934 resultados para Direct modified method
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This study aims to demonstrate how the chemical homogeneity of B cations affects the microstructure and electrical responses of (1-x) PMN-xPT ceramics. Two methodologies were employed to synthesize three different compositions, with x assuming the values 0.10, 0.28, and 0.35. If compared to conventional method, the Ti-modified columbite route, which is characterized by higher B cation homogeneity, leads to PMN-PT powders and ceramics with lower content of PNT pyrochlore phase and, for 0.65PMN-0.35PT composition, minor amount of tetragonal phase is found. Conclusively, PMN-PT ceramics obtained by modified route favors B cations homogeneity, enhancing the dielectric, ferroelectric and piezoelectric properties.
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This work describes a modified sol-gel method for the preparation of V2O5/TiO2 catalysts. The samples have been characterized by N-2 adsorption at 77 K, X-ray Diffractometry (XRD), Scanning Electronic Microscopy (SEM/EDX) and Fourier Transform Infrared Spectroscopy (FT-IR). The surface area increases with the vanadia loading from 24 m(2) g(-1) for pure TiO2 to 87 m(2) g(-1) for 9 wt% of V2O5. The rutile form is predominant for pure TiO2 but becomes enriched with anatase phase when vanadia loading is increased. No crystalline V2O5 phase was observed in the diffractograms of the catalysts. Analysis by SEM showed heterogeneous granulation of particles with high vanadium dispersion. Two species of surface vanadium were observed by FT-IR spectroscopy: a monomeric vanadyl and polymeric vanadates. The vanadyl/vanadate ratio remains practically constant. Ethanol oxidation was used as a catalytic test in a temperature range from 350 to 560 K. The catalytic activity starts around 380 K. For the sample with 9 wt% of vanadia, the conversion of ethanol into acetaldehyde as the main product was approximately 90% at 473 K.
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Solid paraffin-based carbon paste electrodes modified with 2-aminothiazole organofunctionalized silica have been applied to the anodic stripping determination of copper ions in ethanol fuel samples without any sample treatment. The proposed method comprised four steps: (1) copper ions preconcentration at open circuit potential directly in the ethanol fuel sample; (2) exchange of the solution and immediate cathodic reduction of the absorbate at controlled potential; (3) differential pulse anodic stripping voltammetry; (4) electrochemical surface regeneration by applying a positive potential in acid media. Factors affecting the preconcentration, reduction and stripping steps were investigated and the optimum conditions were employed to develop the analytical procedure. Using a preconcentration time of 20 min and reduction time of 120 s at -0.3 V versus Ag/AgCl(sat) a linear range from 7.5 x 10(-8) to 2.5 x 10(-6) mol L(-1) with detection limit of 3.1 x 10(-8) mol L(-1) was obtained. Interference studies have shown a decrease in the interference effect according to the sequence: Ni > Zn > Cd > Pb > Fe. However, the interference effects of these ions have not forbidden the application of the proposed method. Recovery values between 98.8 and 102.3% were obtained for synthetic samples spiked with known amounts of Cu(2+) and interfering metallic ions. The developed electrode was successfully applied to the determination of Cu(2+) in commercial ethanol fuel samples. The results were compared to those obtained by flame atomic absorption spectroscopy by using the F-test and t-test. Neither F-value nor t-value have exceeded the critical values at 95% confidence level, confirming that there are no significant differences between the results obtained by both methods. (c) 2006 Elsevier B.V. All rights reserved.
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This work describes the synthesis and characterization of 2-aminothiazole-modified silica gel (SiAT), as well as its application for preconcentration (in batch and column technique) of Cu(II), Ni(II) and Zn(II) in ethanol medium. The adsorption capacities of SiAT determined for each metal ion were (mmol g(-1)): Cu(II)=1.20, Ni(II)=1.10 and Zn(II)=0.90. In addition, results obtained in flow experiments, showed a recovery of ca. 100% of the metal ions adsorbed in a column packed with 500 mg of SiAT. The eluent was 2.0 mol L-1 HCl. The sorption-desorption of the studied metal ions made possible the development of a preconcentration method for metal ions at trace level in fuel ethanol using flame AAS for their quantification.
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This study proposes to synthesize (1-x)PMN-xPT powders, where 0.10 < x < 0.45, using the T-modified columbite route. This methodology consists in the preparation of the MNT columbite precursor via the polymeric precursor method, followed by the solid state reaction with PbO to get the PMN-PT powders. It was verified that from 15 mol% of Ti, the MNT presents the coexistence of two main phases with different crystal symmetry: Rutile and Columbite. However, the synthesis of (1-x)PMN-xPT powders is not affected by this event. A detailed study of structural effects in MNT and PMN-PT powders as function of Ti content was made using the Rietveld method. It was also demonstrated that powders possess high chemical and microstructural homogeneity.
