Apport de l'analyse thermique differentielle quantitative a l'etude du polymorphisme du nitrate de potassium a la pression atmospherique |
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Authors: | M Harmelin |
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Institution: | (1) Laboratoire de Recherches Microanalytiques du C. N. R. S., Paris, France;(2) Present address: Centre d'Etudes de Chimie Métallurgique du C. N. R. S., 15, rue Georges-Urbain, 94 Vitry-sur-Seine |
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Abstract: | Résumé Application de l'ATD quantitative à l'étude des transformations structurales du nitrate de potassium. Les échantillons (1 à 8 mg) sont chauffés et refroidis dans l'azote sec, à la pression atmosphérique. Au refroidissement, on observe toujours les transitions successives I III II. Le pic exothermique correspondant à I III apparaît dans un intervalle de température très reproductible (118 – 120°). Les mesures de surface confirment la parfaite réversibilité de I III déjà signalée par C. Mazières. Les transitions III I et II I ont lieu pratiquement à la même température (127–130°) mais l'aire du pic endothermique correspondant à III I est plus faible et représente 51.5 % de la valeur observée pour II I. En prenant H=13.2 cal/g comme valeur de référence pour la transition II I, on trouve H=6.8± 0.2 cal/g pour III I. La transformation III II suit un processus en deux étapes, fortement influencé par le traitement thermique antérieur de la phase I.
The changes in the structure of potassium nitrate have been studied by differential thermal analysis. The samples were heated and cooled in a stream of dry nitrogen, at atmospheric pressure. On cooling, the following transformations have been observed: I III II. The exothermic peak corresponding to the I III transformation appeared at 118–120° with good reproducibility. Surface area measurements show the complete reversibility already observed by Mazières for the I III transformation. The III I and the II I processes take place at the same temperature (127–130°), but the peak corresponding to the III I change is of lower intensity, representing only 51.5% of that of the peak belonging to the II I transition. If the enthalpy change belonging to process II I, H=13.2 cal/g, that belonging to transition III I, H=6.8±0.2 cal/g. Transformation III II proceeds in two steps and is greatly influenced by the preceding heat treatment of phase I.
Zusammenfassung Quantitative Differentialthermoanalyse wurde zur Untersuchung der strukturellen Umwandlungen von Kaliumnitrat herangezogen. Die Proben (1–8 mg) wurden in trockenem Stickstoff bei atmosphärischem Druck erhitzt und abgekühlt. Beim Abkühlen lassen sich immer die sukzessiven Umwandlungen I III II beobachten. Die dem Übergang I III entsprechende exothermische Spitze erscheint sehr reproduzierbar bei 118–120°. Die Oberflächenmessungen bezeugen die vollständige Reversibilität von I III, schon früher angegeben von Mazières. Die Übergänge III I und II I erfolgen praktisch bei gleicher Temperatur (127–130°), doch die endothermische Spitze von III I ist schwächer und entspricht nur 51.5% des für II I beobachteten Wertes. H=13.2 cal/g als Referenzwert für Übergang II I genommen, ergibt sich H=6.8±0.2 cal/g für III I. III II Übergang verläuft in zwei Schritten, die durch das thermische Vorleben der Phase I stark beeinflußt sind.
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![zcy](/content/v00646315m763300/xxlarge1079.gif) ![mcy](/content/v00646315m763300/xxlarge1084.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![ncy](/content/v00646315m763300/xxlarge1085.gif) ![icy](/content/v00646315m763300/xxlarge1080.gif) ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![vcy](/content/v00646315m763300/xxlarge1074.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![khcy](/content/v00646315m763300/xxlarge1093.gif) ![ncy](/content/v00646315m763300/xxlarge1085.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) 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![mcy](/content/v00646315m763300/xxlarge1084.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) , ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![dcy](/content/v00646315m763300/xxlarge1076.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![kcy](/content/v00646315m763300/xxlarge1082.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) ![zcy](/content/v00646315m763300/xxlarge1079.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) ![ncy](/content/v00646315m763300/xxlarge1085.gif) ![ncy](/content/v00646315m763300/xxlarge1085.gif) ![ucy](/content/v00646315m763300/xxlarge1091.gif) ![Mcy](/content/v00646315m763300/xxlarge1052.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) ![zcy](/content/v00646315m763300/xxlarge1079.gif) ![icy](/content/v00646315m763300/xxlarge1080.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![khcy](/content/v00646315m763300/xxlarge1093.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![dcy](/content/v00646315m763300/xxlarge1076.gif) I III. ![Pcy](/content/v00646315m763300/xxlarge1055.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![khcy](/content/v00646315m763300/xxlarge1093.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![dcy](/content/v00646315m763300/xxlarge1076.gif) III I II I ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![icy](/content/v00646315m763300/xxlarge1080.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![khcy](/content/v00646315m763300/xxlarge1093.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![dcy](/content/v00646315m763300/xxlarge1076.gif) ![yacy](/content/v00646315m763300/xxlarge1103.gif) ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) ![kcy](/content/v00646315m763300/xxlarge1082.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![icy](/content/v00646315m763300/xxlarge1080.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![kcy](/content/v00646315m763300/xxlarge1082.gif) ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![zhcy](/content/v00646315m763300/xxlarge1078.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) ![mcy](/content/v00646315m763300/xxlarge1084.gif) ![ycy](/content/v00646315m763300/xxlarge1099.