Thermal decomposition of some analgesic agents

Thermogravimetry, derivative thermogravimetry (TG, DTG) and differential scanning calorimetry (DSC), were used to study the thermal behaviour of mefenamic acid, ibuprofen, acetaminophen, sodium diclofenac, phenylbutazone, dipyrone and salicylamide. The results led to thermal stability data and also to the interpretation concerning the thermal decomposition. © 1996 Akadémial Kiadó.

Mechanism of phase formation in Pb(ZrxTi1-x)O3 synthesized by a partial oxalate method

The phase formation mechanism, as well as the morphotropic phase boundary, of lead zirconate titanate (PZT) processed by a partial oxalate method was investigated by simultaneous thermal analysis (TG-DTA) and by qualitative and quantitative X-ray diffraction (XRD). The results show that the ZrxTi1-xO2 (ZT) phase reacts with PbO forming the PZT phase without intermediate phases. XRD analysis showed the coexistence of rhombohedral and tetragonal phases for 0.47 ≤ x ≤ 0.55 with the phase boundary composition for x = 0.51. For low calcination temperatures, preferential formation of the PZT rhombohedral phase was observed. A model for phase formation of PZT by the partial oxalate method is proposed based on the existence of two interfaces of reaction (PbO-PZT and PZT-ZT) and diffusion of cations.

Thermal decomposition of the magnesium, zinc, lead and niobium chelates derived from 8-quinolinol

Solid M-Ox compounds, where M represents Mg(II), Zn(II), Pb(II) and NbO(III), and Ox is 8-quinolinol, have been prepared. Thermogravimetry, derivative thermogravimetry (TG, DTG), differential scanning calorimetry (DSC), nuclear magnetic resonance (NMR) and infrared absorption spectra (IR) have been used to characterize and to study the thermal stability and thermal decomposition of these compounds. © 1997 Akadémiai Kiadó.

Preparation, characterization and spectroscopy of the europium diphenylphosphinate complex

The purpose of this work is to study the preparation and spectroscopic behavior of the europium diphenylphosphinate complex -Eu(DPP)3. Elemental and thermogravimetric analysis, powder X-ray diffractometry, and infrared spectroscopy were applied to characterize the formula of the final product and the sixfold coordination of the Eu3+ ion. Excitation and emission spectra have been recorded at liquid nitrogen and room temperatures. The 5D0→7F2 transition intensity decreases when T decreases in comparison to the 5D0→7F1 transition intensity. Molecular mechanic calculations were developed in order to obtain the spatial coordinates of the Eu3+ and ligand ions. The simple overlap model was used to calculate the total splitting of the 5D0→7F1 transition, 5D0→7F0/5D 0→7F2 ntensity ratio and the intensity parameters, Ωλ (λ=2 and 4). Good agreements between theoretical predictions and experimental results have been obtained with g=2/3 as the effective charge and α=0.8×10-24 cm3 as the isotropic polarizability of the oxygen. © 1998 Elsevier Science S.A.

Thermal behaviour and analytical study of the production of TiSnOx from the mixed 8-hydroxyquinolinates

Solubility and pH precipitation studies were carried out to obtain the binuclear complex {[TiO(C9H6NO)2][Sn(C9H6NO) 2]} involving 8-hydroxyquinoline as chelating agent. The compound, the individual mononuclear complexes and their physical mixture were evaluated by means of techniques such as TG, DTA, elemental analysis, X-ray diffraction, IR spectroscopy. The properties of the original compounds and also the thermoanalytical conditions exerted a great influence on the degree of crystallinity and on the crystalline phase of the mixed oxide obtained as final product of the thermal decomposition.

