137 resultados para Electron spin resonance measurements


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This study present a novel NO sensor made of a spin trap (iron(II)-diethyldithiocarbamate complex, FeDETC) incorporated in a latex rubber matrix and works as a trap for NO, which is detectable by Electron Paramagnetic Resonance (EPR). We explored the optimization of our sensors changing systematically two fabrication parameters: the latex rubber matrix temperature of polymerization and FeDETC concentration inside the matrix. The sensor was prepared in four different temperatures: 4, 10, 20 and 40°C. The FeDETC concentration was also varied from 0.975 to 14.8 mM. We observed a variation of the EPR signals from the sensors prepared at different conditions. We found a high stability of the EPR response from our sensor, 40 days at RT. The best sensor was made with a latex rubber matrix polymerized at 10°C and with a FeDETC concentration of 14.8 mM. In vivo tests show good biocompatibility of our sensor. © 2007 Asian Network for Scientific Information.

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

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This study evaluated the spin concentration and the crystallinity in different classifications of dental composites as a function of the material condition (new, aged and expired). Specimens were obtained according to the factors: composites: Filtek P60, Filtek Z250, Filtek Z350XT, and Filtek Silorane; and material conditions: new, aged, and expired. The syringe composites underwent an accelerated aging protocol (Arrhenius model). The magnetic properties of the composites were characterized using Electron Paramagnetic Resonance (EPR) and the concentration of spins (number of spins/mass) was calculated. The crystallinity of the composites tested was characterized with X-ray diffraction (XRD). Filtek P60 and Filtek Z250 presented similarities in terms of spin concentration and crystallinity, irrespective of the material condition. The aging protocol influenced the composite Filmic Z350XT that exhibited a significant increase in the spin concentration. Besides, lower intensity peaks of the organic matrix and amorphous silica were also observed for both aged and expired Filtek Z350XT. Although a significant lower spin concentration was observed for the silorane composite in comparison to that of the methacrylates, a decrease in the relative intensity of peaks of the amorphous region related to the organic components in the diffractograms was observed. The material conditions tested influence the crystallinity and the magnetic properties of the composites evaluated. (C) 2014 Elsevier Ltd. All rights reserved.

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Oxidation states of transition metal cations in spinels-type oxides are sometimes extremely difficult to determine by conventional spectroscopic methods. One of the most complex cases occurs when there are different cations, each one with several possible oxidation states, as in the case of the magnetoresistant Mn(2-x)V(1+x)O4 (x=0, 1/3 and 1) spinel-type family. In this contribution we describe the determination of the oxidation state of manganese and vanadium in Mn(2-x)V(1+x)O4 (x=0, 1/3,1) spinel-type compounds by analyzing XANES and high-resolution K beta X-ray fluorescence spectra. The ionic models found are Mn22+V4+O4, Mn5/32+V4/33.5+O4 and Mn2+V23+O4. Combination of the present results with previous data provided a reliable cation distribution model. For these spinels, single magnetic electron paramagnetic resonance (EPR) lines are observed at 480 K showing the interaction among the different magnetic ions. The analysis of the EPR parameters show that g-values and relative intensities are highly influenced by the concentration and the high-spin state of Mn2+. EPR broadening linewidth is explained in terms of the bottleneck effect, which is due to the presence of the fast relaxing V3+ ion instead of the weak Mn2+ (S state) coupled to the lattice. The EPR results, at high temperature, are well explained assuming the oxidation states of the magnetic ions obtained by the other spectroscopic techniques. (c) 2013 Elsevier Inc. All rights reserved.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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The effect of phloretin in the structure and hydration of dimiristoyl phosphatidylcholine vesicles (DMPC) was investigated by electron paramagnetic resonance technique (EPR) at the bilayer core of membrane, using 14-PCSL spin label derivative of phosphatidylcoline. The spectra obtained by pure DMPC vesicles and with addition of phloretin were simulated using the Nonlinear Least-Square program, at the tempearature between 15 oC to 50 oC. Through these simulations it was possible to analyse the membrane hydration and bilayer order, to understand the interaction between DMPC aggregates and phloretin. The results show that the phloretin decreases the membrane hydration in both gel and fluid phases. This reduction of water molecules is accompanied by increasing of the bilayer order at this micro-region

