Thermoanalytical investigations of thallous nitrate |
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Authors: | R P Clark F W Reinhardt |
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Institution: | (1) Sandia Laboratories, 87185 Albuquerque, New Mexico, USA |
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Abstract: | Thallous nitrate was investigated using TG, DTA, and DSC in conjunction with gas chromatography and X-ray diffraction analysis. TG showed a weight loss beginning at 380° with a 50 percent loss by 520°. This weight loss was demonstrated to be caused by boiling rather than thermal decomposition. The DTA extrapolated onset temperature for the boiling was 467°. Two solid-solid transition points and the melting point were determined by DTA to be 77, 145, and 207°, respectively. Heat of transition values determined by DSC were 0.15 kcal/mole at 77°, 0.87 kcal/ mole at 145°, and 2.18 kcal/mole for the melting at 207°.
Zusammenfassung Thallium(I)nitrat wurde mittels TG, DTA und DSC, mit Gaschromatographie und Röntgendiffraktionsanalyse gekoppelt, untersucht. TG zeigte einen beginnenden Gewichtsverlust ab etwa 380° und einen Verlust von 50% bis 520°. Es wurde gezeigt, daß dieser Gewichtsverlust eher vom Sieden als von der thermischen Zersetzung verursacht wird. Die aus DTA-Daten extrapolierte Anfangs-Siedetemperatur war 467°. Die Fest-festphasen Übergangspunkte und der Schmelzpunkt lagen, wie durch DTA ermittelt, bei 77, 145, bzw. 207°. Die mittels DSC bestimmten Wärmen der Übergangswerte betrugen 0.15 kcal/Mol bei 77°, 0.87 kcal/Mol bei 145° und 2.18 kcal/Mol für das Schmelzen bei 207°.
Résumé On a étudié le nitrate de thallium(I) par TG, ATD et DSC conjointement à la Chromatographie en phase gazeuse et à l'analyse par diffraction des rayons X. La TG révèle une perte de masse à partir d'environ 380°, avec une perte de 50 p. c. à 520°. On montre que cette perte de masse est provoquée par l'ébullition plutôt que par la décomposition thermique. La température initiale de l'ébullition, extrapolée à partir des données ATD, est de 467°. Deux points de transition solide-solide ainsi que le point de fusion ont été déterminés par ATD et correspondent aux températures respectives de 77, 145 et 207°. Les valeurs des chaleurs de transition ont été déterminées par DSC: 0.15 kcal, mol–1 à 77°, 0.87 kcal. mol–1 à 145 et 2.18 kcal. mol–1 pour la fusion à 207°.
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![Tcy](/content/j4mm0134q128t865/xxlarge1058.gif) , ![scy](/content/j4mm0134q128t865/xxlarge1089.gif) ![ocy](/content/j4mm0134q128t865/xxlarge1086.gif) ![ocy](/content/j4mm0134q128t865/xxlarge1086.gif) ![tcy](/content/j4mm0134q128t865/xxlarge1090.gif) ![vcy](/content/j4mm0134q128t865/xxlarge1074.gif) ![iecy](/content/j4mm0134q128t865/xxlarge1077.gif) ![tcy](/content/j4mm0134q128t865/xxlarge1090.gif) ![scy](/content/j4mm0134q128t865/xxlarge1089.gif) ![tcy](/content/j4mm0134q128t865/xxlarge1090.gif) ![vcy](/content/j4mm0134q128t865/xxlarge1074.gif) ![iecy](/content/j4mm0134q128t865/xxlarge1077.gif) ![ncy](/content/j4mm0134q128t865/xxlarge1085.gif) ![rcy](/content/j4mm0134q128t865/xxlarge1088.gif) ![acy](/content/j4mm0134q128t865/xxlarge1072.gif) ![vcy](/content/j4mm0134q128t865/xxlarge1074.gif) ![ncy](/content/j4mm0134q128t865/xxlarge1085.gif) 77, 145 207°. ![Zcy](/content/j4mm0134q128t865/xxlarge1047.gif) ![ncy](/content/j4mm0134q128t865/xxlarge1085.gif) ![acy](/content/j4mm0134q128t865/xxlarge1072.gif) ![chcy](/content/j4mm0134q128t865/xxlarge1095.gif) ![iecy](/content/j4mm0134q128t865/xxlarge1077.gif) ![ncy](/content/j4mm0134q128t865/xxlarge1085.gif) ![icy](/content/j4mm0134q128t865/xxlarge1080.gif) ![tcy](/content/j4mm0134q128t865/xxlarge1090.gif) ![iecy](/content/j4mm0134q128t865/xxlarge1077.gif) ![pcy](/content/j4mm0134q128t865/xxlarge1087.gif) ![lcy](/content/j4mm0134q128t865/xxlarge1083.gif) ![ocy](/content/j4mm0134q128t865/xxlarge1086.gif) ![pcy](