A thermal behaviour study of solid-state cinnamates of the latter trivalent lanthanides and yttrium(III)

Some new compounds of cinnamic acid with the latter trivalent lanthanides and yttrium(III) were synthesized in the solid state. The compounds have the general formula LnL3, where Ln represents trivalent Eu to Lu or Y ions and L is the cinnamate anion (C6H5-CH=CH-COO-). Thermogravimetry (TG), derivative thermogravimetry (DTG), differential scanning calorimetry (DSC), infrared absorption spectra and X-ray diffraction powder patterns were used to characterize and to study the thermal behaviour of these compounds. © 2002 Elsevier Science B.V. All rights reserved.

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.

Thermogravimetric studies of the decomposition kinetics of four different Hevea rubber clones using Ozawa's approach

Thermal degradation of natural rubber extracted from four different rubber clones of the Hevea brasiliensis species was investigated by thermogravimetry using Ozawa's approach to assess the kinetic parameters of the decomposition process. The results are discussed in terms of the order of reaction, kinetic parameters such as activation energy as a function of conversion degree, and thermal stability for each of the clones.

Thermal Behavior and Spectroscopic Study of Neutral and Cationic Mononuclear Cyclopalladated Compounds

The reactions of the precursor [Pd(N,C-dmba)(MeCN)2](NO 3) (1) (dmba = N,N-dimethylbenzylamine), with the proligands 3,5-dimethylpyrazole (Hdmpz), 2-quinolinethiol (qnSH) and 1,1′- bis(diphenylphosphine)ferrocene (dppf) afforded the compounds [Pd(N,C-dmba)(Hdmpz)(ONO2)]0.5CH2Cl2 (2), [Pd(N,C-dmba)(qnSH)(ONO2)] 0.5CH2Cl2 (3) and [Pd(N,C-dmba)(dppf)](NO3) (4), respectively. The mononuclear species 2,3 and 4 were characterized by elemental analysis, infrared spectroscopy, NMR and thermogravimetric analysis. The IR spectra show bands which are consistent with terminal monodentate nitrate group for 2-3 and ionic nitrate for 4. The 1H and 13C NMR data confirm that coordination of the organic ligands has occurred and the 31P{1H} NMR data for 4 clearly evidences the occurrence in solution of three cyclopalladated species with the dppf acting as a bridging ligand in two cases and as a chelate in one. The thermal behavior of compounds 1-4 suggests that complex 2 is the most stable. The X-ray diffractometry results show the formation of PdO from 1 and 2, Pd2OSO4 from 3, and of a mixture of PdO and Fe 2(PO4)3 from 4, as final decomposition products.

Synthesis, characterization and thermal behaviour of solid-state compounds of 4-methoxybenzoate with some bivalent transition metal ions

Solid-state M-4-MeO-Bz compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and 4-MeO-Bz is 4-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry-differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, elemental analysis and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to have information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds. © 2005 Akadémiai Kiadó, Budapest.

Thermal study of nickel(II) pyrazolyl complexes

The thermal behavior of the pyrazolyl complexes [NiCl2(HPz) 4] (1), [Ni(NCS)2(HPz)4] (2), [NiCl 2(HdmPz)4]·2H2O (3) and [Ni(NCS) 2(HdmPz)4]·2H2O (4) (HPz=pyrazole, HdmPz=3,5-dimethylpyrazole) has been studied by thermogravimetry (TG) and differential thermal analysis (DTA). The TG data indicated that the thermal stability of [NiX2(HL)4] (X=Cl, NCS) compounds varies depending on the pyrazolyl ligand in the following order HL=HPz>HdmPz. From the thermal decomposition of 3 and 4 it was possible to isolate the intermediate compounds [Ni(μ-Cl)2(HdmPz)2] (3a) and [Ni(μ-1,3-NCS) 2(HdmPz)2] (4a), respectively. The final products of the thermal decompositions of 1-4 were identified as NiO by X-ray powder diffraction. © 2005 Akadémiai Kiadó, Budapest.

Study of the thermo-mechanical and electrical properties of conducting composites containing natural rubber and carbon black

This work shows the preparation and characterization of composites obtained by mixing natural rubber (NR) and carbon black (CB) in different percentages aiming suitable mechanical properties, processability and electrical conductivity for future applications as transducers in pressure sensors. The composites NR/CB are characterized through dc conductivity, thermal analysis using differential scanning calorimetry (DSC), dynamic mechanical thermal analysis (DMA), thermogravimetry (TGA) and stress-strain test. The electrical conductivity changed from 10-9 to 10 Sm-1 depending on the percentage of CB in the composite. Besides, it was found a linear (and reversible) dependence of the conductivity on the applied pressure in the range from 0 to 1.6 MPa for the sample 80/20 (NR/CB wt%).

