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Thermal decomposition of [Co(NH3)6]Cl3

Part I. Non-isothermal, quasi-isothermal and scanning electron microscopy studies

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Abstract

The thermal decomposition reactions of [Co(NH3)6]Cl3 were determined in dynamic argon and air atmospheres. The investigations were carried out with simultaneous TG-DTG-DTA measurements under non-isothermal conditions, thermogravimetry under quasi-isothermal conditions, reflectance spectroscopy, absorption spectroscopy, X-ray diffraction and chemical analysis. The data show that the thermal decomposition of [Co(NH3)6]Cl3 occurs in three and four stages in argon and air atmospheres, respectively. The determined sequences are in agreement with that proposed by Simons and Wendlandt [2, 5].

The changes in the morphology of the studied complex crystalline powder in the course of thermal decomposition in air were followed by scanning electron microscopy.

Zusammenfassung

In bewegter Argon- und Luftatmosphäre wurden die Zersetzungsreaktionen für [Co(NH3)6]Cl3 bestimmt. Zu den Untersuchungen wurden folgende Methoden zu Hilfe gezogen: simultane TG-DTG-DTA-Messungen unter nichtisothermen Bedingungen, Thermogravimetrie unter quasi-isothermen Bedingungen, Remissionsspektroskopie, Absorptionsspektroskopie, Röntgendiffraktion und chemische Analyse. Die Ergebnisse zeigen, daß sich [Co(NH3)6]Cl3 in Argon in drei und in Luft in vier Schritten thermisch zersetzt. Die festgestellten Sequenzen stehen in Übereinstimmung mit den von Simon und Wendlandt [2, 5] vorgeschlagenen. Veränderungen in der Morphologie des untersuchten Komplexkristallpulvers wurden über die thermische Zersetzung in Luft mittels Scanning-Elektronen-Mikroskopie beobachtet.

Резюме

В динамической атмос фере аргона и воздуха определены реакции т ермического разложения комплекс а [Co(NH3)6]Cl3. Исследования бы ли проведены с помощью совмещенного ТГ, ДТГ и ДТА метода в неизотер мических условиях, метода терм огравиметрии в квази-изотермическ их условиях, спектрос копии отражения, абсорбцио нной спектроскопии, рентгеноструктурно го и химического анал иза. Полученные результа ты показали, что термическое разложе ние комплекса в атмос фере аргона и воздуха протекает, с оответственно, в три и четыре стадии, по следовательность ко торых согласуется с таково й, предложенной Симонсом и Вепдландо м, Используя сканирую щую электронную микроск опию прослежено морфологическое изм енение порошкообраз ного комплекса в ходе его т ермического разложе ния в атмосфере воздуха.

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Ingier-Stocka, E., Bogacz, A. Thermal decomposition of [Co(NH3)6]Cl3 . Journal of Thermal Analysis 35, 1373–1386 (1989). https://doi.org/10.1007/BF01912914

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