Evolved gas analysis of dichlorobis(thiourea)zinc(II) by coupled TG-FTIR and TG/DTA-MS techniques

Madarász, János and Krunks, M. and Niinisto, L. and Pokol, György (2004) Evolved gas analysis of dichlorobis(thiourea)zinc(II) by coupled TG-FTIR and TG/DTA-MS techniques. JOURNAL OF THERMAL ANALYSIS AND CALORIMETRY, 78 (2). pp. 679-686. ISSN 1388-6150

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Abstract

Identification and monitoring of gaseous species released during thermal decomposition of the title compound 1, Zn(tu)(2)Cl-2, (tu=thiourea, (NH2)(2)C=S) have been carried out in flowing air atmosphere up to 800degreesC by both online coupled TG-EGA-FTIR and simultaneous TG/DTA-EGA-MS. The first gaseous products of 1, between 200 and 240degreesC, are carbon disulfide (CS2) and ammonia (NH3). At 240degreesC, an exothermic oxidation of CS2 vapors occurs resulting in a sudden release of sulphur dioxide (SO2) and carbonyl sulphide (COS). An intense evolution of hydrogen cyanide (HCN) and beginning of the evolution of cyanamide (H2NCN) and isothiocyanic acid (HNCS) are also observed just above 240degreesC. Probably because of condensation and/or polymerization of cyanamide vapors on the windows and mirrors of the FTIR gas cell optics, some strange baseline shape changes are also occurring above 330degreesC. Above 500degreesC the oxidation process of organic residues appears to accelerate which is indicated by the increasing concentration of CO2, while above 600degreesC zinc sulfide starts to oxidize resulting in the evolution of SO2. All species identified by FTIR gas cell were also confirmed by mass spectrometry, except for HNCS.

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