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- Author or Editor: J. O. Hill x
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The thermal decomposition of mercury(I) and (II) sulfates has been investigated by thermogravimetry. The solid-state decomposition products have been characterized by infrared and Raman spectroscopy, mass spectrometry and an X-ray diffraction method. It is concluded that mercury(I) sulfate decomposes in two steps, initially forming a mixture of metallic mercury and mercury(II) sulfate — the latter subsequently decomposes without forming a stable intermediate. The stoichiometry of disproportionation of mercury(I) sulfate and the thermal stability range of mercury(I) and mercury(II) sulfates have been established.
The pyrolysis of a suite of brown coal samples and bituminous coal maceral concentrates is investigated by non-isothermal thermogravimetry. The TG data for these coals reveal a two-stage pyrolysis process. The activation energy for the primary pyrolysis stage is considerably higher than that for the secondary pyrolysis stage. It is evident that a particular coal may be characterised by the weighted mean apparent pyrolysis activation energy which correlates with the corresponding specific energy of the coal.
A thermogravimetry study of a series of cyclophane bis(sulfoxides) (1–6) has shown that thermal decomposition of these compounds occurs in two stages with a stepwise loss of the sulfoxide groups at well defined decomposition temperatures. The stepwise thermal cleavage has been rationalized in terms of the stereochemistry of the sulfoxide groups and the strain associated with the resultant elimination products.
Lithium, sodium, potassium and ammonium bisulphate have been shown by detailed TG/DTA studies to have limited application as molten solvents. By contrast, the eutectic bisulphate systems, ammonium-potassium bisulphate and sodium-potassium bisulphate, appear to be excellent molten solvents in view of their low melting points, long liquid ranges and prolonged thermal stability at 200°. In contrast to previous studies, potassium pyrosulphate has been found to be an excellent molten solvent, provided rigorous preliminary drying procedures have been applied.
A new tin dithiocarbamate containing sulphur bridges, di-μ-sulphidobis [bis(N,N-diethyldithiocarbamato)tin(IV)], has been isolated from the thermal decomposition of tetrakis(N,N-diethyldithiocarbamato)tin(IV). A dimeric structure is proposed on the basis of results from mass spectrometry, infrared spectroscopy, thermal analysis and vapour pressure osmometry.
TG/DTA and Thermal Degradation Mass spectrometry (TDMS) data are presented for a series of nickel(II)thiourea chloride complexes: NiL4Cl2:L=thiourea or methyl-, dimethyl-, tetramethyl-, di-n-butyl, naphthyl-, ethylene- or allylthiourea. Two different thermal decomposition mechanisms are proposed for these complexes, and it is apparent that the thermal decomposition mechanism adopted by a particular complex depends on the structure of the relevant thiourea ligand and not on the nature of the halide ligand or on the existence of geometrical isomerism for these complexes.
