954 resultados para differential calorimetric analysis
Resumo:
This paper was prepared a polymorphic from of curcumin a natural bioactive compound widely used in Indian medicine in the treatment of a range of illnesses. The preparation was the polymorphic crystallization process and solvent mixtures of organic solvents in order to change the dielectric constant of the solution to obtain crystals. The crystal of curcumin has been studied and characterized by absorption spectroscopic in the infrared, X-ray diffraction powder method and by thermo analytical techniques: thermogravimetry and differential therma analysis (TG-DTA) and differential scanning calorimetry (DSC). The DSC of the pure compound (MP=180,19ºC) showed some differences compared the compound crystallized (MP=176.63ºC) in a mixture of solvents thus indicating the phenomenon of polymorphism, and TG-DTA curve of the compound crystallized showed that this was not a solvatomorphic. Finnally the techniques of X-ray diffraction technique FTIR and powder showed a structural change in the compound crystallized, profile-based graphics when compared to the pure compound, which proves that the compound crystallized it is a polymorph
Resumo:
In this study, the drug indomethacin, a non-steroidal anti-inflammatory indoleacetic acid derivative and the complex of indomethacin and lanthanum (III) in solid form were synthesized and characterized by Thermogravimetry (TGA), Differential Thermal Analysis (DTA), Differential Scanning Calorimetry (DSC) and powder X-ray diffractometry (XRD), infrared vibrational spectroscopy by diffuse reflectance (FTIR) and complexometric titration with EDTA. With the TG curves it was possible to determine the stoichiometry of the complex as La(Ind)3·3.5H2O where Ind is the drug indomethacin. The result of thermal analyzes provided information on the thermal stability, enthalpy of dehydration and thermal behavior of the compounds. The infrared spectrum and with the aid of theoretical calculations suggests that the indomethacin is coordinated by the carboxylate group in the bidentate mode
Resumo:
Bi3NbO7 thin films were prepared by the polymeric precursor method. The precursor solutions were prepared with excess of bismuth ranging from 0% to 10% and the pH was controlled to be maintained between 8 and 9. This control was done by adding to the solution niobium and ethylene glycol. The final solution was clear and free of precipitation. After obtaining the precursor solution, has begun the process of characterization of powders with thermogravimetry (TG), differential thermal analysis and X-ray analysis (XRD). The films were obtained by the polymeric precursors, the method is advantageous because it is simple, and low cost involves steps and controlled stoichiometry. The films were annealed and characterized by XRD and SEM and also characterized according to their dialectics properties. We observed that the best results were obtained when the film is thermally at 800 ° C for two hours and 860 ° C for two hour. Under these conditions we obtain Bi3NbO7 thin films with good homogeneity, uniform distribution of the grains, but with the formation of secondary phase, which does not occur in treatments with lower temperature. The dielectric characterization showed that the produced film showed good characteristics with high dielectric constant and low loss
Resumo:
Pós-graduação em Química - IQ
Resumo:
Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
Resumo:
Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
Resumo:
Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
Resumo:
Solid state chelates of general formula H-2[M(EDTA)] . nH2O, where M is Co, Ni, Cu or Zn, and EDTA is ethylenediaminetetraacetate, were prepared. Thermogravimetry-derivative thermogravimetry (TG-DTG), differential thermal analysis (DTA) and complexometry were used to characterize and to study the thermal stability and thermal decomposition of these compounds.
Resumo:
Thermogravimetry, differential thermal analysis, differential scanning calorimetry, IR absorption spectroscopy, X-ray diffraction, and other methods of analysis have been used in the characterization and study of the thermal decomposition of the basic carbonate hydrates of lanthanides and yttrium. These compounds were obtained by precipitation from homogeneous solutions via the hydrolysis of urea, without the addition of an auxiliary anion. The results show that the TG and DTA curves are characteristic for each compound. The results also permit suggestions concerning the compositions and mechanisms of thermal decomposition of these compounds. © 1989.
