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MTDSC provides a step-change increase in the power of calorimetry to characterize virtually all polymer systems including curing systems, blends and semicrystalline polymers. It enables hidden transitions to be revealed, miscibility to be accurately assessed, and phases and interfaces in complex blends to be quantified. It also enables crystallinity in complex systems to be measured and provides new insights into melting behaviour. All of this is achieved by a simple modification of conventional DSC. In 1992 a new calorimetric technique was introduced that superimposed a small modulation on top of the conventional linear temperature program typically used in differential scanning calorimetry. This was combined with a method of data analysis that enabled the sample’s response to the linear component of the temperature program to be separated from its response to the periodic component. In this way, for the first time, a signal equivalent to that of conventional DSC was obtained simultaneously with a measure of the sample’s heat capacity from the modulation. The new information this provided sparked a revolution in scanning calorimetry by enabling new insights to be gained into almost all aspects of polymer characteristics. This book provides both a basic and advanced treatment of the theory of the technique followed by a detailed exposition of its application to reacting systems, blends and semicrystalline polymers by the leaders in all of these fields. It is an essential text for anybody interested in calorimetry or polymer characterization, especially if they have found that conventional DSC cannot help them with their problems.
MTDSC provides a step-change increase in the power of calorimetry to characterize virtually all polymer systems including curing systems, blends and semicrystalline polymers. It enables hidden transitions to be revealed, miscibility to be accurately assessed, and phases and interfaces in complex blends to be quantified. It also enables crystallinity in complex systems to be measured and provides new insights into melting behaviour. All of this is achieved by a simple modification of conventional DSC. In 1992 a new calorimetric technique was introduced that superimposed a small modulation on top of the conventional linear temperature program typically used in differential scanning calorimetry. This was combined with a method of data analysis that enabled the sample’s response to the linear component of the temperature program to be separated from its response to the periodic component. In this way, for the first time, a signal equivalent to that of conventional DSC was obtained simultaneously with a measure of the sample’s heat capacity from the modulation. The new information this provided sparked a revolution in scanning calorimetry by enabling new insights to be gained into almost all aspects of polymer characteristics. This book provides both a basic and advanced treatment of the theory of the technique followed by a detailed exposition of its application to reacting systems, blends and semicrystalline polymers by the leaders in all of these fields. It is an essential text for anybody interested in calorimetry or polymer characterization, especially if they have found that conventional DSC cannot help them with their problems.
Presents a solid introduction to thermal analysis, methods, instrumentation, calibration, and application along with the necessary theoretical background. Useful to chemists, physicists, materials scientists, and engineers who are new to thermal analysis techniques, and to existing users of thermal analysis who wish expand their experience to new techniques and applications Topics covered include Differential Scanning Calorimetry and Differential Thermal Analysis (DSC/DTA), Thermogravimetry, Thermomechanical Analysis and Dilatometry, Dynamic Mechanical Analysis, Micro-Thermal Analysis, Hot Stage Microscopy, and Instrumentation. Written by experts in the various areas of thermal analysis Relevant and detailed experiments and examples follow each chapter.
An all-in-one reference work covering the essential principles and techniques on thermal behavior and response of polymeric materials This book delivers a detailed understanding of the thermal behavior of polymeric materials evaluated by thermal analysis methods. It covers the most widely applied principles which are used in method development to substantiate what happens upon heating of polymers. It also reviews the key application areas of polymers in materials science. Edited by two experts in the field, the book covers a wide range of specific topics within the aforementioned categories of discussion, such as: Crucial thermal phenomena - glass transition, crystallization behavior and curing kinetics Polymeric materials that have gained considerable interest over the last decade The latest advancements in techniques related to the field, such as modulated temperature DSC and fast scanning calorimetry The recent advances in hyphenated techniques and their applications Polymer chemists, chemical engineers, materials scientists, and process engineers can use this comprehensive reference work to gain clarity on the topics discussed within and learn how to harness them in practical applications across a wide range of disciplines.
In this fully updated and revised second edition the authors provide the newcomer and the experienced practitioner with a balanced and comprehensive insight into all important DSC methods, including a sound presentation of the theoretical basis of DSC and TMDSC measurements. Emphasis is layed on instrumentation, the underlying measurement principles, metrologically correct calibrations, factors influencing the measurement process, and on the exact interpretation of the results. The information given enables the research scientist, the analyst and experienced laboratory staff to apply DSC methods successfully and to measure respective properties correctly.
