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M. Feist Institut für Chemie der Humboldt-Universität zu Berlin, Hessische Straße 1-2, D-10115 Berlin

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R. Kunze Bundesanstalt für Materialforschung und -prüfung, Unter den Eichen 87, D-12205 Berlin, Germany

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D. Neubert Bundesanstalt für Materialforschung und -prüfung, Unter den Eichen 87, D-12205 Berlin, Germany

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K. Witke Bundesanstalt für Materialforschung und -prüfung, Unter den Eichen 87, D-12205 Berlin, Germany

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E. Kemnitz Institut für Chemie der Humboldt-Universität zu Berlin, Hessische Straße 1-2, D-10115 Berlin

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Abstract  

(trienH2)[CoCl4], which contains tetrahedral chlorocobaltate(II) anions, decomposes under argon in two stages via a stepwise deprotonation of the cation. The decomposition starts at 310°C with the liberation of HCl, followed at 400°C by the simultaneous release of a further mole of HCl and triene and/or its cracking products. The second decomposition stage is strongly influenced by the atmosphere. In the lower temperature region (<400°C), increasing oxygen contents of the carrier gas lead to decreasing mass losses. Therefore, the solid residues contain various amounts of C,N-containing products as well as coke. The thermal decomposition of the iron(III) compound, which contains μ-oxalato-bridged FeCl4 units, begins with the dehydratation followed by the decay of the complex anion to produce CO, CO2, and HCl. Instead of a binuclear, monooxobridged chloroferrate(III) complex, a [FeCl4] — containing compound is proposed as one of the final products. The third decomposition stage, partially overlaying the preceding one, is the degradation of the organic cation as found for the cobalt compound. The results of thein situ-TA-MS measurements are compared with those obtained from usual TA techniques as well as from the residue characterization by X-ray diffraction, Raman spectroscopy, and chemical analysis.

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Journal of Thermal Analysis and Calorimetry
Language English
Size A4
Year of
Foundation
1969
Volumes
per Year
1
Issues
per Year
24
Founder Akadémiai Kiadó
Founder's
Address
H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
Publisher Akadémiai Kiadó
Springer Nature Switzerland AG
Publisher's
Address
H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
CH-6330 Cham, Switzerland Gewerbestrasse 11.
Responsible
Publisher
Chief Executive Officer, Akadémiai Kiadó
ISSN 1388-6150 (Print)
ISSN 1588-2926 (Online)

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