A TG/DTA/MS study of the oxidation of nickel sulphide |
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Authors: | J G Dunn C E Kelly |
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Institution: | (1) Department of Chemisty, Western Australian Institute of Technology, Perth, Western Australia |
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Abstract: | The oxidative behaviour of synthetic millerite (Ni0.994S) has been studied by TG and DTA in a dynamic oxygen atmosphere (0.2 l min–1) over the temperature range 20–1000° (heating rate 10° min–1). EGA was carried out by a coupled mass spectrometer. The reaction products at various intermediate temperatures were characterized by X-ray powder diffractometry. A reaction sequence has been deduced, in which in the temperature range 550–700° complete oxidation of Ni0.994S had occurred with the formation of NiSO4, Ni3S2, NiO and possibly -Ni7S6. Between 700–800°, NiSO4 continued to be formed, whilst Ni3S2 and -Ni7S6 were oxidised. Above 800°, NiSO4 decomposed to NiO, the latter being the only species evident above 800°.
Zusammenfassung Das oxidative Verhalten von synthetischem Millerit (Ni0.994S) wurde mittels TG und DTA in einer dynamischen Sauerstoffatmosphäre (0.2 l min–1) im Temperaturbereich von 20 bis 1000° (Aufheizgeschwindigkeit 10° min–1) untersucht. EGA wurde mit einem gekoppelten Massenspektrometer durchgeführt. Die Reaktionsprodukte bei verschiedenen Zwischentemperaturen wurden mittels Röntgen-Pulver-Diffraktometrie charakterisiert. Eine Reaktionssequenz wurde abgeleitet, nach welcher im Temperaturbereich von 550 bis 700° die vollständige Oxidierung von Ni0.994S unter Bildung von NiSO4, Ni3S2, NiO und wahrscheinlich -Ni7S6 vor sich geht. Zwischen 700 und 800° wird NiSO4 auch weiterhin gebildet, während Ni7S2 und -Ni7S6 oxidiert wurden. Oberhalb von 800° wurde NiSO4 zu NiO zersetzt, das einzig nachweisbare Produkt oberhalb von 800°.
Résumé On a étudié l'oxydation de la millérite synthétique (Ni0.994S) par TG et ATD en atmosphère dynamique d'oxygène (0,2 1· min–1) et dans l'intervalle de températures allant de 20 à 1000° (vitesse de chauffage 10°· min–1). L'analyse des gaz émis s'est effectuée avec un spectromètre de masse couplé. Les produits de réaction ont été caractérisés à diverses températures intermédiaires par diffractométrie de poudre aux rayons X. On a déduit une séquence de réactions, selon laquelle, dans l'intervalle compris entre 550 et 700°, l'oxydation complète de Ni0.994S a lieu avec formation de NiSO4, Ni3S2, NiO et probablement -Ni7S6. Entre 700 et 800°, la formation de NiSO4 se poursuit tandis que Ni3S2 et -Ni7S6 sont oxydés. Au-dessus de 800°, NiSO4 se décompose en NiO qui constitue l'unique composé qui puisse être décelé au-dessus de 800°.
