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30 years of research in thermal analysis and calorimetry

A personal review

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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.

Zusammenfassung

Die vom Autor im Zeitraum 1964 bis 1993 geführte Forschungsarbeit im Bereich Thermoanalyse und Kalorimetrie wird zusammengefaßt und kurz rezensiert. Die wichtigsten Forschungsarbeiten konzentrierten sich auf die Untersuchung von Koordinationsverbindungen, im speziellen auf Metalldithiocarbamat-Komplexe. Unter anderem wurde eine bedeutsame Lösungskalorimetrie-Untersuchung von einigen Metalldithiocarbamat-Komplexen durchgeführt. DSC wurde zur Bestimmung der Sublimationsenthalpien vieler Metalldithiocarbamate und Metallpentan-2,4-dionatkomplexe und Lösungskalorimetrie zur Untersuchung der Thermochemie der letzteren Komplexgruppe eingesetzt. Thermoanalytische Untersuchungen einiger anorganischer geschmolzener Salzsysteme wurden initiiert. Thermometrische Titrimetrie wurde zur Untersuchung metallmakrocyclischer Ligandensysteme in wäßrigem Milieu angewendet, insbesondere an Systemen mit Bedeutung für die Umwelt. Es wurden Temeperaturkalibrierungsstandards für TMA vorgeschlagen und TMA zur Untersuchung mechanischer Eigenschaften einiger gewöhnlicher anorganischer Verbindungen eingesetzt. DTA wurde zur Untersuchung eines breiten Kreises von Phenolen und anschließend als eine Analysetechnik zur Bestimmung der Komponenten von Phenolgemischen im festen Zustand eingesetzt. Thermometrische Titrimetrie wurde zur Bestimmung des Phenolgehaltes von Weinsorten angewendet. Es wurde eine umfassende thermoanalytische Untersuchung australischer Braunkohle unternommen, einschließlich der DSC-Bestimmung der spezifischen Energie der Kohle, einer TG/DTA-Untersuchung der Kohlepyrolyse- und Verbrennungsprozesse sowie einer TG/DTA- und EGA-Untersuchung das kationischen Katalyseeffektes auf Kohlepyrolyseprozesse. Durch die Veröffentlichung von Spezialisten-Rezensionen, die Präsentation von Symposien-Rezensionen und die mündliche Präsentation von Kurzkursen, insbesondere in der Südostasienregion wurden thermoanalytische und kalorimetrische Techniken ausführlich publiziert und gefördert. Vorliegende Arbeit bringt insbesondere die Verschiedenartigkeit von möglichen Anwendungen der Thermoanalyse und der kalorimetrischen Techniken und die erstrangige Bedeutung thermodynamischer Daten für eine grundlegenden Rationalisierung chemischer Erscheinungen zum Ausdruck.

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Hill, J.O. 30 years of research in thermal analysis and calorimetry. Journal of Thermal Analysis 42, 607–621 (1994). https://doi.org/10.1007/BF02548538

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