265 resultados para Powders: solid state reaction
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Foram sintetizados compostos Ln-L no estado sólido, onde Ln significa os lantanídeos leves trivalentes e L é o piruvato. Estes compostos foram caracterizados e estudados utilizando-se a Termogravimetria e Termogravimetria derivada (TG/DTG), calorimetria exploratória diferencial (DSC) difratometria de raios X pelo método do pó, espectroscopia na região do infravermelho, análise elementar e complexometria. Os resultados permitiram obter informações com respeito a composição, desidratação, sitio de coordenação, comportamento térmico e a decomposição térmica destes compotos.
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Solid-state compounds of general formula Ln(2)L(3)center dot nH(2)O, where L represents 1,4-bis(3-carboxy-3-oxo-prop-1-enyl)benzene and Ln = La, Ce, Pr, Nd, Sm, were synthesized. Complexometric titrations with EDTA, thermogravimetry (TG), differential thermal analysis (DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, elemental analysis and infrared spectroscopy have been employed to characterize and to study the thermal behavior of these compounds in dynamic air atmosphere. The results led to information about the composition, dehydration, crystallinity, and thermal decomposition of the synthesized compounds.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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The main goal in this work is to conduct a quantitative analysis of the mechanical stir casting process for obtaining particulate metal matrix composites. A combined route of stirring at semi-solid state followed by stirring at liquid state is proposed. A fractional factorial design was developed to investigate the influence and interactions of factors as: time, rotation, initial fraction and particle size, on the incorporated fraction. The best incorporations were obtained with all factors at high levels, as well as that very long stirring periods have no strong influence being particle size and rotation the most important factors on the incorporated fraction. Particle wetting occurs during stirring at semisolid state, highlighting the importance of the interactions between particles and the alloy globularized phase. The role of the alloying element Mg as a wettability-promoting agent is discussed. The shear forces resulting from the stirring system is emphasized and understood as the effect of rotation itself added to the propeller blade geometry.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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A method for the attachment of 2-mercaptothiazoline (MTZ) to modified silica gel has been developed. In the first step, a new silylant agent was synthesized, named SiMTZ, by the reaction between MTZ molecule and chloropropyltrimethoxysilane (SiCl). SiMTZ and tetraethylortosilicate were co-condensed in the presence of n-dodecylamine, a neutral surfactant template, to produce a modified ordered hexagonal mesoporous silica named HMTZ. The modified material contained 0.89 +/- 0.03 mmol of 2-mercaptothiazoline per gram of silica. FT-IR, FT-Raman, Si-29- and C-13-NMR spectra were in agreement with the proposed structure of the modified mesoporous silica in the solid state. HMTZ material has been used for divalent mercury adsorption from aqueous solution at 298 I K. The series of adsorption isotherms were adjusted to a modified Langmuir equation. The maximum number of moles of mercury adsorbed gave 2.34 +/- 0.09 mmol/g of material. The same interaction was followed by calorimetric titration on an isoperibol calorimeter. The HMTZ presented a high capacity for the removal of the contaminant mercury from water. The Delta H and Delta G values for the interaction were determined to be -56.34 +/- 1.07 and -2.14 +/- 0.11 kJ mol(-1). This interaction process was accompanied by a decrease of entropy value (- 182 J mol(-1) K-1). Thus, the interaction between mercury and HMTZ resulted in a spontaneous thermodynamic system with a high favorable exothermic enthalpic effect. (c) 2007 Elsevier B.V. All rights reserved.
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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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The present work describes the preparation and characterization of polyelectrolyte coatings of poly-L-lysine (PLL) to modify a glassy carbon electrode and its application to the pre-accumulation of nitroprusside (NP). The effects of the coating on the electrochemical reduction of NP were investigated. The performance of the modified electrode indicates that the drug can be immobilized by electrostatic interaction and the voltammetric signal monitored at all pH values in the range of 2-12. The strong interaction between NP and PLL stabilizes the complex on the electrode surface and minimizes the chemical reaction of lost CN- ions as a subsequent reaction of electron transfer, which could improve the action mechanism of NP.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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The synthesis and characterization of a new organic ligand monooctyldiphenylphosphinate (L) is described, as well as a new Eu(3+) diketonate complex [Eu(tta)(3)(L)(2)] (tta = thenoyltrifluoracetone). The ligand (L) was formed by substitution reaction (80% yield) and characterized by uni- and bidimensional (1)H, (13)C and (31)P NMR experiments, to confirm its molecular structure. The coordination of (L) to Eu(3+) in the complex [Eu(tta)(3)(L)(2)] was confirmed by FT-IR spectra. The emission spectra present the same profile when excited in Eu(3+) or in the ligands, suggesting an energy transfer from ligands to Eu(3+) ions. The emission spectra of the precursor [Eu(tta)(3)(H(2)O)(2)], and [Eu(tta)(3)(L(2))] present bands arising from f-f intra-configurational transitions. The only (5)D(0)-(7)F(0) transition shows the presence of at least one site without symmetry center. The FWHM of such transition is 7 cm(-1) and 57 cm(-1) for [Eu(tta)(3)(H(2)O)(2)] and [Eu(tta)(3)(L)(2)] complexes, respectively. This widening is provided by the presence of large groups around Eu(3+) ion. The calculated intensity parameters Omega(2) and Omega(4) show that the interaction features between center-ion and ligand are different; the small value of Omega(4) is related to long range effects of alkyl chain. The Langmuir isotherms of this ligand and complex have been investigated although their hydrolysis in water subphase does not allow stable monolayers. (C) 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
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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)