Resumo:
The synthesis of calcium titanate, CaTiO3, was performed by mechanical activation and thermal treatment. Milling for up to 360 minutes in a planetary ball mill mechanically activated an equimolar mixture of CaCO 3 and TiO2 powders. A small amount of mechanically activated mixtures was pressed into briquettes and calcined at 850°C for two hours. The effect of mechanical activation on the solid-state reaction was studied using X-ray powder diffraction and differential thermal analysis. The change of morphology and size of powder particles due to milling, were determined by SEM, while BET analysis was used to determine the specific surface area of the powder. The sintering process was followed by a dilatometer during thermal treatment up to 1300°C. The main conclusion of the analysis of conducted investigations is that CaTiO3 ceramics can be obtained from an activated mixture at a much lower temperature than reported in the literature owing to acceleration of the chemical reaction and sintering.
Resumo:
Solid state Ln-4-Me-BP compounds, where Ln stands for heavier trivalent lanthanides (gadolinium to lutetium) and yttrium(III) and 4-Me-BP is 4-methylbenzylidenepyruvate (CH3-C6H4-CH=CH-COCOO-), have been synthesized. Elemental analysis, complexometry, X-ray powder diffractometry, infrared spectroscopy and simultaneous thermogravimetry-differential thermal analysis (TG-DTA), have been used to characterise and to study the thermal behaviour of these compounds. The results provided information concerning the stoichiometry, crystallinity, ligand's denticity, thermal stability and thermal decomposition. © 2002 Elsevier Science B.V. All rights reserved.
Resumo:
The basic carbonates of lanthanum with 10%, 20%, 50% and 80% of europium were prepared by precipitation from homogeneous solutions via the hydrolysis of urea, without the addition of an auxiliary anion, at two different temperatures. Elemental analysis, complexometric methods, X-ray diffraction patterns, solid state IR absorption, thermogravimetry/derivative thermogravimetry (TG/DTG) and differential thermal analysis (DTA) were used to characterise the compounds and study their thermal behaviour.
Resumo:
Thermogravimetry (TG) up to 900°C, differential thermal analysis (DTA) up to 1100°C and gravimetric data up to 1200°C, have been used to study the thermal decomposition of ammonium selenate and of the double selenates of lanthanides, and yttrium, and ammonium. The results provided the composition and thermal stability and also an interpretation of the thermal decomposition mechanisms. © 1994.
Resumo:
Solid state chelates of general formula H[Ln(EDTA)] · nH2O (Ln = trivalent lanthanide (except for promethium) or yttrium; EDTA = ethylenediaminetetraacetate) were prepared. Thermogravimetry, differential thermal analysis. X-ray diffraction and complexometry were used to characterize and study the thermal stability and thermal decomposition of these compounds. © 1993.
Resumo:
Pechini's method has been successfully used to prepare Li-doped MgNb2O6(MN) at short time and low temperature. It consists in the preparation of metal citrate solution, which is polymerized at 250°C to form a high viscous resin. This resin was burned in a box type furnace at 400°C/2h and ground in a mortar. Successive steps of calcination up to 900°C were used to form a crystalline precursor. SEM, DTA and XRD were used to characterize the powders. MN precursor powders containing from 0.1 to 5.0 mol% of LiNbO3 additive was prepared aiming better dielectric properties and microstructural characteristics of the PMN prepared from columbite route. SEM analysis showed that particles increased by sintering, forming large agglomerates. The surface area is also substantially reduced with the increase in additive amount above 1.0 mol%. In XRD pattern of the precursor material with 5.0 mol% of additive was observed the LiNbO3 phase of trigonal structure. XRD data were used for Rietveld refinement and a decrease in microstrain and pronounced increase in crystallite size with the increase of LiNbO3 were observed. It is in agreement with the particle morphologies observed by SEM analysis.