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  • Author or Editor: J. A. García x
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Abstract  

Sodium titanium germanate with a semicrystalline framework (STG) of the formula Na3H(TiO)3(GeO)(GeO4)3·7H2O was synthesized under mild hydrothermal conditions and its proton form, H4(TiO)3(GeO)(GeO4)3·8H2O (STG-H), was prepared by acid treatment of the sodium compound. The STG was characterized by elemental analysis, TGA, FT-IR, and X-ray powder diffraction. A comparative ion exchange examination of the STG-H towards alkali and alkaline earth metals in a broad pH and concentration range was carried out. It was found that the STG is a moderately weak cation exchanger, possessing high ion exchange capacity (up to 4.0 meq/g) and showing preference for heavy alkali and alkaline earth metals. The STG selectivity towards Cs+ and Sr2+ ions in the presence of competitive metal ions and certain organic compounds was also studied. The data obtained suggest that the sodium titanium germanate is a more selective exchanger for Sr2+ ion than its titanium silicate analogue, K3H(TiO)4(SiO4)3·4H2O.

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The thermal decompositions of divalent cobalt, cadmium, nickel and copper salicylates and intermediates formed during the decomposition processes were investigated by means of thermogravimetry. Two intermediates were identified in each case, except for copper(II) salicylate.

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Abstract  

Solid bisphenol-A epoxy resin of medium molecular mass was cured using a Lewis acid initiator (ytterbium(III) trifluoromethanesulfonate) in three different proportions (0.5, 1 and 2 phr). A kinetic study was performed in a differential scanning calorimeter. The complete kinetic triplet was determined (activation energy, pre-exponential factor, and integral function of the degree of conversion) for each system. A kinetic analysis was performed with an integral isoconversional procedure (free model), and the kinetic model was determined both with the Coats-Redfern method (the obtained isoconversional value being accepted as the effective activation energy) and through the compensation effect. All the systems followed the same isothermal curing model simulated from non-isothermal ones. The growth-of-nuclei Avrami kinetic model A3/2 has been proposed as the polymerization kinetic model. The addition of initiator accelerated the reaction especially when 2 phr was added. 0.5 and 1 phr showed very few kinetic differences between them.

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Abstract  

Solid bisphenol-A epoxy resin (DGEBA) of medium molecular mass was cured using o-tolylbiguanide (TBG) as cross-linking agent. In order to improve the kinetics of the reactive system, two Lewis acid catalysts (erbium(III) and ytterbium(III) trifluoromethanesulfonates) were added in proportions of 1 phr. The kinetic study was performed by dynamic scanning calorimetry (DSC) and the complete kinetic triplet (E, A and g(α)) determined. The kinetic analysis was performed with an integral isoconversional procedure (model-free), and the kinetic model was determined by the Coats-Redfern method and through the compensation effect (IKR). All the systems followed the m=1.5/n=0.5 isothermal curing model simulated from non-isothermal experiments. The addition of a little proportion of ytterbium or erbium triflates accelerated the curing process. In order to extract further information about the role of the lanthanide triflates added to epoxy/TBG systems, the kinetic results were compared with our previous kinetic studies made on DGEBA/lanthanide triflates initiated systems.

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Journal of Thermal Analysis and Calorimetry
Authors:
L. Núñez-Regueira
,
J. Rodríguez-Añón
,
J. Proupín-Castiñeiras
, and
A. Romero-García

Abstract  

Calorific values and flammability changes during a year for forest waste originating from silviculture task in Galicia (NW Spain) are reported. These waste materials are becoming to be used as alternative fuels. The present study was made on several hardwood forest species. These forest species occupy nowadays approximately 30% of the total forest surface of Galicia. Calorific values were measured by static bomb calorimeter in an oxygen atmosphere. Flammability was determined using a standard epiradiator. Simultaneously, some other parameters such as elementary chemical composition, heavy metal contents, moisture, density, ash percentage after combustion in the bomb, and main bioclimatic characteristics, were also determined.

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Journal of Thermal Analysis and Calorimetry
Authors:
R. Artiaga
,
A. Garcia
,
L. Garcia
,
A. Varela
,
J. Mier
,
S. Naya
, and
M. Grana

Abstract  

The nickel-titanium alloys are usually known as Shape Memory alloys because of their ability to return to some previously defined shape or size when subjected to the appropriate thermal procedure. Mechanical properties of a nickel titanium wire were investigated by DMTA using cylindrical tension mode. The Young"s modulus, the maximum strain and residual deformation have been calculated. Recovery of previously deformed samples was observed in constant stress temperature ramp tests. Relaxation stress behaviour at temperatures above the austenitic transformation has been studied. The strain and frequency ranges of linear response have been determined by dynamic experiments. Strain amplitude of 0.1% and frequency of 1 Hz have been chosen for the temperature ramp dynamic experiments. A big change between 65 and 95C is observed in the storage modulus. The values of E' at temperatures below and above the transition are essentially constant. Finally, the effects of the frequency at different temperatures have been examined.

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Abstract  

Phosphate rocks are used for phosphoric acid production, which is the basis of agricultural phosphate fertilizers. It is known that phosphate ores contain, due to geological reasons, important amounts of natural radioactivity, mainly U-isotopes and daughters. By studying a specific case in Southwestern Spain, it is shown that the operation of phosphate fertilizer factories clearly enhance the natural radiation levels of its close environment. Levels of U-, Th-isotopes, and other natural radionuclides are given for a wide set of different samples, which support such a conclusion. In addition, the study of isotopic ratios gives information on the environmental behavior of such radionuclides.

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Abstract  

The evaporation of octanoic (caprylic) acid was investigated by means of thermogravimetric analysis (temperature range: 300–600 K) under a nitrogen dynamic atmosphere (heating rates: 0.16, 0.31, 0.63, 1.25, 2.5, 5 and 10 K min−1). Kinetic plots for a zero-order process were constructed based on the Arrhenius equation. The activation energy for the evaporation process was calculated via both the Arrhenius plot and Vyazovkin’s isoconversional model-free method.

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Abstract  

The objective of this study is to determine the influence of partial substitutions of Ti4+ by isovalent Hf4+ in the perovskite-type crystalline structure of PbTiO3. Different samples over the whole composition range (0 ≤ x≤1) in the PbTi1-xHfxO3 family have been prepared. Phase transitions have been determined by thermal analysis (differential scanning calorimeter: DSC) and complex impedance spectroscopy (IS) over a wide temperature range. As a consequence of the cation replacement the changes that take place in the different phase transition temperature are reported. By both techniques, thermal analysis and electrical characterization, it is shown that for all compositions prepared there is only one phase transition in a temperature range between 230 and 460 °C. With these results and the previously known crystalline structure of pure PbTiO3 and PbHfO3 perovskites, the phase diagram of the PbTi1-xHfxO3 family is presented including a morphotropic phase transition at x ~ 0.5.

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