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  • Author or Editor: J. Cano x
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Abstract  

“Cut-off” reflectors, which allow obtaining a reflected beam with almost no high energy radiation, as well as different monochromator devices that reflect a beam of monoenergetic and polarized radiation are the most widely employed artifacts to perform the excitation radiation improvement in analytical “non-expensive” TR spectrometers. The aim of this work consisted in testing several monochromator devices: a multilayer structured mirror for soft X-rays (0.7–12.5 nm), as well as different bent and flat crystals of wavelength dispersive spectrometers. The achieved instrumental detection limits for the selected monochromator device are compared with the values obtained using a Suprasil Cut-off reflector and a C-W multilayer (d∼5 nm). Several human corporal fluid samples were analyzed to compare the spectral characteristics when using the Cut-Off Reflector and the RAP flat crystal, respectively.

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Abstract  

Using dynamic mechanical analysis (DMA) we have studied the variation with the frequency of the dynamic mechanical properties (storages modulus,E'; loss modulus,E'' and loss tangent or tan σ) for a system containg a diglycidyl ether of bisphenol A (DGEBA) and 1,3-bisaminomethylcyclohexane (1,3-BAC). These properties were measured both in the glass transition and β transition regions. An increase in frequency caused a shift of tan σ peak positions in both regions toward higher temperature. Finally, we report the activation energies of a DGEBA/1,3-BAC expoxy system for α and β transitions.

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The diffusive and dynamic mechanical behavior of the DGEBA/1,3-BAC epoxy resin system was studied during water absorption. The diffusion of water was investigated at 100% relative humidity, by immersion of specimens in water at 60, 80 and 100°C. In all absorption experiments, water diffusion followed Fick's law. Diffusion coefficients and saturated water concentrations are given for these temperatures. The activation energy for diffusion was determined from the relationship between the diffusion coefficient and the reciprocal of the absolute temperature. The value obtained was 31.2 kJ mol−1. Dynamic mechanical analysis of samples immersed in 100°C water and with various water contents showed both a shift of Tg, defined by thetanδ peak, to lower temperatures and a slight decrease in the dynamic modulus in the presence of water. These effects are probably a result of plasticization.

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Abstract  

The physical aging of a system containing tetraglycidyl-4-4′-diaminodiphenylmethane (TGDDM), with a multifunctional novolac glycidyl ether resin hardened by 4,4′-diaminodiphenylsulphone (DDS) has been investigated by differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA). Samples fully cured were aged at temperatures between 200 and 250C, during periods of time from 1 to a maximum of 336 h. Furthermore, the dynamic mechanical relaxation behaviour annealed at temperature of 220C, was studied, aging during 24 and 168 h. The effect of the enthalpy relaxation during DSC heating scan is shown by the presence of an endothermic peak whose position and intensity depends on the aging conditions, both temperature and time. DSC studies suggest that enthalpy relaxation increases gradually with aging time to a limiting value for each temperature where structural equilibrium is reached. DMA results show that the effect of aging is to cause chain stiffening and a decrease in the height of the peak value of the loss factor.

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Abstract  

Differential scanning calorimetry (DSC) was applied to study the cure kinetics of an epoxy system containing both tetraglycidyl 4,4′-diaminodiphenylmethane (TGDDM) and a multifunctional Novolac glycidyl ether resin, cured with 4,4′-diaminodiphenylsulfone (DDS). The experimental data were analyzed in terms of a mechanistic model proposed by Cole, which includes the etherification reaction. The kinetics can be completely described in terms of three rate constants, which obey the Arrhenius relationship. This model gives a good description of the cure kinetics up to the onset of vitrification. The effect of diffusion control was incorporated to describe the cure in the later stages. By combining the model and a diffusion factor, it was possible to predict the cure kinetics over the whole range of conversion, including an analysis of the evolution of different chemical species during the curing process. Good agreement with the experimental DSC data was achieved with this mechanistic model over the whole range of cure when the etherification reaction was assumed to be of first order with respect to the concentrations of epoxide groups, hydroxy groups, and the tertiary amine groups formed in the epoxide amine reaction.

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Abstract  

A study of an epoxy-cycloaliphatic amine system has been realized using a thermogravimetric technique (TG). Isothermal and non-isothermal (dynamic) methods were employed to determine the kinetic data of this system. Five methods were used for determining the activation energies of this system in the dynamic heating experiments. In two of them (Flynn-Wall-Ozawa, and Kissinger) it is not necessary to have a prior knowledge of the reaction mechanism of the degradation behaviour for this system. In the other ones (Coats and Redfern, Horowitz and Metzger, and Van Krevelen et al.) it is necessary to know this reaction mechanism, besides Criado et al. method was used for determining it. The results have shown that good agreement between the activation energies obtained from all methods can be achieved if it is assumed that the degradation behaviour of this system is of sigmoidal-rate type.

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Abstract  

Using differential scanning calorimetry (DSC) we have studied the physical aging of an epoxy resin based on the diglycidyl ether of bisphenol A (DGEBA) modified by two different contents of an acrylonitrile-butadiene-styrene (ABS) and cured with 1,3-bisaminomethylcyclohexane (1,3-BAC). Samples fully cured were annealed at temperature of 125C for periods of time of 72 and 120 h, to determine the process of physical aging. The apparent activation energy for the enthalpy relaxation, Dh*, is determined as the sample is heated at 10C min-1 following cooling at various rates through the glass transition region. DSC studies suggested that the presence of thermoplastic inhibits the process of relaxation.

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