932 resultados para Crystallization and thermal analysis


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Solid state chelates of general formula H-2[M(EDTA)] . nH2O, where M is Co, Ni, Cu or Zn, and EDTA is ethylenediaminetetraacetate, were prepared. Thermogravimetry-derivative thermogravimetry (TG-DTG), differential thermal analysis (DTA) and complexometry were used to characterize and to study the thermal stability and thermal decomposition of these compounds.

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Solid state Ln-4-Me-BP compounds, where Ln stands for heavier trivalent lanthanides (gadolinium to lutetium) and yttrium(III) and 4-Me-BP is 4-methylbenzylidenepyruvate (CH3-C6H4-CH=CH-COCOO-), have been synthesized. Elemental analysis, complexometry, X-ray powder diffractometry, infrared spectroscopy and simultaneous thermogravimetry-differential thermal analysis (TG-DTA), have been used to characterise and to study the thermal behaviour of these compounds. The results provided information concerning the stoichiometry, crystallinity, ligand's denticity, thermal stability and thermal decomposition. © 2002 Elsevier Science B.V. All rights reserved.

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Solid-state LnL(3) compounds, where L is 2-metboxybenzoate and Ln is light trivalent lanthanides, have been synthesized. Thermogravimetry (TG), differential scanning calorimetty (DSC), X-ray powder diffractometry, infrared spectroscopy and elementary analysis were used to characterize and to study the thermal behaviour of these compounds. The results led to information on the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds. on heating these complexes decompose in three (Ce, Pr) or five (La, Nd, Sm) steps with the formation of the respective oxide: CeO2, Pr6O11 and Ln(2)O(3) (Ln=La, Nd, Sm) as final residues. The theoretical and experimental spectroscopic study suggests predominantly the ionic bond between the ligand and metallic center.

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Solid state chelates of general formula H[Ln(EDTA)] · nH2O (Ln = trivalent lanthanide (except for promethium) or yttrium; EDTA = ethylenediaminetetraacetate) were prepared. Thermogravimetry, differential thermal analysis. X-ray diffraction and complexometry were used to characterize and study the thermal stability and thermal decomposition of these compounds. © 1993.

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Four new heterobimetallic metal carbonyls were synthesized by the reaction of [W(CO)4(bipy)] (1) with copper(I) compounds leading to species with the general formula [W(CO)4(bipy)(CuX)] (X = Cl, N3, ClO4, BF4) (2-5). The metal carbonyl compounds were characterized by elemental analysis, infrared and UV -visible electronic spectroscopy and thermogravimetric analysis. The IR data for 2-5 show carbonyl stretching band patterns similar to compound 1 ; ie they exhibit the same number of bands. The UV - vis results show a dissociation reaction generating the starting compound 1 and CuX as consequence of a weak interaction between 1 and CuX. Thermal decomposition mechanisms as well as the thermal stability are influenced by the CuX fragments. The thermal stability decreases in the order [W(CO)4(bipy)] > [W(CO)4(bipy)(CuCl)] > [W(CO)4(bipy) (CuBF4)]. The X-ray results show the formation of WO3, CuWO4, Cu2O and CuO as final decomposition products.

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The dimeric compound [Pd(dmba)(μ-Cl)]2 (1) (dmba = N,N-dimethylbenzylamine) reacts with KX, in methanol/acetone, affording the analogous dimeric pseudohalide-bridged species [Pd(dmba)(X)]2 [X = NCO(2), SCN(3), CN(4)]. The compounds were characterized by elemental analysis, infrared spectroscopy, NMR and thermogravimetric analysis. The IR data for 2-4 showed bands typical of coordinated pseudohalide ligands indicating clearly the occurrence of the exchange reaction. Their thermal behavior was investigated and suggested that their thermal stability is influenced by the bridging ligand. The thermal stability decreased in the order [Pd(dmba)(μ-SCN)]2>[Pd(dmba)(μ-Cl)] 2>[Pd(dmba)(;u-NCO)]2>[Pd(dmba)(μ-CN)]2. The X-ray results showed the formation of PdO as final decomposition product. © 1999 Elsevier Science Ltd. All rights reserved.

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Solid M-DMBP compounds, where M represents Mg(II), Ca(II), Sr(II), Ba(II), Ni(II), Cu(II), Zn(II), Fe(III), La(III), Th(IV), and DMBP is 4-dimethylaminobenzylidenepyruvate, have been prepared. Thermogravimetry-derivative thermogravimetry (TG-DTG), differential scanning calorimetry (DSC) and other methods of analysis have been used to characterize and to study the thermal stability and thermal decomposition of these compounds. © 1995.