Synthesis and thermal study of 8-hydroxy-quinoline derivatives of the alkaline Earth metals: I. Strontium complexes

Strontium complexes of 5,7-dibromo-, 5,7-dichloro-, 7-iodo- and 5-chloro-7-iodo-8-hydroxyquinoline were precipitated from an aqueous ammonia and acetone medium. The complexes obtained were Sr[(C9H4ONBr2)2]·2.5H 2O; Sr[(C9H4ONCl2)(OH)]·1.5H2O; Sr[(C9H5ONI)2]·5H2O and Sr[(C9H4ONICl)(OH)]·1.25H2O. The residues of their thermal decomposition were SrBr2; a mixture of SrCl2, SrCO3 and SrO3 SrCO3, and SrCO3, respectively. All were characterized by means of thermogravimetry, differential thermal analysis, complexometry with EDTA, atomic absorption spectroscopy, IR spectroscopy and X-ray diffraction. © 1999 Akadémiai Kiadó.

Solid-state compounds of 4-chlorobenzylidenepyruvate with lanthanides preparation and thermal studies

Solid-state compounds Ln-4Cl-BP, where Ln represents lighter trivalent lanthanides and 4Cl-BP is 4-chlorobenzylidenepyruvate, were prepared. Thermogravimetry, derivative thermogravimetry (TG and DTG), differential scanning calorimetry (DSC) and other methods of analysis were used to characterize and to study the thermal behaviour of these compounds.

Contribution to the study of the solid-state reaction of mercury with pure rhodium

Thermogravimetry (TG) and other analysis techniques (EDX, SEM, Mapping surface, X-ray diffraction, inductively coupled argon plasma emission spectroscopy and atomic spectrometry with cold vapor generation) were used to study the reaction of Hg with Rh. The results permitted the suggestion that, when subjected to heat, an electrodeposited Hg film reacts with Rh to form intermetallic products with different stabilities, as indicated by at least three mass loss steps. In the first step, between room temperature and 160°C, only the bulk Hg is removed. From this temperature up to about 175°C, the mass loss can be attributed to the desorption of a film of metallic Hg. The last step, from 175 to 240°C, can be ascribed to the removal of Hg from a thin dark film of RhHg2.

Preparation and thermal decomposition of solid-state cinnamates of lighter trivalent lanthanides

Some new compounds of cinnamic acid with lighter trivalent lanthanides were prepared in the solid state. The compounds have general formula ML3·H2O, where L is cinnamate (C6H5-CH=CH-COO-) and M is La, Ce, Pr, Nd or Sm. Thermogravimetry, derivative thermogravimetry, differential scanning calorimetry, infrared absorption spectra and X-ray diffraction powder patterns were used to characterize and to study the thermal stability and thermal decomposition of these compounds.

Synthesis of manganese porphyrinosilica imprinted with templates using the sol-gel process

The optimized conditions for the preparation of a new manganese porphyrinosilica-template material are reported. The manganese porphyrinosilica-template was prepared by the sol-gel process, by the reaction of -SO2Cl groups present in the phenyl rings of MnTDC(SO2Cl)PPCl with 3-aminopropyltriethoxysilane. The reaction produces a precursor porphyrinopropylsilyl species, which were then polymerized with tetraethoxysilane. The presence of manganese porphyrin on xerogel is confirmed by ultraviolet visible absorption spectroscopy and thermogravimetric analysis (TGA). The prepared materials have surface areas between 19 and 674 m2 g-1. Electron spectroscopy imaging of the materials show that manganese distribution in the xerogel is uniform. Both manganese(III) porphyrinosilica-template and a similar iron(III) porphyrinosilica-template can catalyze the epoxidation of cyclooctene using iodozylbenzene as oxygen donor. The metalloporphyrinosilica-template presents catalytic activity similar to that of metaloporphyrin in solution. © 2000 Elsevier Science B.V. All rights reserved.

Thermal analysis of conductive blends of PVDF and poly(o-methoxyaniline)

The thermal behavior of blends of poly(vinylidene fluoride), or PVDF, and poly(o-methoxyaniline) doped with toluene sulfonic acid was studied by thermogravimetic analysis, electrical conductivity measurements, differential scanning calorimetry, X-ray diffraction and scanning electron microscopy. Blends with thermal and electrical conductivity stabler than the conductive polymer alone were obtained. Nevertheless, degradation occurs after a long period of time (500 h) at high temperatures. The possible association of the conductivity decay with dopant loss, degradation and structural and morphological changes of the blend is discussed. (C) 2000 Elsevier Science Ltd.

