA/FTIR-Coupung hi QualityAssurance, Frank Hoffmann, Rudolf Riesen, andJonathon Foreman 401
10:20 Break
56 10:40 Characterization of the Thermally-InducedResponse of Complex Materials Using SimultaneousTGA-DSC-MS, J.B. Henderson and E. Post 407
57 11:00 Thermal Characterization of Organically ModifiedMontmorillonite, Wei Xie, Zongming Gao, KunleiIiu, Ying Xie, Wei-Ping Pan, Richard Vaia, DougHunter, and Anant Singh 408
xvm
58 11:20 Effects of Brand, Grade, and Fuel Contaminationupon the Thermal Stability of Motor Oils, BrianSisk, Daozhong Zou, Wei-Ping Pan, and Alan Riga 414
59 11:40 Micro-Thermal Analysis and Evolved Gas Analysis,Trevor J. Lever, Mike Reading, and Duncan M. Price 420
APPLICATION OF THERMAL ANALYSISIN INDUSTRY PRODUCT DEVELOPMENT
Oglethorpe A-B; John Rose, Presiding
60 9:00 Multiplexing Frequency Mode Study of PackagingEpoxy Molding Compounds Using DynamicMechanical Analysis, Chi F. Tsang and Hui K. Hui 426
61 9:20 Characterization of Body Lotions Using Thermaland Rheological Analysis, Lin Li, Greg Curran,Ming-Long Yao, and Charles Rohn 432
62 9:40 Customizing Thermal Software, Bruce Cassel, Rich
Linley, and Ken Fielder 438
10:00 Break
63 10:20 DSC and DEA Studies of Underfill Curing Kinetics,Yi He 442
64 10:40 Rapid Quality Control of Materials Using ThermalAnalysis Based on Microtechnologies, JL. Daudon,L. Benoist, G. Hurel, C. Goupil, P. Le Parlouer 448
65 11:00 Measurement of Engine Oil Volatilities Using theTGA Noack Test, W. J. Sichina 454
66 11:20 Thermal Degradation of Styrene Duner MimicsDerived from Vinylnaphthalene, Bob A. Howell, J.J.Powers, and D. B. Priddy 455
XJX
TUESDAY AFTERNOON
BUSINESS MEETING, 12:00-12:45Savannah C; David Dollimore, Presiding
CHARACTERIZATION OF POLYMERS BY TASavannah E; Bernhard Wunderlich, Presiding
67 14:00 Dynamic Mechanical Spectroscopy of Paper, LynnC. Walker 4 56
68 14:20 Semi-Crystalline Polyethylene in the MeltingTemperature Range Studied by Light HeatingTemperature Modulated DSC, Yasuo Saruyama 462
69 14:40 Thermal Decomposition Kinetics of HMX, PeteLofy, Sergey Vyazovkin, and Charles A. Wight 467
15:00 Break
70 15:20 Application of the Oxidative Induction Test (OIT)to Depolymerizing Systems, Lecon Woo, Atul Khare,Samuel Y. Ding, and H. Blom 473
71 15:40 Thermal, Mechanical, and Rheological Comparisonof Stereoblock Flexible Polypropylenes, Atul R.Khare, Sam Ding, Lecon Woo, Chuan Qin, andMichael T.K. Ling 480
72 16:00 Thermal Characterization of PMR Polyimides, WeiXie, Kunlei Liu, Ying Xie, Wei-Ping Pan, and KathyC. Chuang 486
73 16:20 Evolution of Thermal Analysis Over at AlliedSignalDuring 1975-2000: From Advances inInstrumentation to Product-Process-BusinessDevelopment, Yash P. Khanna 4 9 2
74 17:00 Thermal Analysis Characterization of ACommercial Thermal Cure Adhesive, Priya L.Tabaddor, Charles J. Aloisio, Claire H. Plagianis, CarlR. Taylor, and Harvey E. Bair 4 9 5
75 17:20 Student Award Paper
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GENERAL SESSION ANDTHERMAL ANALYSIS OF FOODSavannah D; David Jones, Presiding
76 14:00 Phase Transition of Apple Cuticles: A DSC Study,Poonam Aggarwal 502
