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Summary Polymers have a great interest for the study and design of new materials. Among these materials are epoxy resins, that have good properties, such as low shrinkage during cure, good adhesion, high water and chemical resistance, etc. They have also fast and easy cure in a broad range of temperatures. TTT diagrams are very helpful to design new epoxy materials as they allow the search for very important final properties, such as thermal stability, conversion or glass transition temperature of a material cured through a selected curing cycle. In this work the dependence of the thermal stability on the selected curing cycle for a DGEBA/1,2 DCH system was studied.

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Journal of Thermal Analysis and Calorimetry
Authors: Lisardo Núñez, L. Fraga, M. Núñez, M. Villanueva, and B. Rial
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Abstract  

The thermal degradation of the epoxy systems diglycidyl ether of bisphenol A (BADGE n=0)/1, 2 diamine cyclohexane (DCH) and diglycidyl ether of bisphenol A (BADGE n=0)/1, 2 diaminecyclohexane (DCH) containing calcium carbonate filler immersed and not immersed in hydrochloric acid have been studied by thermogravimetric analysis in order to compare their decomposition processes and to determine the reaction mechanism of the degradation processes. The value of the activation energies, necessary for this study, were calculated using various integral and differential methods. Analysis of the results suggests that hydrochloric acid does not affect the decomposition of the epoxy network and that the reaction mechanisms produce sigmoidal-type curves for the systems not immersed in HCl and deceleration curves for the same systems immersed.

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Journal of Thermal Analysis and Calorimetry
Authors: Lisardo Núñez Regueira, M. Núñez, M. Villanueva, and B. Rial

Abstract  

The influence of agents originated in a municipal landfill on the thermal degradation of a polymeric system composed of a diglycidyl ether of bisphenol A (n=0) and 1,2-diaminecyclohexane was studied by thermogravimetric analysis (TG) in order to obtain the lifetime of this material before and after being attacked. The different data obtained were analyzed to check the resistance of these materials to chemical attack and the possibility of their use as coating materials in plants where those reagents were present. At the optimum temperature of service for this material, 373.16 K, the lifetimes obtained from the experimental results were 2633 years and 2135 years, respectively.

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Journal of Thermal Analysis and Calorimetry
Authors: L. Núñez-Regueira, M. Villanueva, and I. Fraga-Rivas

Abstract  

The study of the degradation of a polymer is important because it can determine the upper temperature limit, the mechanism of a solid-state process, and the life-time for this system. Since the behavior of thermosets is affected by the selection of the curing cycle, it is important to investigate the changes which take place during the thermal degradation of these materials when a change on the sequence of time and temperature is introduced during the curing reaction. In this work, the thermal degradation of two epoxy systems diglycidyl ether of bisphenol A (BADGE n=0)/1, 2 diamine cyclohexane (DCH) cured through different sequences of time and temperature was studied by thermogravimetric analysis in order to determine the reaction mechanism of the degradation processes, and also to check the influence of the curing cycle on this mechanism. Values obtained using different kinetic methods were compared to the value obtained by Kissinger’s method (differential method which do not require a knowledge of the n-order reaction mechanism), and to that obtained through Flynn–Wall–Ozawa method in a previous work.

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A chitin-lipoprotein complex was detected in the pre-exuvial lobster shell. The aqueous extract of this skeleton contains a lipoprotein in its highest molecular weight fraction where the phospholipids constitute the main component. Changes in the lipoprotein crystalline structure with temperature were detected, but not the formation of typical liquid crystals.

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Abstract  

Differential scanning calorimetry was used to study the influence of an epoxy reactive diluent, vinylcyclohexane dioxide, on the curing reaction of a polymeric system composed of diglycidyl ether of bisphenol A (n=0) and 1,2-diaminecyclohexane (DCH). Heat evolution and glass transition temperature, were measured in terms of the added diluent percentage. Experimental results show that both the curing degree and the glass transition temperature of the polymeric system decrease with an increase in the diluent percentage. Dynamic mechanical analysis of several samples also showed that T g decreases with the increase of diluent percentage, thus corroborating DSC measurements.

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Abstract  

The rheological behaviour of the materials diglycidil ether of bisphenol A (n = 0), 1, 2 diamine-cyclohexane and the epoxy reactive diluent vinylcyclohexane dioxide have been studied both separately and mixed before the beginning of the curing reaction. Different kinds of tests such as: preshear and time sweep, flow curve and stress sweep experiments were carried out. From these experiments, interesting information about: viscosity-shear stress and viscosity-shear rate dependences, storage modulus and the linear viscoelastic region were found out. Relationships between concentration of diluent and the final viscosity of the mixed sample and also between percentage of diluent and storage modulus were studied.

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Journal of Thermal Analysis and Calorimetry
Authors: N. Barros, J. Salgado, M. Villanueva, J. Rodriquez-Añón, J. Proupin, S. Feijóo, and M. Martín-Pastor

Abstract

The environmental concern on soil exploitation, linked to global warming by the Kyoto protocol, is responsible for increasing interest in the understanding of the role of the composition and structure of the soil organic matter (SOM) on soil carbon, C, dynamics. Thermal analysis and nuclear magnetic resonance (NMR) are applied to study the thermal properties, the structure and composition of the SOM of six samples with different C contents in order to improve the interpretation of results given by thermal analysis. Results showed that the direct integral of the combustion peaks obtained by DSC and the percentage of SOM given by TG were both directly related to the quantity of total soil C. Thus, soils with higher C content showed higher energy content too. The combustion temperatures of the curves given by DSC are those reported for labile OM. NMR results indicated the presence of aliphatic C, carbohydrates, and a weak signal in the aromatic C band in all the samples that was not detected in the DSC curves. Only two samples showed carboxyl/carbonyl C which was not detected by DSC also.

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Journal of Thermal Analysis and Calorimetry
Authors: J. Salgado, J. Proupín, M. Villanueva, J. Rodríguez-Añón, and N. Barros

Abstract  

Differential scanning calorimetry was applied to assess on seasonally soil organic matter changes. Soils were collected in two sites located in Viveiro (Galicia, Spain). One of them has been used as arable land and the other one was under pinewood. Soil samples were seasonally collected during a year. The heat of combustion and the ignition temperature of the soil organic matter were calculated by analyzing the thermograms obtained by differential scanning calorimetry. The shape and the maximum and end temperatures of the two exothermic peaks observed in the thermograms, yielded information about the relations between the labile and recalcitrant pools, and hence information about carbon stabilization degree in both soils.

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