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![Vcy](/content/k684028865h31915/xxlarge1042.gif) ![ycy](/content/k684028865h31915/xxlarge1099.gif) ![vcy](/content/k684028865h31915/xxlarge1074.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![dcy](/content/k684028865h31915/xxlarge1076.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![ncy](/content/k684028865h31915/xxlarge1085.gif) ![pcy](/content/k684028865h31915/xxlarge1087.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![scy](/content/k684028865h31915/xxlarge1089.gif) ![lcy](/content/k684028865h31915/xxlarge1083.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![dcy](/content/k684028865h31915/xxlarge1076.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![lcy](/content/k684028865h31915/xxlarge1083.gif) ![softcy](/content/k684028865h31915/xxlarge1100.gif) ![ncy](/content/k684028865h31915/xxlarge1085.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![scy](/content/k684028865h31915/xxlarge1089.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![rcy](/content/k684028865h31915/xxlarge1088.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![kcy](/content/k684028865h31915/xxlarge1082.gif) ![tscy](/content/k684028865h31915/xxlarge1094.gif) ![icy](/content/k684028865h31915/xxlarge1080.gif) ![pcy](/content/k684028865h31915/xxlarge1087.gif) ![rcy](/content/k684028865h31915/xxlarge1088.gif) ![kcy](/content/k684028865h31915/xxlarge1082.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![rcy](/content/k684028865h31915/xxlarge1088.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![bcy](/content/k684028865h31915/xxlarge1073.gif) ![lcy](/content/k684028865h31915/xxlarge1083.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![scy](/content/k684028865h31915/xxlarge1089.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![mcy](/content/k684028865h31915/xxlarge1084.gif) ![pcy](/content/k684028865h31915/xxlarge1087.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![rcy](/content/k684028865h31915/xxlarge1088.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![ucy](/content/k684028865h31915/xxlarge1091.gif) 550–700° ![pcy](/content/k684028865h31915/xxlarge1087.gif) ![rcy](/content/k684028865h31915/xxlarge1088.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![kcy](/content/k684028865h31915/xxlarge1082.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![pcy](/content/k684028865h31915/xxlarge1087.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![lcy](/content/k684028865h31915/xxlarge1083.gif) ![ncy](/content/k684028865h31915/xxlarge1085.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![kcy](/content/k684028865h31915/xxlarge1082.gif) ![icy](/content/k684028865h31915/xxlarge1080.gif) ![scy](/content/k684028865h31915/xxlarge1089.gif) ![lcy](/content/k684028865h31915/xxlarge1083.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![ncy](/content/k684028865h31915/xxlarge1085.gif) ![icy](/content/k684028865h31915/xxlarge1080.gif) Ni0.994S ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![bcy](/content/k684028865h31915/xxlarge1073.gif) ![rcy](/content/k684028865h31915/xxlarge1088.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![zcy](/content/k684028865h31915/xxlarge1079.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![ncy](/content/k684028865h31915/xxlarge1085.gif) ![icy](/content/k684028865h31915/xxlarge1080.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) NiSO4, Ni3S2, NiO ![vcy](/content/k684028865h31915/xxlarge1074.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![zcy](/content/k684028865h31915/xxlarge1079.gif) ![mcy](/content/k684028865h31915/xxlarge1084.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![zhcy](/content/k684028865h31915/xxlarge1078.gif) ![ncy](/content/k684028865h31915/xxlarge1085.gif) -Ni7S6. ![Mcy](/content/k684028865h31915/xxlarge1052.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![zhcy](/content/k684028865h31915/xxlarge1078.gif) ![dcy](/content/k684028865h31915/xxlarge1076.gif) 700–800° ![scy](/content/k684028865h31915/xxlarge1089.gif) ![ucy](/content/k684028865h31915/xxlarge1091.gif) ![lcy](/content/k684028865h31915/xxlarge1083.gif) ![softcy](/content/k684028865h31915/xxlarge1100.gif) ![fcy](/content/k684028865h31915/xxlarge1092.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![ncy](/content/k684028865h31915/xxlarge1085.gif) ![icy](/content/k684028865h31915/xxlarge1080.gif) ![kcy](/content/k684028865h31915/xxlarge1082.