149 resultados para Solid state 13C CPMAS NMR


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Solid-state Ln(L)(3) compounds, where Ln stands for trivalent Tb, Dy, Ho, Er, Tm, Yb, Lu and Y, and L is 3-methoxybenzoate, have been synthesized. X-ray powder diffractometry, infrared spectroscopy, complexometry and elemental analysis were used to characterize the compounds. In order to study the thermal behaviour of these compounds simultaneous thermogravimetry and differential thermal analysis (TG-DTA) and differential scanning calorimetry (DSC) were used. The results provided information on the composition, dehydration, polymorphic transformation, thermal stability and thermal decomposition of the synthesized compounds.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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The bis (thiocyanatemercury)tetracarbonyliron, [Fe(CO)4(HgSCN)2], was prepared from [Fe(CO) 5] and Hg(SCN)2, and studied by IR spectroscopy and X-ray diffraction. The compound crystallizes in the tetragonal space group I4,1/a. The unit cell, with dimensions of a = 13.778(3), c = 13.234(3) Å, V = 2512.3(9) Å3, contains four molecules. The iron atom is octahedrally coordinated by four carbonyl groups and two mercury atoms in cis positions. The coordination of the mercury atoms is distorted square-planar, since, besides mercury-iron and mercury-sulphur bonds, there are also mercury-mercury and mercury-nitrogen interactions. The FeHg distance is 2.506(5)Å and the HgFeHg angle is 78.0(1)°. © 1987.

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The 1:1 mixed-ligand [{Cu(N3)2(diEten)}2] (diEten=N,N-diethylethylenediamine) complex has been synthesized and characterized by i.r. spectroscopy and X-ray diffraction. The compound crystallizes in the triclinic space group P1. Its structure consists of a centrosymmetric Cu2N2 unit whose N atoms belong to end-on azido bridges. Each copper atom is also surrounded by three nitrogen atoms; two from one N, N-diethylethylenediamine, and one from the remaining azide. The five nitrogen atoms altogether occupy the vertices of a slightly distorted trigonal bipyramid, and the azidobridges produced a rather short Cu...Cu distance of 3.37 Å. © 1989 Chapman and Hall Ltd.

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Solid state compounds were prepared of Ln-4-MeO-BP, where Ln is a trivalent lanthanide (except promethium) or yttrium, and 4-MeO-BP is 4-methoxybenzylidenepyruvate. 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. © 1993.

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Solid-state compounds Ln-4Cl-BP, where Ln represents lighter trivalent lanthanides and 4Cl-BP is 4-chlorobenzylidenepyruvate, were prepared. Thermogravimetry, derivative thermogravimetry (TG and DTG), differential scanning calorimetry (DSC) and other methods of analysis were used to characterize and to study the thermal behaviour of these compounds.

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Thermogravimetry (TG) and other analysis techniques (EDX, SEM, Mapping surface, X-ray diffraction, inductively coupled argon plasma emission spectroscopy and atomic spectrometry with cold vapor generation) were used to study the reaction of Hg with Rh. The results permitted the suggestion that, when subjected to heat, an electrodeposited Hg film reacts with Rh to form intermetallic products with different stabilities, as indicated by at least three mass loss steps. In the first step, between room temperature and 160°C, only the bulk Hg is removed. From this temperature up to about 175°C, the mass loss can be attributed to the desorption of a film of metallic Hg. The last step, from 175 to 240°C, can be ascribed to the removal of Hg from a thin dark film of RhHg2.

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Some new compounds of cinnamic acid with lighter trivalent lanthanides were prepared in the solid state. The compounds have general formula ML3·H2O, where L is cinnamate (C6H5-CH=CH-COO-) and M is La, Ce, Pr, Nd or Sm. Thermogravimetry, derivative thermogravimetry, differential scanning calorimetry, infrared absorption spectra and X-ray diffraction powder patterns were used to characterize and to study the thermal stability and thermal decomposition of these compounds.

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Pectin lyase (Pl) and polygalacturonase (Pg) production by Thermoascus aurantiacus 179-5 was carried out by means of solid-state determination using orange bagasse and wheat bran as a carbon sources. Pg and Pl had optimum activity at pH 5.0 and 10.5 respectively. Maximal activity of the enzymes were determined at 65 °C. Pg was stable in the acidic to neutral pH range and at 60 °C for 1 h. whereas Pl was stable at acidic pH and at 60 °C for 5 h. © 2002 Elsevier Science Ltd. All rights reserved.