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In the work presented here, Ce0.97Cu0.03O2 nanoparticles were synthesized by a microwave-assisted hydrothermal method under different synthesis temperatures. The obtained nanoparticles were tested as catalysts in preferential oxidation of CO to obtain CO-free H2 (PROX reaction). The samples were characterized by X-ray diffraction, transmission electron microscopy (TEM), electron paramagnetic resonance spectroscopy (EPR) and temperature-programmed reduction (TPR). X-ray diffraction measurements detected the presence of pure cubic CeO2 for all synthesized samples. TEM images of the Ce0.97Cu0.03O2 nanoparticles revealed that samples synthesized at 80°C are composed mainly of nanospheres with an average size of 20 nm. The formation of some nanorods with an average diameter of 8 nm and 40 nm in length, and the size reduction of the nanoparticles from 20 to approximately 15 nm is observed with increasing synthesis temperature. EPR spectra indicated that copper is found well dispersed in sample synthesized at 160°C, located predominant in surface sites of ceria. For samples synthesized at 80 and 120°C, the species are less dispersed than in the other one, resulting in the formation of Cu2+−Cu2+ dimmers at the surface of ceria. TPR profiles presented two reduction peaks, one below 400°C attributed to the reduction of different copper species and a second peak around 800°C attributed to the reduction of Ce4+→ Ce3+ species located in the volume of the nanoparticles. The peak related to the reduction of copper species shifts to lower temperatures with increasing synthesis temperature, i.e., the sample synthesized at 160°C is more easily reduced than the ones synthesized at 120 and 80°C. The nanoparticles showed active as catalysts for the CO-PROX reaction. The microwave-assisted method revealed efficient for the synthesis of Ce0.97Cu0.03O2 nanoparticles with copper species selective for the CO-PROX reaction, which reaches CO conversions up to 92% for the sample synthesized at 160°C.

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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)

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ESR measurements In pressed pellets of doped Poly(3-Methylthiophene)(P3MT) were performed at 10 K and 50 K after cooling the system slowly from room temperature to 110 K, quenching to 77 K and then to 10 K. ESR line asymmetry (A/B) as a function of microwave power was observed and 9.4 GHz conductivity was obtained from Dyson's theory. The data is discussed in terms of Charge-Density Wave (CDW) depinning. At 50 K the threshold electric field is estimated to be less than 1 V/cm. At 10 K a subtle pinning of the CDW was observed around 15 mW.

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In this work it is reported the magnetic behavior of submicron and mesoscopic-size superconducting YBCO powders, prepared by a modified polymeric precursors method. The grain size and microstructure were analyzed using scanning electron microscopy ( SEM). Measurements of magnetization and AC-susceptibility as a function of temperature were performed with a quantum design SQUID magnetometer. Our results indicated significant differences on the magnetic propreties, in connection with the calcination temperature and the pressure used to pelletize the samples. This contribution is part of an effort to study vortex dynamics and magnetic properties of submicron and mesoscopic-size superconducting samples. (C) 2008 Elsevier B. V. All rights reserved.

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We report an experimental and theoretical study of magnetic properties of synthetic eumelanin. The magnetization curves are determined by using both a vibrating sample magnetometer and a superconducting quantum interferometer device in an extended range of magnetic fields ranging from -10 kOe to 10 kOe at different temperatures. We find that the eumelanin magnetization can be qualitatively explained in terms of a simple model of dipolar spheres with an intrinsic magnetic moment. The latter one is experimentally measured by using X-band electron paramagnetic resonance. Our findings indicate that synthetic melanins are superparamagnetic.

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Very intense visible green photoluminescence (PL) was observed at room temperature in structurally ordered-disordered BaZrO3 powders. Ab initio calculations, ultraviolet-visible absorption spectroscopy, electron paramagnetic resonance, and PL were performed. Theoretical and experimental results showed that local defects in the cubic structure caused by [ZrO5 center dot V-O(z)] complex clusters, where V-O(z) = V-O(x), V-O(center dot), and V-O(center dot center dot), play an important role in the formation of hole-electron pairs, giving rise to a charge gradient in the structure which is responsible for PL emission. (c) 2008 American Institute of Physics.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)