Changes on degree of conversion of dual-cure luting light-cured with blue LED

The indirect adhesive procedures constitute recently a substantial portion of contemporary esthetic restorative treatments. The resin cements have been used to bond tooth substrate and restorative materials. Due to recently introduction of the self-bonding resin luting cement based on a new monomer, filler and initiation technology has become important to study the degree of conversion of these new materials. In the present work the polymerization reaction and the filler content of dual-cured dental resin cements were studied by means of infra-red spectroscopy (FT-IR) and thermogravimetry (TG). Twenty specimens were made in a metallic mold (8 mm diameter × 1 mm thick) from each of 2 cements, Panavia® F2.0 (Kuraray) and RelyX™ Unicem Applicap (3M/ESPE). Each specimen was cured with blue LED with power density of 500 mW/cm 2 for 30 s. Immediately after curing, 24 and 48 h, and 7 days DC was determined. For each time interval 5 specimens were pulverized, pressed with KBr and analyzed with FT-IR. The TG measurements were performed in Netzsch TG 209 under oxygen atmosphere and heating rate of 10°C/min from 25 to 700°C. A two-way ANOVA showed DC (%) mean values statistically significance differences between two cements (p < 0.05). The Tukey's test showed no significant difference only for the 24 and 48 h after light irradiation for both resin cements (p > 0.05). The Relx-Y™ Unicem mean values were significantly higher than Panavia® F 2.0. The degree of conversion means values increasing with the storage time and the filler content showed similar for both resin cements. © 2009 Pleiades Publishing, Ltd.

Thermal behaviour of succinic acid, sodium succinate and its compounds with some bivalent transitions metal ions in dynamic N 2 and CO 2 atmospheres

Thermal stability and thermal decomposition of succinic acid, sodium succinate and its compounds with Mn(II), Fe(II), Co(II), Ni(II), Cu(II) and Zn(II) were investigated employing simultaneous thermogravimetry and differential thermal analysis (TG-DTA) in nitrogen and carbon dioxide atmospheres and TG-FTIR in nitrogen atmosphere. On heating, in both atmospheres the succinic acid melt and evaporate, while for the sodium succinate the thermal decomposition occurs with the formation of sodium carbonate. For the transition metal succinates the final residue up to 1180 °C in N 2 atmosphere was a mixture of metal and metal oxide in no simple stoichiometric relation, except for Zn compound, where the residue was a small quantity of carbonaceous residue. For the CO 2 atmosphere the final residue up to 980 °C was: MnO, Fe 3O 4, CoO, ZnO and mixtures of Ni, NiO and Cu, Cu 2O.

Novel cellulose/NbOPO 4.nH 2O hybrid material from sugarcane bagasse

In recent years studies concerning the applications of lignocellulosic/ inorganic couples have resulted in the development of an interesting class of functional materials. In this work a cellulose/NbOPO 4.nH 2O hybrid using cellulose from surgacane bagasse was prepared and characterized in order to test for adsorption applications. The preparation process was conducted by carrying out metallic niobium dilution in hydrofluoric acid in the presence of nitric acid, then adding boric acid to form the complex and, finally, the cellulose sugar cane bagasse was added. Concentrated phosphoric acid was also inserted to precipitate hydrous niobium phosphate particles in the cellulose fiber. This material was characterized by X-ray diffractometry (XRD), thermogravimetry (TG/DTG), and scanning electronic microscopy (SEM) connected to an energy dispersive spectrophotometer (EDS). Results by SEM/EDS show that NbOPO 4.nH 2O was present in structure of the cellulose. During the preparation of the material, using boric acid it was observed that the formation of precipitate occurred in a shorter time than the material prepared without boric acid.

Thermo-gravimetric analysis (TGA) after different exposures of high density polyethylene (HDPE) and poly vinyl chloride (PVC) geomembranes

This paper presents the results of thermogravimetric analysis (TGA) tests in PVC (1.0; 2.0 mm) and HDPE (0.8; 2.5 mm) geomembranes exposed to weathering and leachate after 30 months. The aim of this paper is the comparison of fresh and exposed samples to assess the degradation process concerning the total loss of mass of geomembranes. The exposure was conducted in accordance with the recommendations of ASTM standards. The TGA tests were carried out according to ASTM D6370 and E2105. Results show, for instance, that for PVC geomembrane the largest reductions of plasticizers occurred for samples exposed to weathering. The loss of plasticizers after the exposure contributed to the decrease of deformation and consequent increase in stiffness. TGA tests shows to be a valuable tool to control the quality of the materials. © 2012 ejge.

