354 resultados para Differential Scanning Calorimetry (dsc)
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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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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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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Phase transitions of freeze-dried persimmon in a large range of moisture content were determined by differential scanning calorimetry (DSC). In order to study this transitions at low and intermediate moisture content domains, samples were conditioned by adsorption at various water activities (a(w) = 0.11-0.90) at 25 degreesC. For the high moisture content region, samples were obtained by water addition. At a(w) less than or equal to 0.75 two glass transitions were visible, with T(g) decreasing with increasing water activity due to water plasticizing effect. The first T(g) is due to the matrix formed by sugars and water, the second one, less visible and less plasticized by water, is probably due to macromolecules of the fruit pulp. At a(w) between 0.80 and 0.90 a devitrification peak appeared after T(g) and before T(m). At this moisture content range, the Gordon-Taylor model represented satisfactorily the matrix glass transition curve. At the higher moisture content range (a(w) > 0.90), the more visible phenomenon was the ice melting. T(g) appeared less visible because the enthalpy change involved in glass transition is practically negligible in comparison with the latent heat of melting. In the high moisture content domain T(g) remained practically constant around T(g)' (-56.6 degreesC). (C) 2001 Elsevier B.V. B.V. All rights reserved.
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Glass transition temperature of freeze-dried pineapple conditioned by adsorption at various water activities at 25 degreesC was determined by differential scanning calorimetry (DSC). High moisture content samples corresponding to water activities higher than 0.9, obtained by liquid water addition, were also analysed. The DSC traces showed a well-visible shift in baseline at the glass transition temperature (T(g)). Besides, no ice formation was observed until water activity was equal to 0.75. For water activities lower than 0.88, the glass transition curve showed that T(g) decreased with increasing moisture content and the experimental data could be well-correlated by the Gordon-Taylor equation. For higher water activities, this curve exhibited a discontinuity, with suddenly increasing glass transition temperatures approaching a constant value that corresponds to the T(g) of the maximally freeze-concentrated amorphous matrix. The unfreezable water content was determined through melting enthalpy dependence on the sample moisture content.
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This work describes the preparation and characterization of composite materials obtained by the combination of natural rubber (NR) and carbon black (CB) in different percentages, aiming to improve their mechanical properties, processability, and electrical conductivity, aiming future applications as transducer in pressure sensors. The composites NR/CB were characterized through optical microscopy (OM), DC conductivity, thermal analysis using differential scanning calorimetry (DSC), dynamic mechanical thermal analysis (DMA), thermogravimetry (TGA), and stress-strain test. The electrical conductivity varied between 10(-9) and 10 S m(-1), depending on the percentage of CB in the composite. Furthermore, a linear (and reversible) dependence of the conductivity on the applied pressure between 0 and 1.6 MPa was observed for the sample with containing 80 wt % of NR and 20% of CB. (C) 2007 Wiley Periodicals, Inc.
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The phase transition from the non-polar a-phase to the polar beta-phase of poly(vinylidene fluoride) (PVDF) has been investigated using micro-Raman spectroscopy, which is advantageous because it is a nondestructive technique. Films of alpha-PVDF were subjected to stretching under controlled rates at 80 degrees C, while the transition to P-PVDF was monitored by the decrease in the Raman band at 794 cm(-1) characteristic of the a-phase, along with the concomitant increase in the 839 cm-1 band characteristic of the P-phase. The alpha ->beta transition in our PVDF samples could be achieved even for the sample stretched to twice (2 X -stretched) the initial length and it did not depend on the stretching rate in the range between 2.0 and 7.0 mm/min. These conclusions were corroborated by differential scanning calorimetry (DSC) and X-ray diffraction experiments for PVDF samples processed under the same conditions as in the Raman scattering measurements. Poling with negative corona discharge was found to affect the a-PVDF morphology, improving the Raman bands related to this crystalline phase. This effect is minimized for films stretched to higher ratios. Significantly, corona-induced effects could not be observed with the other experimental techniques, i.e., X-ray diffraction and infrared spectroscopy.
