38 resultados para 2-Epoxy-3-(p-nitrophenoxy) propane

em Biblioteca Digital da Produção Intelectual da Universidade de São Paulo (BDPI/USP)


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Two aspartyl proteases activities were identified and isolated from Trypanosoma cruzi epimastigotes: cruzipsin-I (CZP-I) and cruzipsin-II (CZP-II). One was isolated from a soluble fraction (CZP-II) and the other was solubilized with 3-[(3-cholamidopropyl)-dimethylammonio]-1-propanesulfonate(CZP-I). The molecular mass of both proteases was estimated to be 120 kDa by HPLC gel filtration and the activity of the enzymes was detected in a doublet of bands (56 and 48 kDa) by substrate-sodium dodecyl sulphate-polyacrylamide-gelatin gel electrophoresis. Substrate specificity studies indicated that the enzymes consistently hydrolyze the cathepsin D substrate Phe-Ala-Ala-Phe (4-NO(2))-Phe-Val-Leu-O(4)MP but failed to hydrolyze serine and other protease substrates. Both proteases activities were strongly inhibited by the classic inhibitor pepstatin-A (>= 68%) and the aspartic active site labeling agent, 1,2-epoxy-3-(phenyl-nitrophenoxy) propane (>= 80%). These findings show that both proteases are novel T. cruzi acidic proteases. The physiological function of these enzymes in T. cruzi has under investigation. (c) 2009 Elsevier Inc. All rights reserved.

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The aim of this work was to evaluate the effect of the storage time on the thermal properties of triethylene glycol dimethacrylate/2,2-bis[4-(2-hydroxy-3-methacryloxy-prop-1-oxy)-phenyl]propane bisphenyl-alpha-glycidyl ether dimethacrylate (TB) copolymers used in formulations of dental resins after photopolymerization. The TB copolymers were prepared by photopolymerization with an Ultrablue IS light-emitting diode, stored in the dark for 160 days at 37 degrees C, and characterized with differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and Fourier transform infrared spectroscopy with attenuated total reflection. DSC curves indicated the presence of an exothermic peak, confirming that the reaction was not completed during the photopolymerization process. This exothermic peak became smaller as a function of the storage time and was shifted at higher temperatures. In DMA studies, a plot of the loss tangent versus the temperature initially showed the presence of two well-defined peaks. The presence of both peaks confirmed the presence of residual monomers that were not converted during the photopolymerization process. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 112: 679-684, 2009

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The (2)H(d,p)(3)H and (2)H(d,n)(3)He reactions have been indirectly studied by means of the Trojan Horse Method applied to the quasi-free (2)H((3)He, p(3)H)(1)H (2)H((3)He, n(3)He)(1)H reaction at 18 MeV of beam energy. This is the first experiment where the spectator (here (1)H) has been detected in coincidence with the charged participant, avoiding the limitations of standard neutron detectors. The d - d relative energy has been measured from 1.5 MeV down to 2 keV, at center of mass angles from 40A degrees to 170A degrees. Indirect angular distributions are compared with the direct behaviour in the overlapping regions.

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Synchrotron X-ray powder diffraction was applied to the study of the effect of crystallite size on the crystal structure of ZrO(2)-10 mol% Sc(2)O(3) nanopowders synthesized by a nitrate-lysine gel-combustion route Nanopowders with different average crystallite sizes were obtained by calcination at several temperatures, ranging from 650 to 1200 degrees C The metastable t""-form of the tetragonal phase, exhibiting a cubic unit cell and tetragonal P4(2)/nmc spatial symmetry, was retained at room temperature in fine nanocrystalline powders, completely avoiding the presence of the stable rhombohedral beta phase. Differently, this phase was identified in samples calcined at high temperatures and its content increased with increasing crystallite size The critical maximum crystallite size for the retention of the mestastable t""-form resulted of about 35 nm (C) 2009 Elsevier B.V All rights reserved

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We have investigated the crystal structures and phase transitions of nanocrystalline ZrO(2)-1 to -13 mol % Sc(2)O(3) by synchrotron X-ray powder diffraction and Raman spectroscopy. ZrO(2)-Sc(2)O(3) nanopowders were synthesized by using a stoichiometric nitrate-lysine get-combustion route. Calcination processes at 650 and at 850 degrees C yielded nanocrystalline materials with average crystallite sizes of (10 +/- 1) and (25 +/- 2) nm, respectively. Only metastable tetragonal forms and the cubic phase were identified, whereas the stable monoclinic and rhombohedral phases were not detected in the compositional range analyzed in this work. Differently from the results of investigations reported in the literature for ZrO(2)-Sc(2)O(3) materials with large crystallite sizes, this study demonstrates that, if the crystallite sizes are small enough (in the nanometric range), the metastable t ``-form of the tetragonal phase is retained. We have also determined the t`-t `` and t ``-cubic compositional boundaries at room temperature and analyzed these transitions at high temperature. Finally, using these results, we built up a metastable phase diagram for nanocrystalline compositionally homogeneous ZrO(2)-Sc(2)O(3) solid solutions that strongly differs from that previously determined from compositionally homogeneous ZrO(2)-Sc(2)O(3), Solid solutions with much larger crystallite sizes.