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![lcy](/content/k684028865h31915/xxlarge1083.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![scy](/content/k684028865h31915/xxlarge1089.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![scy](/content/k684028865h31915/xxlarge1089.gif) ![ncy](/content/k684028865h31915/xxlarge1085.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![icy](/content/k684028865h31915/xxlarge1080.gif) ![mcy](/content/k684028865h31915/xxlarge1084.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![ncy](/content/k684028865h31915/xxlarge1085.gif) ![ncy](/content/k684028865h31915/xxlarge1085.gif) ![ycy](/content/k684028865h31915/xxlarge1099.gif) , ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![vcy](/content/k684028865h31915/xxlarge1074.gif) ![rcy](/content/k684028865h31915/xxlarge1088.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![mcy](/content/k684028865h31915/xxlarge1084.gif) ![kcy](/content/k684028865h31915/xxlarge1082.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) Ni3S2 -Ni7S6 ![ucy](/content/k684028865h31915/xxlarge1091.gif) ![zhcy](/content/k684028865h31915/xxlarge1078.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![kcy](/content/k684028865h31915/xxlarge1082.gif) ![icy](/content/k684028865h31915/xxlarge1080.gif) ![scy](/content/k684028865h31915/xxlarge1089.gif) ![lcy](/content/k684028865h31915/xxlarge1083.gif) ![yacy](/content/k684028865h31915/xxlarge1103.gif) ![yucy](/content/k684028865h31915/xxlarge1102.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![scy](/content/k684028865h31915/xxlarge1089.gif) . ![Vcy](/content/k684028865h31915/xxlarge1042.gif) ![shcy](/content/k684028865h31915/xxlarge1096.gif) 800° ![scy](/content/k684028865h31915/xxlarge1089.gif) ![ucy](/content/k684028865h31915/xxlarge1091.gif) ![lcy](/content/k684028865h31915/xxlarge1083.gif) ![softcy](/content/k684028865h31915/xxlarge1100.gif) ![fcy](/content/k684028865h31915/xxlarge1092.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![ncy](/content/k684028865h31915/xxlarge1085.gif) ![icy](/content/k684028865h31915/xxlarge1080.gif) ![kcy](/content/k684028865h31915/xxlarge1082.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![lcy](/content/k684028865h31915/xxlarge1083.gif) ![rcy](/content/k684028865h31915/xxlarge1088.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![zcy](/content/k684028865h31915/xxlarge1079.gif) ![lcy](/content/k684028865h31915/xxlarge1083.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![gcy](/content/k684028865h31915/xxlarge1075.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![scy](/content/k684028865h31915/xxlarge1089.gif) ![dcy](/content/k684028865h31915/xxlarge1076.gif) NiO, ![kcy](/content/k684028865h31915/xxlarge1082.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![ycy](/content/k684028865h31915/xxlarge1099.gif) ![pcy](/content/k684028865h31915/xxlarge1087.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![yacy](/content/k684028865h31915/xxlarge1103.gif) ![vcy](/content/k684028865h31915/xxlarge1074.gif) ![lcy](/content/k684028865h31915/xxlarge1083.gif) ![yacy](/content/k684028865h31915/xxlarge1103.gif) ![iecy](/content/k684028865h31915/xxlarge1077.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![scy](/content/k684028865h31915/xxlarge1089.gif) ![kcy](/content/k684028865h31915/xxlarge1082.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![ocy](/content/k684028865h31915/xxlarge1086.gif) ![chcy](/content/k684028865h31915/xxlarge1095.gif) ![vcy](/content/k684028865h31915/xxlarge1074.gif) ![icy](/content/k684028865h31915/xxlarge1080.gif) ![dcy](/content/k684028865h31915/xxlarge1076.gif) ![ncy](/content/k684028865h31915/xxlarge1085.gif) ![ycy](/content/k684028865h31915/xxlarge1099.gif) ![chcy](/content/k684028865h31915/xxlarge1095.gif) ![acy](/content/k684028865h31915/xxlarge1072.gif) ![scy](/content/k684028865h31915/xxlarge1089.gif) ![tcy](/content/k684028865h31915/xxlarge1090.gif) ![icy](/content/k684028865h31915/xxlarge1080.gif) ![tscy](/content/k684028865h31915/xxlarge1094.gif) ![vcy](/content/k684028865h31915/xxlarge1074.gif) ![ycy](/content/k684028865h31915/xxlarge1099.gif) ![shcy](/content/k684028865h31915/xxlarge1096.gif) 800°.
We wish to thank Dr. T. Kennedy for useful discussions and Messrs. B. Sturman, I. Twaddle, K. Oliver and W. Thomas for technical assistance. |
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本文献已被 SpringerLink 等数据库收录! |
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