Authors:Margit Bán, J. Madarász, Petra Bombicz, G. Pokol, and S. Gál
Composition and structure of crystals of unknown origin, crystallizing spontaneously from ethylenediamine on standing, has
been determined by elemental analysis, FTIR, 1H and 13C NMR spectroscopy and X-ray diffraction. The crystal with molecular formula C6H14N4 has been found to be a highly symmetric
saturated imino compound with double-ring structure, and unambiguously identified as trans-1,4,5,8-tetraazodecalin by 1H NMR and powder X-ray diffraction based on both its specific AA'BB' spin coupling system and simulated XRD pattern calculated
from available data of previous single crystal structure determination, respectively. Simultaneous TG/DTA measurement shows
one-step degradation of this compound. The volatile decomposition products have been followed by both TG/DTA-MS and TG-FTIR.
Group of the largest fragments (m/z=80, 81 and 82) observed by TG/DTA-MS corresponds to an aromatic 1,4-diazine (pyrazine). In the EGA-FTIR spectrum of released
gaseous species measured at the highest evolution rate by TG-FTIR, ethylenediamine can be identified as another decomposition
Authors:M. Zaharescu, A. Jitianu, A. Braileanu, J. Madarász, and G. Pokol
It is well known that SiO2 -based inorganic-organic hybrid materials present significant differences due to the organic moieties bound to the inorganic
network and to the preparation conditions.
In the present work the ageing effect on the thermal stability of the SiO2 -based inorganic-organic hybrid materials prepared using tetraethoxysilan (TEOS), triethoxymethylsilan (MTEOS), triethoxyvinylsilan
(VTEOS), tetramethoxysilan (TMOS), trimethoxymethylsilan (MTMOS) and trimethoxyvinylsilan (VTMOS) was studied.
TG/DTA-MS was used to study the decomposition process of the materials. The structural modifications of the materials during
ageing were studied using spectral methods.
The gels obtained starting with more reactive alkoxides, of methoxy-type, present more complex structures and are less stable
Supramolecular 2,3- and 2,5-pyridinedicarboxylate (PDC) intercalated
ZnAl-layered double hydroxides (2,3- and 2,5-PDC–ZnAl–LDHs) have
been prepared by ion exchange method. The structure and composition of the
intercalated materials have been studied by X-ray diffraction (XRD) and inductively
coupled plasma emission spectroscopy (ICP). The study indicates that the 2,3-PDC
and 2,5-PDC anions are accommodated as interdigitated bilayer and monolayer
arrangement respectively between the sheets of LDHs. Furthermore, their thermal
decomposition processes were studied by the use of in situ high temperature
X-ray diffraction (HT-XRD), and the combined technique of thermogravimetry-differential
thermal analysis-mass spectrometry (TG-DTA-MS) under N2 atmosphere. Based
on the comparison study on the temperatures of both decarboxylation and complete
decomposition of interlayer PDC, it can be concluded that 2,5-PDC–ZnAl–LDHs
has higher thermal stability than that of 2,3-PDC–ZnAl–LDHs.
Thermal properties of cis-1,4-poly(butadiene), Europrene cis, were investigated by means of thermal analysis and complementary methods. Thermal analysis of polymer was carried out both in air and inert atmosphere with a derivatgraph, DSC and internal TG-FTIR coupling system as well as internal TG, DTA-MS coupling system. It was found that investigations in air atmosphere the method of the sample preparation ofcis-1,4-poly(butadiene) influences the results of thermal analysis, which is connected with the rate oxygen diffusion into the reaction zone. Taking into consideration both the method of the sample preparing and atmosphere of thermal studies, the values of activation energy of destruction of cis-1,4-poly(butadiene) were determined. Using TG-FTIR and TG-MS methods, some products of thermal destruction of elastomer were determined.
Authors:I. Szilágyi, J. Madarász, F. Hange, and G. Pokol
Thermal decomposition of ammonium paratungstate
tetrahydrate, (NH4)10[H2W12O42]4H2O has been followed by simultaneous TG/DTA and online evolved
gas analysis (TG/DTA-MS) in flowing 10% H2/Ar directly
up to 900C. Solid intermediate products have been structurally evaluated
by FTIR spectroscopy and powder X-ray diffraction (XRD). A previously unexplained
exothermic heat effect has been detected at 700–750C. On the basis
of TG/DTA as well as H2O and NH3
evolution curves and XRD patterns, it has been assigned to the formation and
crystallization heat of γ-tungsten-oxide (WO2.72/W18O49)
from β-tungsten-oxide (WO2.9/W20O58)
and residual ammonium tungsten bronze.
Thermal decomposition of a mixed valence copper salt, Na4[Cu(NH3)4][Cu(S2O3)2]2·0.5NH3 (1) prepared from pentahydrates of sodium thiosulfate and copper sulphate of various molar ratios in 1:1 v/v aqueous ammonia
solution, has been studied up to 1,000 °C in flowing air by simultaneous thermogravimetric and differential thermal analysis
coupled online with quadrupole mass spectrometer (TG/DTA-MS) and FTIR spectrometric gas cell (TG-FTIR), in comparison. Compound
1 releases first but very slowly some of the included ammonia till 170 °C, then simultaneously ammonia (NH3) and sulphur dioxide (SO2) from 175 to 225 °C, whilst the evolution of SO2 from thiosulfate ligands continues in several overlapping stages until 410 °C, and is escorted by explicit exothermic heat
effects at around 237, 260, 358 and 410 °C. The former two exothermic DTA-peaks correspond to the simultaneous degradation
and air oxidation processes of excess thiosulfate anions not reacted by formation of copper sulfides (both digenite, Cu1.8S and covellite, CuS, checked by XRD) and sodium sulfate, while the last two exothermic peaks are accompanied also by considerable
mass gains, as the result of two-step oxidation of copper sulfides into various oxosulfates. The mass increase continues further
on until 580 °C, when the sample mass begins to decrease slowly, as a continuous decomposition of the intermediate copper
oxosulfates, indicated also by re-evolution of SO2. At 1,000 °C, a residual mass value of 64.3% represents a stoichiometric formation of CuIIO and anhydrous Na2SO4.
Authors:Irena Szczygieł, Zofia Jagoda, Julia Kłak, and Maria Korabik
TG/DTA–MS techniques ( Fig. 8 ) show that the polymeric structure of the complex decomposes first into the components [NiL] 2+ and [Co(NCS) 4 ] 2− . This is reflected by the small ion current signals which have been recorded for the mass
spectra of the complex, BiCl 3 and SC(NH 2 ) 2 were measured by a Renishaw in Via Reflex Laser Raman spectrometer (785 nm excitation). Thermal studies for the complex were performed by a NETZSCH STA 449C TG–DTA–MS Thermal Analyzer under argon atmospheric