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Solid-state M-2-MeO-BP compounds, where M represents bivalent Mn, Fe, Co, Ni, Cu, Zn and 2-MeO-BP is 2-methoxybenzylidenepyruvate have been synthesized. Simultaneous thermogravinietry-differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, elemental analysis and complexometry were used to characterize and to study the thermal stability and thermal decomposition of these compounds. The results led to information about the composition, dehydration, crystallinity and thermal decomposition of the isolated compounds.

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Solid state Ln-DMBP compounds, where Ln represents trivalent lanthanides (except for promethium) and yttrium, and DMBP is 4-dimethylaminobenzylidenepyruvate, were prepared. Thermogravimetry (TG), differential thermal analysis (DTA), and other methods of analysis were used to characterize and to study the thermal stability and thermal decomposition of these compounds. © 1993.

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Mach number and thermal effects on the mechanisms of sound generation and propagation are investigated in spatially evolving two-dimensional isothermal and non-isothermal mixing layers at Mach number ranging from 0.2 to 0.4 and Reynolds number of 400. A characteristic-based formulation is used to solve by direct numerical simulation the compressible Navier-Stokes equations using high-order schemes. The radiated sound is directly computed in a domain that includes both the near-field aerodynamic source region and the far-field sound propagation. In the isothermal mixing layer, Mach number effects may be identified in the acoustic field through an increase of the directivity associated with the non-compactness of the acoustic sources. Baroclinic instability effects may be recognized in the non-isothermal mixing layer, as the presence of counter-rotating vorticity layers, the resulting acoustic sources being found less efficient. An analysis based on the acoustic analogy shows that the directivity increase with the Mach number can be associated with the emergence of density fluctuations of weak amplitude but very efficient in terms of noise generation at shallow angle. This influence, combined with convection and refraction effects, is found to shape the acoustic wavefront pattern depending on the Mach number.

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In this work, mesoporous titania is prepared by templating latex sphere arrays with four different sphere diameters at the micrometric scale (phi > 1 mu m). The mesoporous titania homogeneously covers the latex spheres and substrate, forming a thin coating characterized by N-2 adsorption isotherm, small angle X-rays scattering, atomic force, field emission and transmission electronic microscopies. Mesoporous titania has been templated into different shapes such as hollow particles and monoliths according to the amount of sol used to fill the voids of the close packed latex spheres. Titania topography strongly depends on the adsorption of polymeric segments over latex spheres surface, which could be decreased by changing the dimensions of latex spheres (phi = 9.5 mu m) generating a lamellar architecture. Thus, micrometric latex sphere arrays can be used to achieve new surface patterns for mesoporous materials via a fast and inexpensive chemical route for construction of functional devices in different technological fields such as energy conversion, inclusion chemistry and biomaterials. (C) 2011 Elsevier Inc. All rights reserved.

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The aim of this research was to characterize emulsion systems (ES) containing nonionic ethoxylated surfactants by using rheological, microscopic, and thermogravimetric assays. Three formulations were developed: ES-1: 8.0% (w/w) oleth-20; ES-2: 4.0% (w/w) oleth-20/4.0% (w/w) steareth-21; and ES-3: 8.0% (w/w) steareth-21. The systems showed typical non-Newtonian pseudo-plastic behavior. The presence of a lamellar gel phase was observed for all systems, with ES-2 being more pronounced. Through thermogravimetry, the profiles of the three systems were found to be similar, consisting of two main events, the first one being characterized by loss of water and, beyond 110 degrees C, by loss of the oil phase.

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The most important property of austenitic stainless steels is corrosion resistance. In these steels, the transition between paramagnetic and ferromagnetic conditions occurs at low temperatures. Therefore, the use of austenitic stainless steels in conditions in which ferromagnetism absence is important can be considered. On the other hand, the formation of strain-induced martensite is detected when austenitic stainless steels are deformed as well as machined. The strain-induced martensite formed especially in the machining process is not uniform through the chip and its formation can also be related to the Md temperature. Therefore, both the temperature distribution and the gradient during the cutting and chip formation are important to identify regions in which martensite formation is propitiated. The main objective here is evaluate the strain-induced martensite formation throughout machining by observing microstructural features and comparing these to thermal results obtained through finite element method analysis. Results show that thermal analysis can give support to the martensite identified in the microstructural analysis.