/content/j4mm0134q128t865/xxlarge1087.gif) ![iecy](/content/j4mm0134q128t865/xxlarge1077.gif) ![rcy](/content/j4mm0134q128t865/xxlarge1088.gif) ![iecy](/content/j4mm0134q128t865/xxlarge1077.gif) ![khcy](/content/j4mm0134q128t865/xxlarge1093.gif) ![ocy](/content/j4mm0134q128t865/xxlarge1086.gif) ![dcy](/content/j4mm0134q128t865/xxlarge1076.gif) , ![ocy](/content/j4mm0134q128t865/xxlarge1086.gif) ![pcy](/content/j4mm0134q128t865/xxlarge1087.gif) ![rcy](/content/j4mm0134q128t865/xxlarge1088.gif) ![dcy](/content/j4mm0134q128t865/xxlarge1076.gif) ![iecy](/content/j4mm0134q128t865/xxlarge1077.gif) ![lcy](/content/j4mm0134q128t865/xxlarge1083.gif) ![iecy](/content/j4mm0134q128t865/xxlarge1077.gif) ![ncy](/content/j4mm0134q128t865/xxlarge1085.gif) ![ncy](/content/j4mm0134q128t865/xxlarge1085.gif) ![ycy](/content/j4mm0134q128t865/xxlarge1099.gif) ![pcy](/content/j4mm0134q128t865/xxlarge1087.gif) ![ocy](/content/j4mm0134q128t865/xxlarge1086.gif) ![mcy](/content/j4mm0134q128t865/xxlarge1084.gif) ![ocy](/content/j4mm0134q128t865/xxlarge1086.gif) ![shchcy](/content/j4mm0134q128t865/xxlarge1097.gif) ![softcy](/content/j4mm0134q128t865/xxlarge1100.gif) ![Dcy](/content/j4mm0134q128t865/xxlarge1044.gif) , ![scy](/content/j4mm0134q128t865/xxlarge1089.gif) ![ocy](/content/j4mm0134q128t865/xxlarge1086.gif) ![ocy](/content/j4mm0134q128t865/xxlarge1086.gif) ![tcy](/content/j4mm0134q128t865/xxlarge1090.gif) ![vcy](/content/j4mm0134q128t865/xxlarge1074.gif) ![iecy](/content/j4mm0134q128t865/xxlarge1077.gif) ![tcy](/content/j4mm0134q128t865/xxlarge1090.gif) ![scy](/content/j4mm0134q128t865/xxlarge1089.gif) ![tcy](/content/j4mm0134q128t865/xxlarge1090.gif) ![vcy](/content/j4mm0134q128t865/xxlarge1074.gif) ![iecy](/content/j4mm0134q128t865/xxlarge1077.gif) ![ncy](/content/j4mm0134q128t865/xxlarge1085.gif) ![ncy](/content/j4mm0134q128t865/xxlarge1085.gif) ![rcy](/content/j4mm0134q128t865/xxlarge1088.gif) ![acy](/content/j4mm0134q128t865/xxlarge1072.gif) ![vcy](/content/j4mm0134q128t865/xxlarge1074.gif) 0.15 ![kcy](/content/j4mm0134q128t865/xxlarge1082.gif) ![kcy](/content/j4mm0134q128t865/xxlarge1082.gif) ![acy](/content/j4mm0134q128t865/xxlarge1072.gif) /![mcy](/content/j4mm0134q128t865/xxlarge1084.gif) ![ocy](/content/j4mm0134q128t865/xxlarge1086.gif) ![lcy](/content/j4mm0134q128t865/xxlarge1083.gif) ![pcy](/content/j4mm0134q128t865/xxlarge1087.gif) ![rcy](/content/j4mm0134q128t865/xxlarge1088.gif) 77°, 0,87 ![kcy](/content/j4mm0134q128t865/xxlarge1082.gif) ![kcy](/content/j4mm0134q128t865/xxlarge1082.gif) ![acy](/content/j4mm0134q128t865/xxlarge1072.gif) /![mcy](/content/j4mm0134q128t865/xxlarge1084.gif) ![ocy](/content/j4mm0134q128t865/xxlarge1086.gif) ![lcy](/content/j4mm0134q128t865/xxlarge1083.gif) ![pcy](/content/j4mm0134q128t865/xxlarge1087.gif) ![rcy](/content/j4mm0134q128t865/xxlarge1088.gif) 145° 2.18 ![kcy](/content/j4mm0134q128t865/xxlarge1082.gif) ![acy](/content/j4mm0134q128t865/xxlarge1072.gif) /![mcy](/content/j4mm0134q128t865/xxlarge1084.gif) ![ocy](/content/j4mm0134q128t865/xxlarge1086.gif) ![lcy](/content/j4mm0134q128t865/xxlarge1083.gif) ![dcy](/content/j4mm0134q128t865/xxlarge1076.gif) ![lcy](/content/j4mm0134q128t865/xxlarge1083.gif) ![pcy](/content/j4mm0134q128t865/xxlarge1087.gif) ![lcy](/content/j4mm0134q128t865/xxlarge1083.gif) ![acy](/content/j4mm0134q128t865/xxlarge1072.gif) ![vcy](/content/j4mm0134q128t865/xxlarge1074.gif) ![lcy](/content/j4mm0134q128t865/xxlarge1083.gif) ![iecy](/content/j4mm0134q128t865/xxlarge1077.gif) ![ncy](/content/j4mm0134q128t865/xxlarge1085.gif) ![icy](/content/j4mm0134q128t865/xxlarge1080.gif) ![pcy](/content/j4mm0134q128t865/xxlarge1087.gif) ![rcy](/content/j4mm0134q128t865/xxlarge1088.gif) 207°.
The authors thank F. J. Conrad and W. J. Andrzejewski for gas analysis results and G. T. Gay for X-ray diffraction analyses.This work was supported by the United States Department of Energy. |
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