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The effects of silver insertion on the TiO(2) photocatalytic activity for the degradation of diclofenac potassium were reported here. Techniques such as X-ray diffraction, scanning electron microscopy and UV-Vis spectroscopy were used to comprehend the relation between structure and properties of the silver-modified TiO(2), thin films obtained by the sol-gel method. The lattice parameters and the crystallinity of TiO(2) anatase phase were affected by inserted silver, and the film thickness increased about 4 nm for each 1 wt.% of silver inserted. The degradation of diclofenac potassium and by-products reached an efficiency of 4.6 mg(C) W(-1) when the material was modified with silver. Although the first step of degradation involves only the photochemical process related to the loss of the chlorine and hydrogen atoms. This cyclization reaction leads to the formation of intermediate, which degradation is facilitated by the modified material. (C) 2007 Elsevier B.V. All rights reserved.
A simple method for estimating global DNA methylation using bisulfite PCR of repetitive DNA elements
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We report a method for studying global DNA methylation based on using bisulfite treatment of DNA and simultaneous PCR of multiple DNA repetitive elements, such as Alu elements and long interspersed nucleotide elements (LINE). The PCR product, which represents a pool of approximately 15000 genomic loci, could be used for direct sequencing, selective restriction digestion or pyrosequencing, in order to quantitate DNA methylation. By restriction digestion or pyrosequencing, the assay was reproducible with a standard deviation of only 2% between assays. Using this method we found that almost two-thirds of the CpG methylation sites in Alu elements are mutated, but of the remaining methylation target sites, 87% were methylated. Due to the heavy methylation of repetitive elements, this assay was especially useful in detecting decreases in DNA methylation, and this assay was validated by examining cell lines treated with the methylation inhibitor 5-aza-2'deoxycytidine (DAC), where we found a 1-16% decrease in Alu element and 18-60% LINE methylation within 3 days of treatment. This method can be used as a surrogate marker of genome-wide methylation changes. In addition, it is less labor intensive and requires less DNA than previous methods of assessing global DNA methylation.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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We report results of a study of the B-s(0) oscillation frequency using a large sample of B-s(0) semileptonic decays corresponding to approximately 1 fb(-1) of integrated luminosity collected by the D0 experiment at the Fermilab Tevatron Collider in 2002-2006. The amplitude method gives a lower limit on the B-s(0) oscillation frequency at 14.8 ps(-1) at the 95% C.L. At Delta m(s)=19 ps(-1), the amplitude deviates from the hypothesis A=0 (1) by 2.5 (1.6) standard deviations, corresponding to a two-sided C.L. of 1% (10%). A likelihood scan over the oscillation frequency, Delta m(s), gives a most probable value of 19 ps(-1) and a range of 17
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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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)
Influence of particle size on the properties of Pt-Ru/C catalysts prepared by a microemulsion method
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Pt-Ru/C nanocatalysts were prepared by a microemulsion method using different values of water/surfactant molar ratio in order to get different particle sizes. Crystallite sizes and structural properties were determined by X-ray diffraction. Particle size and distribution were characterized by transmission electron microscopy and average composition was determined by energy-dispersive X-ray analysis. Thermogravimetric analysis was used to estimate the amount of supported metals. Differential scanning calorimetry measurements indicated the presence of hydrous ruthenium oxides in the as-prepared catalysts. Results for the oxidation of adsorbed CO as well as for methanol oxidation revealed significant differences in the behavior of the prepared catalysts. All together, the results demonstrate that the variation of particle size produces changes in other properties of the Pt-Ru/C catalysts and that to establish direct correlations between electrocatalytic activity and particle size is not possible because the effects of the different parameters cannot be separated. (c) 2007 the Electrochemical Society.
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Lanthanum-modified bismuth titanate, Bi4-xLaxTi3O12 (BLT), with x ranging from 0 to 0.75 was grown on Pt/Ti/SiO2/Si substrates using a polymeric precursor solution and spin-coating method. The dielectric constant of highly doped bismuth titanate was equal to 148 while dielectric losses remained low (tan delta = 0.0018), and the films showed well-saturated polarization-electric field curves (2P(r) = 40.6 muC/cm(2) and V-c = 0.99 V). The leakage current densities improve for the lanthanum-doped system. For five-layered BLT films with x = 0.75, a charge storage density of 35 fC/mum(2) and a thickness of 320 nm were found. (C) 2004 Elsevier B.V. All rights reserved.