Some experimental aspects of DSC determination of kinetic parameters in thermal decompositions of solids |
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Authors: | G G T Guarini R Spinicci F M Carlini D Donati |
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Institution: | (1) Institute of Physical Chemistry, University of Florence, Italy;(2) c/o Institute of Organic Chemistry, Centro di Studio del C. N. R. sulla Chimica e la Struttura dei Composti Eterociclici e Loro Applicazioni, Florence, Italy |
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Abstract: | Some particular methods of collecting and treating DSC data for the determination of kinetic parameters in thermal decompositions of solids are suggested. These are mainly concerned with an extrapolation method to avoid the effect of the sample mass; with an approximate method to obtain the activation energy and the exponent of the decay-law for runs at constant temperature in which the total area under the thermal curve is not known with accuracy; and with a method to ascertain whether a particular decomposition takes place by a single mechanism or by a sequence of different mechanisms.
Zusammenfassung Einige besondere Methoden der Sammlung und Verarbeitung von DSC-Daten zur Bestimmung kinetischer Parameter bei der thermischen Zersetzung von Festkörpern werden vorgeschlagen. Diese befassen sich hauptsächlich mit einer Extrapolationsmethode um die Wirkung der Einwaage zu vermeiden; mit einer Annäherungsmethode um die Aktivierungsenergie und den Exponenten des Zersetzungsgesetzes von Versuchen bei konstanter Temperatur zu erhalten, bei welchen die Gesamtoberfläche unter der thermischen Kurve nicht genau bekannt ist; und mit einer Methode zur Bestimmung ob eine bestimmte Zersetzung durch einen einzigen Mechanismus oder durch eine Reihenfolge verschiedener Mechanismen herbeigeführt wird.
Résumé On propose quelques méthodes particulières pour rassembler et traiter les données de l'analyse calorimétrique différentielle (DSC) dans le but de déterminer les paramètres cinétiques de la décomposition des corps solides. Ces méthodes comportent surtout une extrapolation afin d'éviter l'influence de la prise d'essai, une approximation afin d'obtenir l'énergie d'activation et l'exposant de la loi de décomposition pour les expériences effectuées à température constante dans lesquelles la surface totale délimitée par la courbe n'est pas connue avec exactitude, et enfin un moyen de s'assurer si une décomposition particulière est due à un seul mécanisme ou à une succession de divers mécanismes.
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![CHcy](/content/g04w1p84tg108743/xxlarge1063.gif) ![Ncy](/content/g04w1p84tg108743/xxlarge1053.gif) ![Ncy](/content/g04w1p84tg108743/xxlarge1053.gif) ![IEcy](/content/g04w1p84tg108743/xxlarge1045.gif) ![Icy](/content/g04w1p84tg108743/xxlarge1048.gif) ![zhcy](/content/g04w1p84tg108743/xxlarge1078.gif) ![Vcy](/content/g04w1p84tg108743/xxlarge1042.gif) ![IEcy](/content/g04w1p84tg108743/xxlarge1045.gif) ![tcy](/content/g04w1p84tg108743/xxlarge1090.gif) ![Ncy](/content/g04w1p84tg108743/xxlarge1053.gif) ; ![Mcy](/content/g04w1p84tg108743/xxlarge1052.gif) ![IEcy](/content/g04w1p84tg108743/xxlarge1045.gif) ![tcy](/content/g04w1p84tg108743/xxlarge1090.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) ![Dcy](/content/g04w1p84tg108743/xxlarge1044.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) , ![Dcy](/content/g04w1p84tg108743/xxlarge1044.gif) ![Acy](/content/g04w1p84tg108743/xxlarge1040.gif) ![Ucy](/content/g04w1p84tg108743/xxlarge1059.gif) ![SHCHcy](/content/g04w1p84tg108743/xxlarge1065.gif) ![Icy](/content/g04w1p84tg108743/xxlarge1048.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) ![zhcy](/content/g04w1p84tg108743/xxlarge1078.gif) ![Mcy](/content/g04w1p84tg108743/xxlarge1052.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) ![zhcy](/content/g04w1p84tg108743/xxlarge1078.gif) ![Ncy](/content/g04w1p84tg108743/xxlarge1053.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) ![scy](/content/g04w1p84tg108743/xxlarge1089.gif) ![tcy](/content/g04w1p84tg108743/xxlarge1090.gif) ![Ucy](/content/g04w1p84tg108743/xxlarge1059.gif) ![scy](/content/g04w1p84tg108743/xxlarge1089.gif) ![tcy](/content/g04w1p84tg108743/xxlarge1090.gif) ![Acy](/content/g04w1p84tg108743/xxlarge1040.gif) ![Ncy](/content/g04w1p84tg108743/xxlarge1053.