77 14:20 The Influence of Processing Conditions on theThermal Analysis of Foods, Jonathon A. Foremanand Georg Widmann 507
78 14:40 Invited Lecture: Application of StepwiseTemperature and Pressure Scanning ThermalAnalysis hi Identifying Retrograde Vitrification hiPolymers and hi Foaming Process Development,Paul Handa (invited speaker) 511
15:20 Break
79 15:40 Cycloalkanes Solubility Determination ThroughDifferential Scanning Calorimeter, Paul H. Young,David Dollimore, and Constance A. Schall 512
80 16:00 An Alternative Method to the Curing Study ofPolymeric Die Attach Adhesives Using DynamicMechanical Analysis, Chi F. Tsang and Hui K. Hui 518
81 16:20 Vapor Pressure Determination byThermogravimetry, Duncan M. Price 524
82 16:40 Microcalorimetry DSC Study of the Compatibilityof Energetic Materials, Albert S. Tompa and WilliamF. Bryant, Jr. 530
83 17:00 Comparison of Oxidative Behavior of Materials byDSC under Varying Pressure Conditions, S.Knappe, E. Treser, and B. Fidler 538
84 17:20 Temperature and Heat Flow Calibration of A DSCInstrument Between -140°C and 160°C, MarkusSchubnell, Rudolf Riesen, and Jonathon Foreman 539
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RHEOLOGY SESSIONOglethorpe A-B; Larry Judovits, Presiding
85 14:00 Invited Lecture: The Rheology and ThermalProperties of Personal Products, Ming-Long Yao,Charles L. Rohn (invited speaker), and John Suwardie 545
86 14:40 Introduction to Rheology for the Non-Rheologist,Kevin P. Menard 549
87 15:00 Rheological and Dynamic Thermal Analysis ofFailed Engine Oils, Alan Riga 552
88 15:20 Practical Polymer Rheology for Quality Control,
Donald E. De Laney and James F. Reilly 553
15:40 Break
89 16:00 A Comparison of Rotational Rheometry andCompressional Rheometry, Peter R. Whittingstall,Russell R. Ulbrich, Bernard Costello and Raoul E.
Smith 558
90 16:20 Rheometry and the Yield Point, Terence E Richards 564
91 16:40 Rheology as a Quality Control Tool, Cesar Gonzalez 571
92 17:00 Advances hi On-line Capillary Rheology, BurkeNelson 572
93 17:20 Practical Applications of Rheology to SolvingProblems in the Coatings Industry, Mark S. Shon 578
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WEDNESDAY MORNING
PLENARY LECTURESavannah C; David Dollimore, Presiding
94 8:00 Application of Thermal Analysis hi Freeze-Dryingof Pharmaceuticals, Steven L. Nail 579
8:40 Break
PHARMACEUTICAL APPLICATIONS OF THERMAL ANALYSISSavannah E; Steven L. Nail, Presiding
95 9:00 The Use of Low Frequency Dielectric Spectroscopyas a Means of Characterising an Amorphous DrugSubstance, Renren He and Duncan Q. M. Craig 580
96 9:20 Hard to Swallow Dry: A New Mechanism forAnhydrous Thermal Decomposition of Aspirin,Nicoleigh Gamble and Charles A. Wight 585
97 9:40 MDSC Study of Melting and Glass Transitions hiElastomeric Dental Impression Materials, JeannieM. Vickery, William A. Brantley, and Thomas A.Bardin 591
98 10:00 Applications of TMDSC in Freeze-Drying ProcessDevelopment, Shawn A. Knopp and Steven L. Nail 597
99 10:20 The Calculation of the Vapor pressures ofAntioxidants Over a Range of Temperatures UsingThermogravimetry, Pauline Phang and DavidDollimore 598
10:40 Break
