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.
The complex [Pd(2-Phpy)(-Cl)]2 reacts with pyridines (L=pyridine, α-picoline and γ-picoline), amines (L=isopropylamine, tert-butylamine) and ammonia to form the corresponding ortho-palladatedderivatives [Pd(2-Phpy)ClL]. The compounds have been characterized by C, H and Nanalyses and spectroscopic methods
(IR and 1H and 13C NMR).TG, DTG and DSC studies of the complexes were carried out in dynamic nitrogen atmosphere. From DSC analyses the heats
of decomposition were calculated. The kinetics ofthe first step of thermal decomposition were evaluated from TG data by isothermal
methods for L=pyridine and isopropylamine. The activation energies obtained are in the range 90–100 kJ mol-1. The best
fitting for data was observed for R2 and A1.5 kinetic models.
Heat capacity measurements between 293 K and 363 K have been carried out in order to elucidate the different states appearing
in 2-amino-2-methyl-1,3 propanediol (AMP) plastic crystal. The results allowed one of them to be identified as a glassy crystal.
The changes of enthalpy, entropy and Gibbs free energy thermodynamic functions with temperature have been calculated from
the experimental heat capacity values.
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.
Using dynamic mechanical analysis (DMA) we have studied thermal degradation for a system containing a diglycidyl ether of
bisphenol A (DGEBA) and 1,3-bisaminomethylcylohexane (1,3-BAC). The changes of dynamic mechanical properties during thermal
degradation indicated a shift of the glass transition temperature (Tg) to higher temperatures and a decrease in the peak value of the dynamic loss factor (tan δ) with an increasing of aging time.
The value of dynamic storage modulus (E′) at the rubbery state showed an increase with aging time, whiteE′ at the glassy state only underwent a moderate change with increased thermal degradation. From these results it can be argued
that thermal degradation during the stage prior to the onset of the severe degradation involves structural changes in the
epoxy system, as further crosslinking and loss of dangling chains in the crosslinked network.
Collection of uranium by salicyliden and glutariliden chitosans /Schiff's Bases/ was investigated to obtain information on uranium recovery from ores, especially carnotites. The collection of uranium by salicyliden /SDQ/ and glutariliden /GDQ/ chitosans was very rapid during the first 20 min and was affected by the pH of the solution, contact time and temperature. Uranium collected on SDQ and GDQ was easily eluted with diluted sodium bicarbonate solution. Also uranyl and vanadyl ions were separated from each other by using these biopolymers.
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.
The 1 ∶ 4 complexes of cobalt (II) and manganese (II) thiocyanates with morpholine (Morph), [M(NCS)2(Morph)4] (M=Co, Mn), were prepared and studied by means of thermogravimetry, derivative thermogravimetry and differential scanning calorimetry. By thermal treatment of the above compounds, the 1∶2 and 1∶1 complexes, [M(NCS)2(Morph)2] (M=Co, Mn; n=1, 2), were formed. Magnetic data, infrared and electronic spectra and molar conductance values for the compounds are reported. All the complexes contain N-bonded morpholine and the 1∶4 complexes are suggested to have a monomericcis pseudooctahedral structure with N-bonded thiocyanate, whereas the 1∶2 and 1∶1 complexes are considered to have a six-coordinated polymeric configuration involving bridging NCS groups.