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By means of synchrotron X-ray powder diffraction (SXPD) and Raman spectroscopy, we have detected, in a series of nanocrystalline and compositionally homogeneous ZrO(2)-Y(2)O(3) solid solutions, the presence at room temperature of three different phases depending on Y(2)O(3) content, namely two tetragonal forms and the cubic phase. The studied materials, with average crystallite sizes within the range 7-10 nm, were synthesized by a nitrate-citrate gel-combustion process. The crystal structure of these phases was also investigated by SXPD. The results presented here indicate that the studied nanocrystalline ZrO(2)-Y(2)O(3) solid solutions exhibit the same phases reported in the literature for compositionally homogeneous materials containing larger (micro)crystals. The compositional boundaries between both tetragonal forms and between tetragonal and cubic phases were also determined. (C) 2011 Elsevier B.V. All rights reserved.

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We have studied the normal and superconducting transport properties of Bi(1.65)Pb(0.35)Sr(2)Ca(2)Cu(3)O(10+delta) (Bi-2223) ceramic samples. Four samples, from the same batch, were prepared by the solid-state reaction method and pressed uniaxially at different compacting pressures, ranging from 90 to 250 MPa before the last heat treatment. From the temperature dependence of the electrical resistivity, combined with current conduction models for cuprates, we were able to separate contributions arising from both the grain misalignment and microstructural defects. The behavior of the critical current density as a function of temperature at zero applied magnetic field, J (c) (T), was fitted to the relationship J (c) (T)ae(1-T/T (c) ) (n) , with na parts per thousand 2 in all samples. We have also investigated the behavior of the product J (c) rho (sr) , where rho (sr) is the specific resistance of the grain-boundary. The results were interpreted by considering the relation between these parameters and the grain-boundary angle, theta, with increasing the uniaxial compacting pressure. We have found that the above type of mechanical deformation improves the alignment of the grains. Consequently the samples exhibit an enhance in the intergranular properties, resulting in a decrease of the specific resistance of the grain-boundary and an increase in the critical current density.

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We performed measurements of electrical resistivity as a function of temperature, rho(T), in polycrystalline samples of YBa(2)Cu(3)O(7-delta) (Y-123) subjected to different uniaxial compacting pressures. We observed by using X-ray diffractometry that samples have a very similar composition. Most of the identified peaks are related to the superconducting Y-123 phase. Also, from the X-ray diffraction patterns performed, in powder and pellet samples, we estimated the Lotgering factor along the (00l) direction, F((00l)). The results indicate that F((00l)) increases from 0.13 to 0.16. From electrical resistivity measurements as a function of temperature, we were able to separate contributions arising from both the grain misalignment and microstructural defects. We found appreciable degradation in the normal-state transport properties of samples with an increase in uniaxial compacting pressure. It seems that this type of behavior is associated with an increase in the influence of microstructural defects at the intergranular level. The experimental results are analyzed in the framework of a current conduction model of granular samples.

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The disclosure of magnetic ionic liquids (MILs) as stable dispersions of surface modified gamma-Fe(2)O(3) or CoFe(2)O(4) nanoparticles (NPs) in the 1-n-butyl-3-methylimidazolium tetrafluoroborate (BMIBF(4)) ionic liquid is reported. The magnetic NPs were characterized by X-ray powder diffraction, transmission electron microscopy, and Raman spectroscopy. The surface modified NPs have proved to form stable dispersions in BMIBF(4) in the absence of water and behave like a magnetic ionic liquid. The MILs have been characterized by Raman spectroscopy, magnetic measurements, and DSC. The stability of the magnetic NPs in BMIBF(4) is consistently explained by assuming the formation of a semiorganized protective layer composed of supramolecular aggregates in the form of [(BMI)(2)(BF(4))(3)](-). A superparamagnetic behavior and saturation magnetization of ca. 18 emu/g for a sample containing 30% w/w maghemite NPs/BMIBF(4) have been inferred from static and dynamic magnetic measurements. DSC results have shown that the MIL composed of 30% w/w CoFe(2)O(4) NPs/BMIBF(4) remains a liquid phase down to -84 degrees C.

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This paper presents a systematic comparison of OSL signals from Al(2)O(3):C when stimulated with blue and green light. Al(2)O(3):C detectors were irradiated with various doses and submitted to various bleaching regimes using yellow, green and blue light. Most of the investigations were carried out using Luxel (TM)-type detectors used in the commercial Luxet (TM) and InLight (TM) dosimetry systems (Landauer Inc.). Al(2)O(3):C single crystals and Al(2)O(3):C powder were also used to complement the investigations. The results show that, although blue stimulation provides faster readout times (OSL curves that decayed faster) and higher initial OSL intensity than green stimulation, blue stimulation introduced complicating factors. These include incomplete bleaching of the dosimetric trap when the Al(2)O(3):C detectors are bleached with yellow or green light and the OSL is recorded with blue light stimulation, and an increased residual level due to stimulation of charge carriers from deep traps. The results warrant caution when using blue stimulation to measure the OSL signal from Al(2)O(3):C detectors, particularly if the doses involved are low and the detectors have been previously exposed to high doses. (C) 2010 Elsevier Ltd. All rights reserved.

