Heat transfer errors in quantitative differential thermal analysis |
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Authors: | V V Vaidya P S Nicholson |
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Institution: | (1) Department of Metallurgy and Materials Science, McMaster University, Hamilton, Ontario, Canada |
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Abstract: | A DTA apparatus has been built to examine some of the errors neglected in present quantitative DTA. The heat transfer characteristics within DTA systems were found to limit in situ measurements of powder thermal conductivity. It was also demonstrated that the negligence of heat lost to the DTA block from the sample cell during an exothermic reaction and heat gained from the DTA block by the sample cell during endothermic reactions lead to large errors in quantitative estimations. A modified double differential thermocouple DTA was designed to take these heat losses into account. The apparatus was calibrated with CaCO3 and kaolinite endotherms and the kaolinite exotherm and tested on the SrCO3 rhombic trigonal inversion endotherm. The result was found to be in good agreement with accepted literature values.
Zusammenfassung Ein DTA-Apparatur wurde gebaut um einige in der gegenwärtig üblichen quantitativen DTA vernachlässigte Fehler zu prüfen. Es wurde gefunden, daß die Wärmeübertragungscharakteristika in DTA-Systemen die in situ Messungen der Wärmeleitfähigkeit von Pulvern begrenzen. Es wurde ebenfalls gezeigt, daß die Vernachlässigung von Wärmeverlusten der Probezelle an den DTA-Block bei exothermen Reaktionen und vom Wärmegewinn der Probezelle vom DTA-Block bei endothermen Reaktionen zu bedeutenden Fehlern in den quantitativen Bestimmungen führt. Ein DTA-Gerät mit doppeltem Differentialthermoelement wurde entworfen um diese Wärmeverluste zu berücksichtigen. Der Apparat wurde mittels der endothermen Reaktionen von CaCO3 und Kaolinit, bzw. mittels der exothermen Reaktion von Kaolinit geeicht und an der Inversion von rhombischem zu trigonalem SrCO3 erprobt.
Résumé On a réalisé un appareil ATD pour étudier certaines erreurs négligées jusqu'à présent en ATD quantitative. On a trouvé ainsi que les caractéristiques du transfert de chaleur limitent la mesure in situ de la conductivité thermique des poudres. On montre également que le fait de négliger les échanges de chaleur entre la cellule renfermant l'échantillon et le bloc ATD (pertes ou gains de chaleur suivant que les réactions sont exothermiques ou endothermiques) conduit à des erreurs considérables dans les dosages. Un double thermocouple différentiel a été conçu pour tenir compte de ces pertes. L'étalonnage de l'appareil a été ré alisé à l'aide des réactions endothermiques de CaCO3 et de la kaolinite et contrôlé avec la transition endothermique de SrCO3 (rhomboédrique-trigonal).
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![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![ncy](/content/n8g572xl07628773/xxlarge1085.gif) ![kcy](/content/n8g572xl07628773/xxlarge1082.gif) ![acy](/content/n8g572xl07628773/xxlarge1072.gif) . ![Icy](/content/n8g572xl07628773/xxlarge1048.gif) ![scy](/content/n8g572xl07628773/xxlarge1089.gif) ![pcy](/content/n8g572xl07628773/xxlarge1087.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![lcy](/content/n8g572xl07628773/xxlarge1083.gif) ![softcy](/content/n8g572xl07628773/xxlarge1100.gif) ![zcy](/content/n8g572xl07628773/xxlarge1079.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![vcy](/content/n8g572xl07628773/xxlarge1074.gif) ![acy](/content/n8g572xl07628773/xxlarge1072.gif) ![dcy](/content/n8g572xl07628773/xxlarge1076.gif) ![vcy](/content/n8g572xl07628773/xxlarge1074.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![jcy](/content/n8g572xl07628773/xxlarge1081.gif) ![ncy](/content/n8g572xl07628773/xxlarge1085.gif) 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![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) ![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![ncy](/content/n8g572xl07628773/xxlarge1085.gif) ![tscy](/content/n8g572xl07628773/xxlarge1094.gif) ![icy](/content/n8g572xl07628773/xxlarge1080.gif) ![acy](/content/n8g572xl07628773/xxlarge1072.gif) ![lcy](/content/n8g572xl07628773/xxlarge1083.gif) ![ncy](/content/n8g572xl07628773/xxlarge1085.gif) ![acy](/content/n8g572xl07628773/xxlarge1072.gif) ![tcy](/content/n8g572xl07628773/xxlarge1090.gif) ![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) ![mcy](/content/n8g572xl07628773/xxlarge1084.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![pcy](/content/n8g572xl07628773/xxlarge1087.gif) ![acy](/content/n8g572xl07628773/xxlarge1072.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) , ![pcy](/content/n8g572xl07628773/xxlarge1087.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![zcy](/content/n8g572xl07628773/xxlarge1079.gif) ![vcy](/content/n8g572xl07628773/xxlarge1074.