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Glass transition temperatures of freeze-dried tomato conditioned at various water activities at 25 C were determined by differential scanning calorimetry (DSC). Air-dried tomato with and without osmotic pre-treatment in sucrose/NaCl solutions was also analyzed. Thermograms corresponding to the low water activity domain (0.11 less than or equal to a(w) less than or equal to 0.75) revealed the existence of two glass transitions, which were attributed to separated phases formed by sugars and water and other natural macromolecules present in the vegetable. Both transitions were plasticized by water and experimental data could be well correlated by the Gordon-Taylor equation in the low-temperature domain, and by the Kwei model in the high-temperature domain. For higher water activities, the low-temperature glass transition curve exhibited a discontinuity, with suddenly increased glass transition temperatures approaching a constant value that corresponds to the T-g of the maximally freeze-concentrated amorphous matrix. The unfreezable water content was determined through the melting enthalpy dependence on the moisture content. (C) 2002 Elsevier B.V. Ltd. All rights reserved.
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Solid compounds of general formula ML(2) . nH(2)O [where M is Mg, Ca, Sr or Ba; L=4 methoxybenzylidenepyruvate (4-MeO-BP); n = 4, 1 or 0] have been synthetized. Thermogravimetry (TG), derivative thermogravimetry (DTG), differential scanning calorimetry (DSC), x-ray diffraction powder patterns and elemental analysis have been used to characterize the compounds. The thermal stability of these compounds as well as that of the decomposition products were studied using Pt or Al2O3 crucibles in an air or a CO2 atmosphere.
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We have used surface tension measurements, differential scanning calorimetry (DSC), dynamic light scattering (DLS), and cryo-transmission electron microscopy (cryo-TEM) to investigate the dynamic and structural behavior of octadecyltrimethylammonium bromide (C(18)TAB) micelles in water and NaBr solution. The surface tension data for fixed C(18)TAB concentrations of 25 mM and varied NaBr additions (0-50 mM) shows that the critical micelle concentration (cmc) increases after an initial decrease at 0.5 mM NaBr. This unusual effect has been explained using results from DSC and DLS. At low salt concentrations (below ca. 25 mM) the relaxation time distribution is bimodal with a dominant fast mode due to spherical micelles. Above ca. 35 mM NaBr disklike structures are favored and the relaxation time distribution is more closely unimodal. The postulated sphere-to-disk transition is supported by cryo-TEM micrographs. A pronounced increase in the micellar effective hydrodynamic radius (R-H) is observed as the NaBr concentration is increased above about 35 mM; below 35 mM the R-H of the spherical micelles changes Little with ionic strength.
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The influence of additions of 2, 4, 6, 8, 10 and 12 mass% Ag on the thermal behavior of the Cu-8 mass% Al alloy was studied using differential scanning calorimetry (DSC), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffractometry (XRD). The results indicate that the presence of silver introduces new thermal events, due to the formation of a silver-rich phase and, for additions of 10 and 12 mass% Ag, it is possible to verify the formation of the gamma (1) phase (Cu9Al4) and the metastable transitions which are only observed in alloys with a minimum of 9 mass% Al.
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Cellulose-phosphate composite membranes have been prepared from bacterial cellulose membranes ( BC) and sodium polyphosphate solution. The structure and thermal behavior of the new composites were evaluated by X-ray diffraction (XRD), P-31-nuclear magnetic resonance (NMR), scanning electron microscopy (SEM), differential scanning calorimetry (DSC), thermogravimetry (TG) and thermomechanical analysis (TMA). From XRD analyses the I alpha and I beta cellulose crystalline phases were identified together with crystalline sodium phosphate that covers the cellulose microfibrils as revealed by SEM. P-31 NMR spectra show peaks assigned to Q(0) and Q(1) phosphate structures to be compared to the Q(2) units that characterize the precursor polyphosphate. Glass transition temperature, T-g, obtained from TMA curves and thermal stability obtained from TG and DSC measurements, were observed to be dependent on the phosphate content.
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Oxamniquine polymeric prodrug with potential antischistosomal activity was prepared using dextran T-70 as a carrier, which was analysed by (HNMR)-H-1, C-13 NMR and IR spectroscopy. The formation of the oxamniquine salt was confirmed by thermogravimetric analysis (TG) and differential scanning calorimetry (DSC) which showed a different thermal behaviour when compared to the physical mixture.