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Pulsed bed calorimetry

A jump in speed and sensitivity

Journal of Thermal Analysis and Calorimetry
Authors: S. Walter, A. Hadj Mebarek, and S. Diyani

Abstract  

Conventional calorimetry has always the difficulty of choosing between near to equilibrium working conditions and high thermal ramp rates. Thus, either the transport phenomena and sample homogeneities are good but the signals become weak due to thermal losses, or the signals are sharp, but strong gradients across the sample lead to chemical and thermal heterogeneities. The described pulsed fluidized bed technique, by strongly stirring the sample, allows good sample homogeneities even at high ramp rates. Moreover, the permanently regenerated cover gas allows as well a good heat transfer towards the thermocouples as a constant atmosphere composition leading to very precise onset temperatures.

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Abstract  

Several DTA experiments followed by calorimetric works are reviewed here to emphasise the importance of complementary role of both techniques. The thermal analysis is advantageous in the sense that it gives quickly the overall view of thermal behaviour of a material under various conditions. Calorimetric work provides accurate heat capacity data which enable to derive thermodynamic functions including the enthalpy and entropy. The latter quantity is especially important in judging whether the material obeys the third law of thermodynamics. However, calorimetric work leads occasionally to an erroneous conclusion if the work is not preceded by thermal analysis performed under various conditions. Sometimes, quality of information obtained by DTA exceeds that obtained by laborious calorimetry.

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Abstract  

Polymorphism of trilaurin mixed with 4% of cholesterol was studied with a setup coupling calorimetry and phase characterisation by in-situ X-ray diffraction (Microcalix). Four polymorphic forms were identified. Monotropic and enantiotropic transitions were identified from the reconstruction of Gibbs free energy diagram which allows the control of trilaurin polymorphism.

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Abstract  

Calorimetry deals with the energetics of atoms, molecules, and phases and can be used to gather experimental details about one of the two roots of our knowledge about matter. The other root is structural science. Both are understood from the microscopic to the macroscopic scale, but the effort to learn about calorimetry has lagged behind structural science. Although equilibrium thermodynamics is well known, one has learned in the past little about metastable and unstable states. Similarly, Dalton made early progress to describe phases as aggregates of molecules. The existence of macromolecules that consist of as many atoms as are needed to establish a phase have led, however, to confusion between colloids (collections of microphases) and macromolecules which may participate in several micro- or nanophases. This fact that macromolecules can be as large or larger than phases was first established by Staudinger as late as 1920. Both fields, calorimetry and macromolecular science, found many solutions for the understanding of metastable and unstable states. The learning of modern solutions to the problems of materials characterization by calorimetry is the topic of this paper.

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Abstract  

The paper gives a review on recent progress on new methods, instrumental innovations and new trends in low temperature calorimetry as reported in the last five years in the literature. The paper refers to establishing strictly adiabatic conditions, improved analysis of quasi-adiabatic experiments, high resolution adiabatic and isoperibol scanning calorimeters and microcalorimeters for the study of µ-samples.

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The heat capacityC p of a sample can be considered as a frequency dependent quantity; its behaviour can reflect the dynamics of enthalpy fluctuations. In order to take into account the dynamic nature of the measured quantity, calorimetry can mimic experimental methods as those of dielectrometry, performing experiments in time domain or in frequency domain.

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]. J. Chiu P. G. Fair 1979 Determination of thermal conductivity by differential scanning calorimetry Thermochimica Acta

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References 1 Hemminger , W. and Höhne , G. , Calorimetry , Verlag Chemie , 1984 . 2 Regenass , W

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Abstract  

This paper explains why directly agitated test cells are sometimes required in order to obtain good adiabatic calorimetry data that can be used with confidence to predict large scale plant behaviour. Experiments for methyl methacrylate polymerisation are reported. Simple procedures are presented for calculating genuine thermo-kinetic parameters from data which includes energy dissipation from the stirrer drive system.

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Abstract  

The research in thermal analysis and calorimetry, conducted by the author over the period 1964 to 1993, is summarised and concisely reviewed. The major investigations have focussed on thermal analysis studies of coordination compounds, particularly the metal dithiocarbamate complexes. A significant solution calorimetric study of some metal dithiocarbamate complexes has also been undertaken. DSC has been applied to determine the sublimation enthalpies of many metal dithiocarbamate and metal pentane-2,4-dionate complexes and solution calorimetry has been applied to study the thermochemistry of the latter group of complexes. Thermal analysis investigations of several inorganic molten salt systems have been initiated. Thermometric titrimetry has been applied to study metal-macrocyclic ligand systems in aqueous media and particularly those systems of environmental significance. Temperature calibration standards for TMA have been proposed and TMA has been applied to study the mechanical properties of several common inorganic compounds. DTA has been applied to study a wide variety of phenols and has subsequently been applied as an analytical technique to determine the components of solid state phenol mixtures. Thermometric titrimetry has been applied to determine the phenolic content of wines. A comprehensive thermal analysis study of Australian brown coal has been undertaken, involving the DSC determination of coal specific energy, a TG/DTA study of the coal pyrolysis and combustion processes and a TG/DTA and EGA study of the cation catalytic effect on the coal pyrolysis process. Thermal analysis and calorimetric techniques have been extensively publicised and promoted by the publication of specialist reviews, the presentation of symposia review papers and the oral presentation of short courses, particularly in the SE Asian region. This review essentially reveals the diversity of possible application of thermal analysis and calorimetric techniques and the primary significance of thermodynamic data in the fundamental rationalisation of chemical phenomena.

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