100 11:00 Calculation of the Vapor Pressure-TemperatureRelationship Using Thermogravimetry for the DrugAllopurinol, Lori Burnham, David Dollimore, andKen Alexander 602
xxiii
101 11:20 A Thermal Analysis Study of the Evaporation ofMethyl Salicylate, Y. H. Cheng, Y. I. Huang, K.Alexander, and David Dollimore 607
102 11:40 The Thermal Analysis Study of the Drug Captopril,Y. I. Huang, Y. Cheng, K. Alexander, and DavidDollimore 612
MODULATED TEMPERATURE PROGRAMS AND THEIRUSE IN TASavannah D; Peter Whittingstall, Presiding
103 9:00 Thermal Analysis of Freeze Dried Formulations,Vicky L. Kett, Duncan Q. M. Craig, and D. Deutsch 618
104 9:20 The Origin of Multiple Glass Transitions in FrozenAqueous Solutions, Liu-Quan Chang, Xiao-Lin Tang,Michael J. Pikal, Nate Milton, and Leonard Thomas 624
105 9:40 Characterization of a Partially Amorphous DrugSubstance Using Temperature Modulated DSC andMicrothermal Analysis, Paul G. Royall, and DuncanQ. M. Craig 629
106 10:00 Freeze-Drying Modeled By MDSC®, Steven R.Aubuchon and Leonard C. Thomas 634
10:20 Break
107 10:40 Gelation, Vitrification, and the Autoacceleration orGel Effect During the Cure of an UnsaturatedPolyester Resin, Guy Van Assche, Els Verdonck, andBruno Van Mele 640
108 11:00 The Measurement of Tg in Ambient CureThermoset Coatings Using Modulated DSC, BruceL. Neff and Robert J. Barsotti 646
109 11:20 Utility of Modulated DSC® hi Monitoring Solvent-Based Coating Cure, Leonard C. Thomas, and StevenR. Aubuchon 652
110 11:40 Advantages of MDSC® Versus DSC for Analysis ofPolymer Blends, P. Whittingstall and S.R. Aubuchon 657
xxiv
TUTORIAL SESSIONOglethorpe A-B; Keith Kociba, Presiding
Tl 9:00 Introduction to ASTM Methods, Alan Riga
T2 9:20 Introduction to Thermal Analysis, Vijay Reddy
T3 9:40 DTA/DSC, Bill Sichina
10:00 Break
T4 10:20 TG, TG/DTA, TG/EGA, Mark Kelsey
T5 10:40 TMA/Dilatometry, Jack Henderson or ErwinKaisersberger
T6 11:00 DMA, Kathy Lavanga
T7 11:20 DEA/TSC, Dave Shepherd
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WEDNESDAY AFTERNOON
PHARMACEUTICAL APPLICATIONS OF THERMAL ANALYSISSavannah E; Steven L. Nail, Presiding
111 13:30 A Thermal Analysis Study of Myristic Acid, LiShen, K. S. Alexander, and David Dollimore 663
112 13:50 Phase Diagram from the Mixtures of Ibuprofen andStearic Acid, Supaporn Lerdkanchanaporn and DavidDollimore 669
113 14:10 Use of DSC for Study of the Complex SettingReaction and Microstructural Stability of aGallium-Based Dental Alloy, Randa E. Shaker,William A. Brantley, Qiang Wu, and Bill M .Culbertson 677
114 14:30 Thermally Stimulated Currents of PharmaceuticalProducts, Marc Galop and George L. Collins 683
14:50 Break
SURFACE CHARACTERIZATIONB Y THERMAL ANALYSIS TECHNIQUES
Savannah E; Alan Riga, Presiding
115 15:10 Problem Solving with Micro-Thermal Analysis,Duncan M . Price, Mike Reading, and Trevor J. Lever 689
116 15:30 Generalised and Localized Heating in Micro-Thermal Analysis, Mike Reading, Duncan M . Price,and Trevor J. Lever 690
117 15:50 Micro Thermal Analysis Calibration, Repeatabilityand Reproducibility, Roger L. Blaine, C. GraySlough, and Duncan M . Price *>91