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The electronic and optical properties of grossular garnet are investigated using density functional theory (DFT) within generalized gradient approximation (GGA). The calculated lattice parameters are in good agreement with the experiment data. The electronic structure shows that grossular has a direct band gap of 5.22 eV. The dielectric functions, reflective index, extinction coefficient, reflectivity and energy-loss spectrum are calculated. The optical properties of grossular are discussed based on the band structure calculations. The O 2p states and Si 3s play a major role in these optical transitions as initial and final states, respectively. The absorption spectrum is localized in the ultraviolet range between 30 and 250 nm. Finally, we concluded that pure grossular crystal does not absorb radiation in the visible range. (c) 2009 Elsevier B.V. All rights reserved.

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A Li(2)O-B(2)O(3)-Al(2)O(3) glass system, un-doped and doped with LiF, and/or TiO(2) was synthesized by the fusion method and its physical properties were investigated by thermoluminescence (TL), X-ray diffraction (XRD), electron paramagnetic resonance (EPR), atomic force microscopy (AFM) and differential thermal analysis (DTA). The samples were subjected to gamma-rays from a colbalt-60 ((60)Co) source. These techniques provided evidence of LiF and LiF doped with Ti crystal formation in the glass system. A TL glow peak at about 433 K was sensitive to (60)Co gamma-rays and showed good linearity with doses and consequently could be used to quantify radiation doses. Crown Copyright (C) 2011 Published by Elsevier B.V. All rights reserved.

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High energy band gap hosts doped with lanthanide ions are suitable for optical devices applications To study the potential of Ta(2)O(5) as a host compound pure and Eu(2)O(3)-doped Ta(2)O(5) crystal fibers were grown by the laser-heated pedestal growth technique in diameters ranging from 250 to 2600 pm and in lengths of up to 50 mm The axial temperature gradient at the solid/liquid interface of pure Ta(2)O(5) fibers revealed a critical diameter of 2200 gm above which the fiber cracks X-ray diffraction measurements of the pure Ta(2)O(5) single crystals showed a monoclinic symmetry and a growth direction of [1 (1) over bar 0] An analysis of the pulling rate as a function of the fiber diameter for Eu(2)O(3)-doped Ta(2)O(5) fibers indicated a well defined region in which constitutional supercooling is absent Photoluminescence measurements of pure Ta(2)O(5) crystals using excitation above the band gap (3 8 eV) were dominated by a broad unstructured green band that peaked at 500 nm Three Eu(3+)-related optical centers were identified in the doped samples with nominal concentrations exceeding 1 mol% Two of these centers were consistent with the ion in the monoclinic phase with different oxygen coordinations The third one was visible in the presence of the triclinic phase (C) 2010 Elsevier B V All rights reserved

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Photoexpansion and photobleaching effects have been observed in amorphous GeS(2) + Ga(2)O(3) (GGSO) thin films, when their surfaces were exposed to UV light. The photoinduced changes on the surface of the samples are indications that the structure has been changed as a result of photoexcitation. In this paper, micro-Raman, energy dispersive X-ray analysis (EDX) and backscattering electrons (BSE) microscopy were the techniques used to identify the origin of these effects. Raman spectra revealed that these phenomena are a consequence of the Ge-S bonds` breakdown and the formation of new Ge-O bonds, with an increase of the modes associated with Ge-O-Ge bonds and mixed oxysulphide tetrahedral units (S-Ge-O). The chemical composition measured by EDX and BSE microscopy images indicated that the irradiated area is oxygen rich. So, the present paper provides fundamental insights into the influence of the oxygen within the glass matrix on the considered photoinduced effects. (C) 2010 Elsevier B.V. All rights reserved.

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A dinuclear ruthenium(II) complex double-bridged by an N-aromatic ligand 2-mercaptopyridine (2-pyridinethiol or 2-pyridyl mercaptan) and a methyl sulfoxide (dmso) have been characterized by X-ray crystallography. The reported compound with formula [Ru(2)Cl(3) (mu-pyS)(mu-dmso)(dmso)(4)] center dot 2H(2)O, [C(15)H(36)Cl(3)NO(7)S(6)Ru(2)] (P2/c, a = 13.8175(2) angstrom, b = 10.5608(2) angstrom, c = 21.3544 (3) angstrom, beta = 106.090(1)degrees, V = 2,994.05(8) angstrom(3), Z = 4) represents a seven-membered ring system with both rutheniums in an octahedral geometry. All the hydrogen bonds (C-H-Cl) and the van der Waals contacts give rise to three-dimensional network in the structure and add stability to the dinuclear compound. To our knowledge, this is the first time that the formation of a dinuclear ruthenium(II) complex double-bridged by an N-aromatic ligand 2-mercaptopyridine and dmso have been reported. The study also provided valuable insight into bioinorganic chemistry as continuing efforts are being made to develop metal-based cancer chemotherapeutics. A major feature of this paper is the resolution of a double bridged ruthenium structure which contributes to a better understanding of ruthenium reactivity.