Thermal decomposition of copper(II) and zinc carbonate hydroxides by means of TG-MS

Summary For the quantitative analyses of evolved CO₂and H₂O during the thermal decomposition of solids, calibration curves, i.e. the amounts of evolved gases vs. the corresponding peak areas of mass chromatograms measured by TG-MS, were plotted as referenced by the reaction stoichiometry of the thermal decomposition of sodium hydrogencarbonate NaHCO₃. The accuracy and reliability of the quantitative analyses of the evolved CO₂and H₂O based on the calibration curves were evaluated by applying the calibration curves to the mass chromatograms for the thermal decompositions of copper(II) and zinc carbonate hydroxides. It was indicated from the observed ratio of evolved CO₂and H₂O that the compositions of copper(II) and zinc carbonate hydroxides examined in this study correspond to mineral malachite, Cu₂CO₃(OH)₂, and hydrozincate, Zn₅(CO₃)₂(OH)₆, respectively. Reliability of the present analytical procedure was confirmed by the fairly good agreement of the mass fraction of the evolved gases calculated from the analytical values with the total mass-loss during the thermal decompositions measured by TG.     

Thermal properties of high-T c superconductors

The termal stabilities of several families of high-T _c superconductors (HTSC), as well as the dependence of phase transitions on temperature and stoichiometry, have been studied by X-ray diffraction, DTA, TG and DSC. Experimental results are discussed in the context of decomposition models.     

Investigations on Preparation,Crystal Structure and Thermal Stability of Bis(O-ethylcarbonodithiolato-S,S′)(1,10-phenanthroline-N~1,N~(10))cobalt(II) Complex:[Co(Et-XA)_2·phen]·H_2O (XA=xanthate)

IntroductionTheincreasingcommercialvalueoftransitionmetalcomplexesofxanthateshasarousedconsiderableinterestintheirchemistry .Whiletheiranalyticalapplicationsarewellknown ,1theyarenowfindingextensiveuseinvulcan izationofrubber ,frothfloatationprocessforconcentrationofsulphideores ,asantioxidants ,lubricants ,2 ,3andhavebeenfoundtopossessfungicidalandinsecticidalactivi ties .4 Recently ,molecularrecognitionbetweenhostandguestmolecules ,inclusionphenomenaandnoncovalentmolecularinteractionarefunda…     

Combining thermal analysis with other techniques to monitor the decomposition of poly(m-phenylene isophthalamide)

The pyrolysis behaviour of Nomex, poly(m-phenylene isophthalamide) fibres under argon has been investigated up to a temperature of 1173 K with different methods to get direct information on the progressive changes taking place in the solid material and its carbon fibre residues. The main stages of the pyrolytic degradation of the fibres were determined by thermal analysis (TG and DTA) and their chemical and morphological evolution through the different steps was subsequently followed by Fourier transform infrared spectroscopy (FTIR) and atomic force microscopy (AFM) measurements, respectively, on samples treated to various temperatures. This revised version was published online in July 2006 with corrections to the Cover Date.     

Thermal decomposition study on mixed ligand thymine complexes of divalent nickel(II) with dianions of some dicarboxylic acids

Thermal decomposition of mixed ligand thymine (2,4-dihydroxy-5-methylpyrimidine) complexes of divalent Ni(II) with aspartate, glutamate and ADA (N-2-acetamido)iminodiacetate dianions was monitored by TG, DTG and DTA analysis in static atmosphere of air. The decomposition course and steps of complexes [Ni(C₅H₆N₂O₂)(C₄H₅NO₄)²⁻(H₂O)₂]·H₂O, [Ni(C₅H₆N₂O₂)(C₅H₇NO₄)²⁻(H₂O)₂]·H₂O and [Ni(C₅H₆N₂O₂)(C₆H₈N₂O₅)²⁻(H₂O)₂]·1.5H₂O were analyzed. The final decomposition products are found to be the corresponding metal oxides. The kinetic parameters namely, activation energy (E*), enthalpy (ΔH*), entropy (ΔS*) and free energy change of decomposition (ΔG*) are calculated from the TG curves using Coats–Redfern and Horowitz–Metzger equations. The stability order found for these complexes follows the trend aspartate > ADA > glutamate.     

Effect of grinding on thermal reactivity of ceramic clay minerals

The effect of grinding on thermal behavior of pyrophyllite and talc as commonly used ceramic clay minerals was investigated by DTA, TG, emanation thermal analysis (ETA), B.E.T. surface area (s.a.) measurements, X-ray diffraction (XRD) and scanning electron microscopy (SEM). A vibratory mill was used in this study, grinding time was 5 min. It was found that the grinding caused an increase in surface area and a grain size reduction of the samples. From TG and DTA results it followed that grinding caused a decrease of the temperature at which the structure bound OH groups released. The formation of high temperature phases was enhanced with the ground samples. For the ground talc sample the crystallization of non-crystalline phase into orthorhombic enstatite was observed in the range of 800°C. For ground pyrophyllite a certain agglomeration of grains was observed in the range above 950°C. Moreover, for both clays the ETA characterized a closing up of subsurface irregularities caused by grinding as a decrease of the emanation rate in the range 250–400°C. The comparison of thermal analysis results with the results of other methods made it possible to better understand the effect of grinding on the ceramic clays.     

Estimation of the lipophilicity of antiarrhythmic and antihypertensive active 1-substituted pyrrolidin-2-one and pyrrolidine derivatives

The lipophilicity of some antiarrhythmic and antihypertensive active 1-[2-hydroxy- or 1-[2-acetoxy-3-(4-aryl-1-piperazinyl)propyl]pyrrolidin-2-one derivatives (1-12) has been investigated. Their lipophilicity (R(MO) and log k') was determined by reversed-phase thin-layer chromatography and reversed-phase high-performance liquid chromatography with mixtures of acetonitrile and Tris buffer as mobile phases. The partition coefficients of compounds 1-12 (log P(ScilogP)) were also calculated with the ScilogP program. Comparison of R(MO), log k' and calculated log D(7.0 ScilogP) values enabled calculation of clog D(7.0 TLC) and clog D(7.0 HPLC) values. Preliminary quantitative structure-activity relationship studies indicated that for active compounds there is a dependence between affinity for alpha(2)-adrenoceptors and their clog D(7.0 HPLC) values.     

Characterization of phase transition of Ba2-xSrxIn2O5 by thermal analysis and high temperature X-ray diffraction

The phase transitions of Ba_2-xSr_xIn₂O₅ were investigated with various thermal analyses and high-temperature X-ray diffraction. It was clarified that crystal structure of Ba_2-xSr_xIn₂O₅ with x=0.0~0.4 varies from brownmillerite through distorted perovskite to another distorted perovskite with increase of temperature. The phase transition from brownmillerite to distorted perovskite was revealed to be first order, whereas transition from distorted perovskite to another one was second order. The specimen with x≥0.5 showed only one first order phase transition from brownmillerite to distorted perovskite. The phase diagram of Ba_2-xSr_xIn₂O₅ was established and existence of tricritical point at ~1100°C with x=0.4~0.5 was suggested. This revised version was published online in August 2006 with corrections to the Cover Date.