Synthesis, characterization and thermal study of solid mandelate of some bivalent transition metal ions in CO2 and N2 atmospheres

Solid state M-L, where M stands for bivalent transition metals (Mn(II), Fe(II), Co(II), Ni(II), Cu(II) and Zn(II)) and L is mandelate, were synthesized. Simultaneous thermogravimetry and differential scanning calorimetry, elemental analysis and complexometry were used to establish the stoichiometry and to study the thermal behaviour of these compounds in CO2 and N2 atmospheres. The results show that all the compounds were obtained in the anhydrous state and in agreement with the general formula ML2. The thermal decomposition of the compounds occurs in a single (Cu(II)), two (Ni(II)) three (Fe(II), Co(II)), four (Mn(II)) and five (Zn(II)) steps. The results also provided information concerning the ligand's denticity, thermal behaviour, final residues and identification of gaseous products evolved during the thermal decomposition of these compounds. © 2012 Akadémiai Kiadó, Budapest, Hungary.

Thermal and spectroscopic studies of solid oxamate of light trivalent lanthanides

Solid-state LnL3·1.25H2O compounds, where L is oxamate and Ln is light trivalent lanthanides, have been synthesized. Simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), experimental and theoretical infrared spectroscopy, TG-DSC coupled to FTIR, elemental analysis, complexometry, and X-ray powder diffractometry were used to characterize and to study the thermal behavior of these compounds. The results led to information about the composition, dehydration, thermal stability, thermal decomposition, and gaseous products evolved during the thermal decomposition of these compounds in dynamic air atmosphere. The dehydration occurs in a single step and through a slow process. The thermal decomposition of the anhydrous compounds occur in a single (Ce), two (Pr), and three (La, Nd to Gd) steps with the formation of the respective oxides, CeO2, Pr 6O11, and Ln2O3 (Ln = La, Nd to Gd). The theoretical and experimental spectroscopic study suggests that the carboxylate group and amide carbonyl group of oxamate are coordinate to the metals in a bidentate chelating mode. © 2012 Akadémiai Kiadó, Budapest, Hungary.

The thermal, rheological and structural properties of cassava starch granules modified with hydrochloric acid at different temperatures

Starch is arguably one of the most actively investigated biopolymer in the world. In this study, the native (untreated) cassava starch granules (Manihot esculenta, Crantz) were hydrolyzed by standard hydrochloric acid solution at different temperatures (30 °C and 50 °C) and the hydrolytic transformations were investigated by the following techniques: simultaneous thermogravimetry-differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), as well as non-contact atomic force microscopy (NC-AFM), X-ray diffraction (XRD) powder patterns, and rapid viscoamylographic analysis (RVA). After the treatment with hydrochloric acid at different temperatures, the thermal stability, a gradual loss of pasting properties (viscosity), alterations in the gelatinization enthalpy (ΔHgel), were observed. The use of NC-AFM and XRD allowed the observation of the surface morphology and topography of the starch granules and changes in crystallinity of the granules, respectively. © 2012 Elsevier B.V. All rights reserved.

Thermal behavior of some antihistamines

Thermogravimetry (TG), differential scanning calorimetry (DSC), polarized light thermal microscopy (PLTM), as well as X-ray powder diffraction (XRD) and Fourier transformed infrared spectroscopy (FTIR) were used to study the thermal behavior and the chemical structure of cimetidine, famotidine, ranitidine-HCl, and nizatidine. The TG-DSC curves show that the famotidine and ranitidine-HCl suffer decomposition during melting and they are thermally less stable in comparison with cimetidine and nizatidine, the latter being the most stable of all the drugs studied in this study. The DSC curves of famotidine and ranitidine-HCl show exothermic peaks immediately after the melting, confirming the occurrence of thermal decomposition. The DSC curves also show that the cimetidine and nizatidine have some thermal stability after melting. The thermal events shown in the PLTM images are consistent with the results shown in the TG-DSC and DSC curves. The XRD patterns show that the cimetidine and famotidine are less crystalline compared with ranitidine-HCl and nizatidine. The theoretical FTIR bands are in agreement with those obtained experimentally, and in some cases, no difference is observed between the theoretical and experimental values, even being identical in one of the cases. © 2012 Akadémiai Kiadó, Budapest, Hungary.