Table of Contents Table of Contents 1 Atoms, small, and large molecules 2 Basics of thermal analysis 3 Dynamics of chemical and phase changes 4 Thermal analysis tools 5 Structure and properties of materials 6 Single component materials 7 Multiple component materials App. A.1 Table of thermal properties of linear macromolecules and related small molecules - the ATHAS data bank App. A.2 Radiation scattering App. A.3 Derivation of the Rayleigh ratio App. A.4 Neural network predictions App. A.5 Legendre transformations, Maxwell relations, linking of entropy and probability, and derivation of (dS/dT) App. A.6 Boltzmann distribution, harmonic vibration, complex numbers, and normal modes App. A.7 Summary of the basic kinetics of chemical reactions App. A.8 The ITS 1990 and the Krypton-86 length standard App. A.9 Development of classical DTA to DSC App. A.10 Examples of DTA and DSC under extreme conditions App. A.11 Description of an online correction of the heat-flow rate App. A.12 Derivation of the heat-flow equations App. A.13 Description of sawtooth-modulation response App. A.14 An introduction to group theory, definitions of configurations and conformations, and a summary of rational and irrational numbers App. A.15 Summary of birefringence and polarizing microscopy App. A.16 Summary of X-ray diffraction and interference effects App. A.17 Optical analog of electron double diffraction to produce Moire patterns.
Thermal Characterization of Polymeric Materials is a critical review and a concise evaluation of the application of thermal analysis in polymer science and engineering. This book is divided into nine chapters that specifically tackle the instrumentation, theory, and a wide variety of applications of thermal characterization. The introductory chapters provide an overview of all aspects of thermal analytical methods and apparatus and the theory underlying the basic principles of thermal analysis. These chapters also examine the theories and functions of state for thermometry, dilatometry, thermomechanical analysis, calorimetry, thermogravimetry. These topics are followed by a discussion on single-component and multicomponent systems and their phase transitions, as influenced by concentration, pressure, deformation, molecular weight, and copolymerization. The subsequent chapters explore the influence of important chemical and physical parameters on the glass transition, crystallization, and melting of thermoplastic materials. The discussion then shifts to the theoretical aspects of polymer-polymer compatibility, phase separation, and miscibility in mixed polymer systems. This book further considers the thermal analysis in thermosets, elastomers, and fibers. The concluding chapters present the methods of obtaining information on the relative flammability properties of polymers, for screening fire retardant additives, and for studying the mechanism of flame inhibition. These chapters also look into the thermal analysis of antioxidants, stabilizers, lubricants, plasticizers, impact modifiers, and fire retardants. Polymer scientists and researchers will find this book invaluable.
In recent years, multicomponent polymers have generated much interest due to their excellent properties, unique morphology and high-end applications. Book focusses on thermal, thermo-mechanical and dielectric analysis of polymers and multicomponent polymeric systems like blends, interpenetrating polymeric networks (IPNs), gels, polymer composites, nanocomposites. Through these analyses, it provides an insight into the stability of polymer systems as a function of time, processing and usage. Aimed at polymer chemists, physicists and engineers, it also covers ASTM /ISO and other standards of various measurement techniques for systematic analysis in materials science.
Temperature-modulated differential scanning calorimetry (TMDSC) generated with a centrosymmetric saw-tooth oscillation can be considered to be a sinusoidal modulation with multiple frequencies. Different harmonics of the Fourier series of the heat-flow rate and heating rate of a single sawtooth-modulation can be deconvoluted to extract data pertaining to different frequencies. In order to give the higher harmonics similar amplitudes, a complex, but simple-to-program, sawtooth-modulation is generated for the harmonics 1,3,5,7 and 9. In this fashion a single experiment can produce a frequency-dependent analysis under identical thermal history. Application of this method to TMDSC includes the calibration for heat capacity determination of high precision, even if steady state and a negligible temperature gradient are not achieved. The measurement of the frequency (?) dependence of the heat-flow rate (AHF) and sample temperature (ATs) allows to evaluate the expression: CP=AHF/(ATs??)[1+(???)2]0.5 where the relaxation time ? is to be determined empirically from the multiple data generated by the single run. Typical values for the relaxation time for commercial calorimeters are between 3 and 9 s rad-1. Frequency-dependent, apparent reversing heat capacities in the glass transition region and within first-order transition regions may also be analyzed to study local equilibria in globally metastable polymeric solids.