118 16:10 The Application of Micro-TA Technique hi theUniformity of Polymer Blend, Jiemin Liu, Wei Xie,Charles W. M . Lee, and Wei-Ping Pan 697
XXVI
119 16:30 The Study of Compatibilizing Effect of BlockCopolymer hi PE/PS Blend Using Micro-TATechnique, Jiemin Liu, Wei Xie, Charles W. M. Lee,and Wei-Ping Pan 702
120 16:50 Surface and Solution Properties ofOrganophosphorus Chemicals and PerformanceRelationships hi Wear Tests, Alan Riga and W. RockPistillo 708
MODULATED TEMPERATURE PROGRAMSAND THEIR USE IN TA
Savannah D; Peter Whittingstall, Presiding
121 13:30 Invited Lecture: MTDSC What It Is, What Is Isn't,What It Can Do, and What It Can't Do, MikeReading (invited speaker) 714
122 14:10 An Examination of Experimental Conditions forModulated Temperature TMA, Jonathon Foreman,Blaine Weddle, and Rudolf Riesen 715
123 14:30 Verification of Crystallization and CrystalPerfection Processes Seen hi the MDSC®Nonreversing Signal, Len Thomas and Steven R.Aubuchon 718
124 14:50 Why Separation of the Total Signal into theReversing and Nonreversing Signals During MeltingChanges with Experimental Conditions, Steven R.Aubuchon and Leonard C. Thomas 724
15:10 Break
125 15:30 Considerations of the 2nd and 3rd Laws ofThermodynamics with Regard to TMDSCMeasurements hi the Melting Regions, WilliamSichina 730
126 15:50 A Study of Enthalpic Relaxation of Poly(EthyIeneTerephthalate) by Conventional and ModulatedTemperature Differential Scanning Calorimetry,Nicola A. Bailey, James N. Hay, and Duncan M. Price 731
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127 16:10 Characterization of the Glassy Behavior of aGround Drug Using Temperature Modulated DSC,John Murphy, Duncan Q. M. Craig, Attia Hasnain,and Murti Vemuri 737
128 16:30 Increased Understanding of the Modulated HeatFlow Signal During Polymer Melting, Peter R.Whittingstall and Leonard Thomas 743
APPLICATIONS OF THERMAL ANALYSIS TO FD3ERS ANDFILMS, ELASTOMERS, COMPOSITE AND COATINGS
Oglethorpe A-B; Rita Buehner, Presiding
129 13:30 Orientation Specific Thermal Properties ofPolyimide Film, Robert J. Samuels and Nancy E.Mathis 749
130 13:50 The Utility of Kinetic Analysis hi the Determinationof Reaction Mechanism, Bob A. Howell 755
131 14:10 Accurate Temperature Calibration of Film andFiber Measurements by TMA/SDTA, Rudolf Riesen,Markus Schubnell, and Jonathon Foreman 756
132 14:30 Effects of Temperature, Pressure, and Aging on thePolymer Transitions of Plastic Bonded Explosives,Mary S. Campbell and Danielle A. Garcia 762
133 14:50 New Instrument for Thermal Management Design,Nancy E. Mathis
768134 15:50 Characterization of Polymer Coatings on Silicon
Wafers by Using TG/FTIR/MS, Dun Chen and DavidMcMorran 774
15:30 Break
135 15:10 Optimizing Cure of UV Powder Coatings UsingDifferential Photocalorimetry (DPC), Sanjay Padakiand Rita W. Buehner 775
xxviii
136 16:10 Eliminating Density and Heat CapacityRequirements in Transient Thermal ConductivityMeasurements, Nancy E. Mathis 782
137 16:30 Thermal Conductivity Homogeneity andTopography Characterization, Nancy E. Mathis andMiksa DeSorgo 788
138 16:50 Fiber Distortion of Thick Tapered CompositeStructure, Stanley J. Ng, Steve J. Claus, and Fred E.Arnold 794