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![mcy](/content/v00646315m763300/xxlarge1084.gif) ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![ucy](/content/v00646315m763300/xxlarge1091.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) (127–130°), ![ncy](/content/v00646315m763300/xxlarge1085.gif) ![icy](/content/v00646315m763300/xxlarge1080.gif) , ![scy](/content/v00646315m763300/xxlarge1089.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![vcy](/content/v00646315m763300/xxlarge1074.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![vcy](/content/v00646315m763300/xxlarge1074.gif) ![ucy](/content/v00646315m763300/xxlarge1091.gif) ![yucy](/content/v00646315m763300/xxlarge1102.gif) ![shchcy](/content/v00646315m763300/xxlarge1097.gif) ![icy](/content/v00646315m763300/xxlarge1080.gif) ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![khcy](/content/v00646315m763300/xxlarge1093.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![dcy](/content/v00646315m763300/xxlarge1076.gif) III I ![bcy](/content/v00646315m763300/xxlarge1073.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![lcy](/content/v00646315m763300/xxlarge1083.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![lcy](/content/v00646315m763300/xxlarge1083.gif) ![bcy](/content/v00646315m763300/xxlarge1073.gif) ![ycy](/content/v00646315m763300/xxlarge1099.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) ![vcy](/content/v00646315m763300/xxlarge1074.gif) ![yacy](/content/v00646315m763300/xxlarge1103.gif) ![yacy](/content/v00646315m763300/xxlarge1103.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![lcy](/content/v00646315m763300/xxlarge1083.gif) ![kcy](/content/v00646315m763300/xxlarge1082.gif) 51,5% ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![khcy](/content/v00646315m763300/xxlarge1093.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![dcy](/content/v00646315m763300/xxlarge1076.gif) II I. ![Pcy](/content/v00646315m763300/xxlarge1055.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![khcy](/content/v00646315m763300/xxlarge1093.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![dcy](/content/v00646315m763300/xxlarge1076.gif) II I ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![icy](/content/v00646315m763300/xxlarge1080.gif) ![yacy](/content/v00646315m763300/xxlarge1103.gif) ![lcy](/content/v00646315m763300/xxlarge1083.gif) H=13,2 ![kcy](/content/v00646315m763300/xxlarge1082.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) / . ![Pcy](/content/v00646315m763300/xxlarge1055.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![khcy](/content/v00646315m763300/xxlarge1093.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![dcy](/content/v00646315m763300/xxlarge1076.gif) III I ![scy](/content/v00646315m763300/xxlarge1089.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![vcy](/content/v00646315m763300/xxlarge1074.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![vcy](/content/v00646315m763300/xxlarge1074.gif) ![ucy](/content/v00646315m763300/xxlarge1091.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![Delta](/content/v00646315m763300/xxlarge916.gif) 6,8 ± 0,2 ![kcy](/content/v00646315m763300/xxlarge1082.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) / . ![Pcy](/content/v00646315m763300/xxlarge1055.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![khcy](/content/v00646315m763300/xxlarge1093.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) III II ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![icy](/content/v00646315m763300/xxlarge1080.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![khcy](/content/v00646315m763300/xxlarge1093.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![dcy](/content/v00646315m763300/xxlarge1076.gif) ![icy](/content/v00646315m763300/xxlarge1080.gif) ![dcy](/content/v00646315m763300/xxlarge1076.gif) ![vcy](/content/v00646315m763300/xxlarge1074.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![ucy](/content/v00646315m763300/xxlarge1091.gif) ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![ncy](/content/v00646315m763300/xxlarge1085.gif) ![ncy](/content/v00646315m763300/xxlarge1085.gif) ![ncy](/content/v00646315m763300/xxlarge1085.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![gcy](/content/v00646315m763300/xxlarge1075.gif) ![scy](/content/v00646315m763300/xxlarge1089.gif) ![icy](/content/v00646315m763300/xxlarge1080.gif) ![lcy](/content/v00646315m763300/xxlarge1083.gif) ![softcy](/content/v00646315m763300/xxlarge1100.gif) ![ncy](/content/v00646315m763300/xxlarge1085.gif) ![vcy](/content/v00646315m763300/xxlarge1074.gif) ![lcy](/content/v00646315m763300/xxlarge1083.gif) ![icy](/content/v00646315m763300/xxlarge1080.gif) ![yacy](/content/v00646315m763300/xxlarge1103.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![pcy](/content/v00646315m763300/xxlarge1087.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![dcy](/content/v00646315m763300/xxlarge1076.gif) ![ycy](/content/v00646315m763300/xxlarge1099.gif) ![dcy](/content/v00646315m763300/xxlarge1076.gif) ![ucy](/content/v00646315m763300/xxlarge1091.gif) ![shchcy](/content/v00646315m763300/xxlarge1097.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![mcy](/content/v00646315m763300/xxlarge1084.gif) ![icy](/content/v00646315m763300/xxlarge1080.gif) ![chcy](/content/v00646315m763300/xxlarge1095.gif) ![iecy](/content/v00646315m763300/xxlarge1077.gif) ![kcy](/content/v00646315m763300/xxlarge1082.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![bcy](/content/v00646315m763300/xxlarge1073.gif) ![rcy](/content/v00646315m763300/xxlarge1088.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) ![bcy](/content/v00646315m763300/xxlarge1073.gif) ![ocy](/content/v00646315m763300/xxlarge1086.gif) ![tcy](/content/v00646315m763300/xxlarge1090.gif) ![kcy](/content/v00646315m763300/xxlarge1082.gif) ![fcy](/content/v00646315m763300/xxlarge1092.gif) ![acy](/content/v00646315m763300/xxlarge1072.gif) ![zcy](/content/v00646315m763300/xxlarge1079.gif) I.
Mémoire présenté en l'honneur du 70e anniversaire du Professeur Clément Duval. |
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