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) ![Vcy](/content/g04w1p84tg108743/xxlarge1042.gif) ![Icy](/content/g04w1p84tg108743/xxlarge1048.gif) ![tcy](/content/g04w1p84tg108743/xxlarge1090.gif) , ![pcy](/content/g04w1p84tg108743/xxlarge1087.gif) ![Rcy](/content/g04w1p84tg108743/xxlarge1056.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) ![Icy](/content/g04w1p84tg108743/xxlarge1048.gif) ![scy](/content/g04w1p84tg108743/xxlarge1089.gif) ![khcy](/content/g04w1p84tg108743/xxlarge1093.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) ![Icy](/content/g04w1p84tg108743/xxlarge1048.gif) ![lcy](/content/g04w1p84tg108743/xxlarge1083.gif) ![Dcy](/content/g04w1p84tg108743/xxlarge1044.gif) ![Acy](/content/g04w1p84tg108743/xxlarge1040.gif) ![Ncy](/content/g04w1p84tg108743/xxlarge1053.gif) ![Ncy](/content/g04w1p84tg108743/xxlarge1053.gif) ![ycy](/content/g04w1p84tg108743/xxlarge1099.gif) ![Rcy](/content/g04w1p84tg108743/xxlarge1056.gif) ![Acy](/content/g04w1p84tg108743/xxlarge1040.gif) ![scy](/content/g04w1p84tg108743/xxlarge1089.gif) ![pcy](/content/g04w1p84tg108743/xxlarge1087.gif) ![Acy](/content/g04w1p84tg108743/xxlarge1040.gif) ![pcy](/content/g04w1p84tg108743/xxlarge1087.gif) ![pcy](/content/g04w1p84tg108743/xxlarge1087.gif) ![Rcy](/content/g04w1p84tg108743/xxlarge1056.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) ![tcy](/content/g04w1p84tg108743/xxlarge1090.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) ![Mcy](/content/g04w1p84tg108743/xxlarge1052.gif) ![Mcy](/content/g04w1p84tg108743/xxlarge1052.gif) ![IEcy](/content/g04w1p84tg108743/xxlarge1045.gif) ![khcy](/content/g04w1p84tg108743/xxlarge1093.gif) ![Acy](/content/g04w1p84tg108743/xxlarge1040.gif) ![Ncy](/content/g04w1p84tg108743/xxlarge1053.gif) ![Icy](/content/g04w1p84tg108743/xxlarge1048.gif) ![zhcy](/content/g04w1p84tg108743/xxlarge1078.gif) ![Mcy](/content/g04w1p84tg108743/xxlarge1052.gif) ![Icy](/content/g04w1p84tg108743/xxlarge1048.gif) ![lcy](/content/g04w1p84tg108743/xxlarge1083.gif) ![Icy](/content/g04w1p84tg108743/xxlarge1048.gif) ![IEcy](/content/g04w1p84tg108743/xxlarge1045.gif) ![IEcy](/content/g04w1p84tg108743/xxlarge1045.gif) ![Mcy](/content/g04w1p84tg108743/xxlarge1052.gif) ![IEcy](/content/g04w1p84tg108743/xxlarge1045.gif) ![scy](/content/g04w1p84tg108743/xxlarge1089.gif) ![tcy](/content/g04w1p84tg108743/xxlarge1090.gif) ![pcy](/content/g04w1p84tg108743/xxlarge1087.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) ![scy](/content/g04w1p84tg108743/xxlarge1089.gif) ![lcy](/content/g04w1p84tg108743/xxlarge1083.gif) ![IEcy](/content/g04w1p84tg108743/xxlarge1045.gif) ![Dcy](/content/g04w1p84tg108743/xxlarge1044.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) ![Vcy](/content/g04w1p84tg108743/xxlarge1042.gif) ![Acy](/content/g04w1p84tg108743/xxlarge1040.gif) ![tcy](/content/g04w1p84tg108743/xxlarge1090.gif) ![IEcy](/content/g04w1p84tg108743/xxlarge1045.gif) ![lcy](/content/g04w1p84tg108743/xxlarge1083.gif) ![softcy](/content/g04w1p84tg108743/xxlarge1100.gif) ![Ncy](/content/g04w1p84tg108743/xxlarge1053.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) ![scy](/content/g04w1p84tg108743/xxlarge1089.gif) ![tcy](/content/g04w1p84tg108743/xxlarge1090.gif) ![Rcy](/content/g04w1p84tg108743/xxlarge1056.gif) ![Acy](/content/g04w1p84tg108743/xxlarge1040.gif) ![zhcy](/content/g04w1p84tg108743/xxlarge1078.gif) ![lcy](/content/g04w1p84tg108743/xxlarge1083.gif) ![Icy](/content/g04w1p84tg108743/xxlarge1048.gif) ![CHcy](/content/g04w1p84tg108743/xxlarge1063.gif) ![Ncy](/content/g04w1p84tg108743/xxlarge1053.gif) ![ycy](/content/g04w1p84tg108743/xxlarge1099.gif) ![Mcy](/content/g04w1p84tg108743/xxlarge1052.gif) ![IEcy](/content/g04w1p84tg108743/xxlarge1045.gif) ![khcy](/content/g04w1p84tg108743/xxlarge1093.gif) ![Acy](/content/g04w1p84tg108743/xxlarge1040.gif) ![Ncy](/content/g04w1p84tg108743/xxlarge1053.gif) ![Icy](/content/g04w1p84tg108743/xxlarge1048.gif) ![zhcy](/content/g04w1p84tg108743/xxlarge1078.gif) ![Mcy](/content/g04w1p84tg108743/xxlarge1052.gif) ![Ocy](/content/g04w1p84tg108743/xxlarge1054.gif) .
Work supported by the Italian Consiglio Nazionale delle Ricerche (C. N. R.). Contrac No. 71.01589.03. |
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