Characterization of curaua fiber

This paper describes the chemical, thermal and thermomechanical characterization of curaua fiber. The research of the thermal and thermomechanical properties of natural fibers is of major interest, considering their increasing utilization in several applications, and the large temperature range to which the fibers are submitted.

Preparation and characterization of BaBi2Nb2O9(BBN) ceramics synthetized by polymeric precursors method

Pure BBN powders and with addition of 1 and 2 wt% in excess of bismuth were obtained by Pechini Method. The powders calcined at 300°C/4h were analyzed by TG/DTA to study the temperature of organic matter decomposition. A systematic study of calcination temperature and time to the formation of the BBN phase was performed and the phase formation was accompanied by XRD. The calcined powders at 800°C during 2h were analyzed by infrared spectroscopy and by BET. The powders were isostaticaly pressed and sintered at temperatures ranging from 900°C to 1000°C. The ceramics were characterized by XRD to control the crystalline phase and by SEM to analyze the microstructure.

Borohidreto complexos de cobre (I) contendo difosfinas. Caracterização espectroscópica e comportamento térmico

Tetrahydroborate complexes of copper (I) with bidentate phosphines, [Cu(η 2-BH 4)(dppm)] (1), [Cu(η 2-BH 4)(dppe)] (2), [Cu(η 2-BH 4)(cis-dppet)] (3) and [Cu(η 2-BH 4)(dppb)] (4) (dppm = bis(diphenylphosphino)methane; dppe = 1,2-bis(diphenylphosphino) ethane; cis-dppet = 1,2-cis(diphenylphosphino)ethene; dppb = 1,4-bis(diphenylphosphino)butane) were prepared and characterized by elemental analysis, infrared spectroscopy, NMR and thermogravimetric analysis. The IR data for 1-4 showed bands typical of a bidentate coordination of BH 4 group to the copper atom and the 31P{ 1H} NMR spectra indicated that the phosphorous atoms are chelating the metal centre. The thermal behavior of the compounds was investigated and suggested that their thermal stability is influenced by the phosphines. Their thermal stability decreased as follows: [Cu(η 2-BH 4)(dppe)] (2) > [Cu(η 2-BH 4)(dppm)] (1) > [Cu(η 2-BH 4)(dppb)] (4) > [Cu(η 2-BH 4)(cis-dppet)] (3). According to thermal analysis and X-ray diffraction patterns all compounds decomposed giving Cu(BO 2) 2, CuO, CuO 2 and Cu as final products.

Structural study of aged saturated silica gels obtained from tetramethoxysilane sonohydrolysis with different water/tetramethoxysilane molar ratio

The structural characteristics of saturated silica sonogels were studied by means of small-angle x-ray scattering (SAXS) and thermogravimetric analysis (TG), after a long time of aging in saturated conditions. The sonogels were obtained by a sol-gel routine from ultrasound stimulated tetramethoxysilane (TMOS) hydrolysis carried out with the initial water/TMOS molar ratio (r) ranging from 2 to 10. The saturated sonogel structure can be described as composed by mass fractal-like aggregates (clusters) of primary silica particles, all imbibed in a liquid phase. The values of the mass fractal dimension (D) of the clusters was found all around 2.5, while the characteristic size of the clusters (ξ) was found generally increasing with r, going from approximately 2.3 nm (r = 2) to 4.5 nm (r = 10). The volume fraction of the clusters was estimated from the SAXS data. The results were compared to the values of weight loss fraction at the inflection point that has been found in the derivative of the TG curve, which should accounts for the instant in which the meniscus of the liquid phase penetrates into the clusters under a rapid evaporation process as in a TG test.