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![lcy](/content/n8g572xl07628773/xxlarge1083.gif) ![yacy](/content/n8g572xl07628773/xxlarge1103.gif) ![yucy](/content/n8g572xl07628773/xxlarge1102.gif) ![acy](/content/n8g572xl07628773/xxlarge1072.gif) ![ucy](/content/n8g572xl07628773/xxlarge1091.gif) ![chcy](/content/n8g572xl07628773/xxlarge1095.gif) ![icy](/content/n8g572xl07628773/xxlarge1080.gif) ![tcy](/content/n8g572xl07628773/xxlarge1090.gif) ![ycy](/content/n8g572xl07628773/xxlarge1099.gif) ![vcy](/content/n8g572xl07628773/xxlarge1074.gif) ![acy](/content/n8g572xl07628773/xxlarge1072.gif) ![tcy](/content/n8g572xl07628773/xxlarge1090.gif) ![ecy](/content/n8g572xl07628773/xxlarge1101.gif) ![tcy](/content/n8g572xl07628773/xxlarge1090.gif) ![tcy](/content/n8g572xl07628773/xxlarge1090.gif) ![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![pcy](/content/n8g572xl07628773/xxlarge1087.gif) ![lcy](/content/n8g572xl07628773/xxlarge1083.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![pcy](/content/n8g572xl07628773/xxlarge1087.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![tcy](/content/n8g572xl07628773/xxlarge1090.gif) ![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) . ![Pcy](/content/n8g572xl07628773/xxlarge1055.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) ![icy](/content/n8g572xl07628773/xxlarge1080.gif) ![bcy](/content/n8g572xl07628773/xxlarge1073.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![acy](/content/n8g572xl07628773/xxlarge1072.gif) ![lcy](/content/n8g572xl07628773/xxlarge1083.gif) ![icy](/content/n8g572xl07628773/xxlarge1080.gif) ![bcy](/content/n8g572xl07628773/xxlarge1073.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![vcy](/content/n8g572xl07628773/xxlarge1074.gif) ![acy](/content/n8g572xl07628773/xxlarge1072.gif) CaCO3 ![ecy](/content/n8g572xl07628773/xxlarge1101.gif) ![ncy](/content/n8g572xl07628773/xxlarge1085.gif) ![dcy](/content/n8g572xl07628773/xxlarge1076.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![tcy](/content/n8g572xl07628773/xxlarge1090.gif) ![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![mcy](/content/n8g572xl07628773/xxlarge1084.gif) ![icy](/content/n8g572xl07628773/xxlarge1080.gif) ![kcy](/content/n8g572xl07628773/xxlarge1082.gif) ![acy](/content/n8g572xl07628773/xxlarge1072.gif) ![mcy](/content/n8g572xl07628773/xxlarge1084.gif) ![ecy](/content/n8g572xl07628773/xxlarge1101.gif) ![kcy](/content/n8g572xl07628773/xxlarge1082.gif) ![zcy](/content/n8g572xl07628773/xxlarge1079.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![tcy](/content/n8g572xl07628773/xxlarge1090.gif) ![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) ![mcy](/content/n8g572xl07628773/xxlarge1084.gif) ![icy](/content/n8g572xl07628773/xxlarge1080.gif) ![kcy](/content/n8g572xl07628773/xxlarge1082.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![kcy](/content/n8g572xl07628773/xxlarge1082.gif) ![acy](/content/n8g572xl07628773/xxlarge1072.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![lcy](/content/n8g572xl07628773/xxlarge1083.gif) ![icy](/content/n8g572xl07628773/xxlarge1080.gif) ![icy](/content/n8g572xl07628773/xxlarge1080.gif) ![tcy](/content/n8g572xl07628773/xxlarge1090.gif) ![pcy](/content/n8g572xl07628773/xxlarge1087.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![vcy](/content/n8g572xl07628773/xxlarge1074.gif) ![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) ![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![ncy](/content/n8g572xl07628773/xxlarge1085.gif) ![ecy](/content/n8g572xl07628773/xxlarge1101.gif) ![ncy](/content/n8g572xl07628773/xxlarge1085.gif) ![dcy](/content/n8g572xl07628773/xxlarge1076.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![tcy](/content/n8g572xl07628773/xxlarge1090.gif) ![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) ![icy](/content/n8g572xl07628773/xxlarge1080.gif) ![kcy](/content/n8g572xl07628773/xxlarge1082.gif) ![pcy](/content/n8g572xl07628773/xxlarge1087.gif) ![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) ![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![khcy](/content/n8g572xl07628773/xxlarge1093.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![dcy](/content/n8g572xl07628773/xxlarge1076.gif) ![tcy](/content/n8g572xl07628773/xxlarge1090.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) ![icy](/content/n8g572xl07628773/xxlarge1080.gif) ![gcy](/content/n8g572xl07628773/xxlarge1075.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![ncy](/content/n8g572xl07628773/xxlarge1085.gif) ![lcy](/content/n8g572xl07628773/xxlarge1083.gif) ![softcy](/content/n8g572xl07628773/xxlarge1100.gif) ![ncy](/content/n8g572xl07628773/xxlarge1085.gif) ![ycy](/content/n8g572xl07628773/xxlarge1099.gif) ![rcy](/content/n8g572xl07628773/xxlarge1088.gif) ![ocy](/content/n8g572xl07628773/xxlarge1086.gif) ![mcy](/content/n8g572xl07628773/xxlarge1084.gif) ![bcy](/content/n8g572xl07628773/xxlarge1073.gif) ![icy](/content/n8g572xl07628773/xxlarge1080.gif) ![chcy](/content/n8g572xl07628773/xxlarge1095.gif) ![iecy](/content/n8g572xl07628773/xxlarge1077.gif) ![scy](/content/n8g572xl07628773/xxlarge1089.gif) ![kcy](/content/n8g572xl07628773/xxlarge1082.gif) ![icy](/content/n8g572xl07628773/xxlarge1080.gif) SrCO3.
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