Quantitative Phase Analyses Through The Rietveld Method with X-Ray Powder Diffraction Data of Heat-Treated Carbamazepine Form III

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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.

Synthesis and crystal phase evaluation of hydroxylapatite using the rietveld-maximum entropy method

Bioceramic systems based on hydroxylapatite (HAP) are an important class of bioactive materials that may promote bone regeneration. The aim of this research was to evaluate how the stoichiometry of HAP influences its microstructural properties when diagnosed using the combined Rietveld method and Maximum entropy method (MEM). The Rietveld Method (RM) is recognizably a powerful tool used to obtain structural and microstructural information of polycrystalline samples analyzed by x-ray diffraction. Latterly have combined the RM with the maximum entropy method (MEM), with the goal of improve structural refinement results. The MEM provides high resolution maps of electron density and their analysis leave the accurate localization of atoms inside of unit cell. Like that, cycles Rietveld-MEM allow an excellent structural refinement In this work, a hydroxylapatite sample obtained by emulsion method had its structure refined using one cycle Rietveld-MEM with x-ray diffraction data. The indices obtained in initial refinement was Rwp = 7.50%, Re = 6.56%, S - 1.14% e RB = 1.03%. After MEM refinement and electron densities maps analysis to correction of atomics positions, the news indicators of Rietveld refinement quality was Rwp = 7.35%, Re = 6.56%, S = 1.12% and RB = 0.75%. The excellent result obtained to RB shows the efficiency of MEM as auxiliary in the refinement of structure of hydroxylapatite by RM.

A neural networks-based method for single-phase harmonic content identification

A neural method is presented in this paper to identify the harmonic components of an ac controller. The components are identified by analyzing the single-phase current waveform. The method effectiveness is verified by applying it to an active power filter (APF) model dedicated to the selective harmonic compensation. Simulation results using theoretical and experimental data are presented to validate the proposed approach. © 2008 IEEE.

Harmonic content identification based on neural method for single phase power systems

An alternative method is presented in this paper to identify the harmonic components of non-linear loads in single phase power systems based on artificial neural networks. The components are identified by analyzing the single phase current waveform in time domain in half-cycle of the ac voltage source. The proposed method is compared to the fast Fourier transform. Simulation and experimental results are presented to validate the proposed approach.

Mechanisms of phase formation along the synthesis of Mn-Zn ferrites by the polymeric precursor method

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Acute phase proteins: a potential approach for diagnosing chronic infection by Trypanosoma vivax

O objetivo do presente estudo foi verificar possíveis alterações nas proteínas de fase aguda em ovinos infectados experimentalmente com Trypanosoma vivax. Para tanto, foram utilizados oito ovinos machos, sendo quatro usados como controle e quatro infectados com 10(5) tripomastigotas de T. vivax. Colheram-se amostras de sangue em dois tempos antes da infecção e, posteriormente, aos 5, 7, 9, 11, 13, 15, 20, 30, 45, 60, 75, 90, 105 e 120 dias após a infecção (dpi); após centrifugação e aliquotização das amostras. As proteínas de fase aguda foram separadas por eletroforese em gel de acrilamida, contendo dodecil sulfato de sódio, e suas concentrações foram determinadas através de densitometria computadorizada. A dosagem de proteína total foi realizada pelo método colorimétrico do biureto. A contagem dos tripanossomas foi realizada diariamente, utilizando-se uma alíquota de 5 µL de sangue disperso em lâmina de microscopia, sob lamínula de 22 × 22 mm, contando-se os parasitos em 100 campos microscópicos, com objetiva de 40×, multiplicados pelo fator de correção do microscópio, e o resultado expresso em parasitos por mL de sangue. Para a análise estatística, empregou-se o teste de Wilcoxon a 5% de probabilidade. Foi observada a diminuição de diversas proteínas de fase aguda e aumento de antitripsina e transferrina que podem ser utilizadas para auxiliar no diagnóstico da infecção por T. vivax, principalmente na fase crônica da infecção.

A Study of Compost Added to a Casing Technique in Agaricus bisporus Cultivation from Phase III Bulk Compost

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Photoluminescence of barium-calcium titanates obtained by the microwave-assisted hydrothermal method (MAH)

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Application of an HPLC method for analysis of propolis extract

Propolis obtained from honeybee hives has been widely used in medicine, cosmetics, and industry due to its versatile biological activities (antioxidant, antimicrobial, fungicidal, antiviral, antiulcer, immunostimulating, and cytostatic). These activities are mainly attributed to the presence of flavonoids in propolis, which points out the interest in quantifying these constituents in propolis preparations, as well as validation of analytical methodologies. High-performance liquid chromatography (HPLC) methods have been reported to quantify isolated flavonoids or these compounds in complex biological matrices, such as herbal raw materials and extractive preparations. An efficient, precise, and reliable method was developed for quantification of propolis extractive solution using HPLC with UV detection. The chromatograms were obtained from various gradient elution systems (GES) tested in order to establish the ideal conditions for the analysis of propolis extractive solution, using methanol and water: acetonitrile (97.5 : 2.5, v/v) as mobile phase. Gradient reversed phase chromatography was performed using a stainless steel column (250 x 4.6 mm i.d., 5 mum) filled with Chromsep RP 18 (Varian), column temperature at 30.0 +/- 0.1degreesC and detection at 310 nm. The main validation parameters of the method were also determined. The method showed linearity for chrysin in the range 0.24-2.4 mug mL(-1) with good correlation coefficients (0.9975). Precision and accuracy were determined. The obtained results demonstrate the efficiency of the proposed method. The analytical procedure is reliable and offers advantages in terms of speed and cost of reagents.

Reversed phase HPLC determination of zidovudine in rat plasma and its pharmacokinetics after a single intranasal dose administration

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Development of a new high-performance liquid chromatographic method for the determination of ceftazidime

A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanol-water (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 mu g/mL. The values for interday and intraday precision (relative standard deviation) were < 1 %. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.

Development and validation of an analytical method by RP-HPLC for quantification of sibutramine hydrochloride in pharmaceutical capsules

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Development and validation of HPLC method for analysis of dexamethasone acetate in microemulsions

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Structural phase transition study of FePt alloys using ab initio calculation

The FePt alloy undergoes the cubic to tetragonal lattice transformation in the ferromagnetic state. We calculated the electronic structure for both cubic and tetragonal structures using the FPLAPW method with APW + lo. Comparing the density of states of the cubic and tetragonal structures, it is expected that the lattice transformation is caused by the band Jahn-Teller effect. (C) 2009 Elsevier B.V. All rights reserved.