913 resultados para Fourier and Laplace Transforms
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In this paper, we report a detailed structural and electronic characterization of PbMoO4 crystals by using a conventional hydrothermal (CH) method. The samples were characterized by X-ray diffraction (XRD), Fourier transform Raman (FT-Raman), field-emission gun scanning electron microscopy (FEG-SEM) and photoluminescence (PL) measurements. In addition, first-principles quantum mechanical calculations based on the density functional theory were employed in order to understand the band structure and density of states for the PbMoO4. Analysis of both theoretical and experimental results allows to rationalize the role of order-disorder effects in the observed green PL emissions in these ordered powders.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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This paper reports on the development and validation of a simple and sensitive method that uses solid phase extraction (SPE) and liquid chromatography with ultraviolet detection to analyze fluoxetine (FLX) and norfluoxetine (NFLX) in human plasma samples. A lab-made C18 SPE phase was synthesized by using a sol–gel process employing a low-cost silica precursor. This sorbent was fully characterized by nuclear magnetic resonance (NMR), Fourier-transform infrared spectroscopy (FT-IR), and scanning electron microscopy (SEM) to check the particles' shape, size and C18 functionalization. The lab-made C18 silica was used in the sample preparation step of human plasma by the SPE-HPLC-UV method. The method was validated in the 15 to 500 ng mL 1 range for both FLX and NFLX using a matrix matched curve. Detection limits of 4.3 and 4.2 ng mL 1 were obtained for FLX and NFLX, respectively. The repeatability and intermediary precision achieved varied from 7.6 to 15.0% and the accuracy ranged from 14.9 to 9.1%. The synthesized C18 sorbent was compared to commercial C18 sorbents. The average recoveries were similar (85–105%), however the lab-made C18 silica showed fewer interfering peaks in the chromatogram. After development and validation, the method using the lab-made C18 SPE was applied to plasma samples of patients under FLX treatment (n ¼ 6). The concentrations of FLX and NFLX found in the samples varied from 46.8–215.5 and 48.0–189.9 ng mL 1 , respectively.
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The electrooxidation of hydroxylamine, NH2OH, in 0.1 M phosphate buffer (PB, pH = 7) on Pt-, and Pd-modified Au electrodes prepared by galvanic displacement of underpotential deposited Cu, was investigated by electrochemical techniques and three and in situ vibrational probes, substrate-induced surface enhanced Raman scattering, SI-SERS, surface enhanced infrared absorption, SEIRAS, and Fourier transform infrared reflection-absorption, IRAS, spectroscopies. Analyses of the results obtained made it possible to identify at low overpotentials, solution phase (sol) and adsorbed (ads) nitric oxide, NO, as well as solution phase nitrous oxide, N2O. As the potential was increased, the peak(s) ascribed to NO(ads) gained in intensity and new features associated with NO2−(ads) and NO2−(sol) were clearly discerned. Further excursion toward higher potentials yielded an additional peak assigned to NO2(ads). This behavior is analogous to that found for bare Au electrodes in a potential region in which the metal is at least partially oxidized under otherwise the same experimental conditions.
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Objective: This study aims to evaluate the degree of conversion (DC) and hydrolytic degradation through the Vickers hardness test (HV) of a nanofilled (Filtek™ Z-250, 3M) and a microhybrid (Filtek™Supreme-XT, 3M) composite resin. Materials and methods: Eight disk-shaped specimens (4 mm diameter × 2 mm thick, ISO 4049) of each material were prepared for each test. Composites were inserted into single increment in a metallic matrix and light-cured for 40 seconds. VH readings were performed for each specimen at predetermined intervals: immediately after polymerization (control), 1, 2, 3, 7, 14, 21, 30 and 180 days. After curing, initial hardness measurements were performed and the specimens were immersed in artificial saliva at 37°C. For DC (%), specimens were ground, pressed with KBr and analyzed by FT-IR spectrophotometer. Results: Student t-test showed that there was no difference between the resins for DC (p = 0.252). ANOVA analysis revealed that Z-250 VH means were all greater than S-XT, for both top and bottom surfaces, whatever the storage-period in artificial saliva (p < 0.001). After 180 days of storage, the hardness obtained for S-XT was similar with that at the baseline, for both top and bottom surfaces. While for Z-250 hardness was not significantly different from baseline only for top surface, but there was a significant decrease observed in hardness for bottom surface. Conclusion: The materials tested showed no evidence of hydrolytic degradation in a significant way, in a 6-month storagetime in artificial saliva. Nanofilled resin presents a monomer conversion comparable to the conventional microhybrid.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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The purpose of this study was to characterize and to evaluate the bioactivity potential of experimental root canal sealers (ES) based on Portland cement, epoxy resin with nano- and micro-particles of niobium or zirconium oxide used as radiopacifiers in comparison to AH Plus and MTA Fillapex. Methods Specimens of the sealers (10 mm in diameter × 1 mm thick) were prepared and the radiopacity was evaluated according to ISO 6876 (2012) specifications. Characterization of the sealers was performed under the scanning electron microscope (SEM) immediately after setting and after immersion for 28 days in Hank's balanced salt solution (HBSS). In addition X-ray energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy were also performed. The pH and calcium ion release were measured after 1, 7, 14, 21 and 28 days after completion of seating using a digital pH meter and an atomic absorption spectrophotometer, respectively. Results The experimental sealers exhibited an average radiopacity of 2.5 mm thickness of aluminum, which was similar to MTA Fillapex (P > 0.05) and inferior to AH Plus (P < 0.05). AH Plus did not show bioactivity. Although the experimental sealers did not exhibit the formation of hydration product, they encouraged the deposition of crystalline spherical structures of calcium deficient phosphate. The highest pH and calcium release values were observed with the experimental sealers (P < 0.01). ES-Nb-micro was the only sealer to present hexagonal shaped crystal deposition. Significance Novel root canal sealers based on a mixture of Portland cement, epoxy resin and radiopacifier exhibited a degree of bioactivity although no evidence of cement hydration was demonstrated on material characterization. The radiopacifier particle size had limited effect on the sealer microstructure and chemical properties.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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The anticancer drug paclitaxel was encapsulated into a bio-nanocomposite formed by magnetic nanoparticles, chitosan and apatite. The aim of this drug carrier is to provide a new perspective against breast cancer. The dynamics of the pure and encapsulated drug were investigated in order to verify possible molecular changes caused by the encapsulation, as well as to follow which interactions may occur between paclitaxel and the composite. Fourier transformed infrared spectroscopy, thermal analysis, inelastic and quasi-elastic neutron scattering experiments were performed. These very preliminary results suggest the successful encapsulation of the drug.
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
Structural and optical properties of Er3+ doped SiO2-Al2O3-GeO2 compounds prepared by a simple route
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)