872 resultados para Solid state NMR


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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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Solid state Ln-4-Me-BP compounds, where Ln stands for lighter trivalent lanthanides (lanthanum to europium) and 4-Me-BP is 4-methylbenzylidenepyruvate, have been synthesized. Elemental analysis, complexometry, X-ray powder diffractometry, infrared spectroscopy and simultaneous thermogravimetry-differential thermal analysis (TG-DTA), have been used to characterize and to study the thermal behaviour of these compounds. The results provided information concerning the stoichiometry, crystallinity, thermal stability and thermal decomposition. (C) 2002 Elsevier B.V. B.V. All rights reserved.

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By close control of experimental variables affecting precipitation, solid-state compounds of the type Th(OH)(m)L4-m.nH(2)O, where L stands for 4-methoxy-benzylidenepyruvate, cinnamylidenepyruvate or 4-dimethylaminocinnamylidene-pyruvate; m=0 to 3 and n=0.5-3 were isolated. Chemical analysis, TG, DTG, DSC and X-ray powder diffractometry have been employed to characterize and to study the thermal behavior of these compounds in dynamic air atmosphere. In all cases, hydration water is slowly lost between 30 and 160degreesC; a continuous, slow rate, mass loss is observed thereafter and beyond 280-400degreesC the rate of decomposition/oxidation increased rapidly, to give ThO2 as the final product, beginning at 412-510degreesC. The results associated with the hydroxo-compounds indicate that the loss of constitution water (OH ions) and the decomposition / oxidation of the organic moieties occur as simultaneous process.

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Solid-state M-2-Cl-BP, where M stands for Mn, Fe, Co, Ni, Cu, Zn and Pb and 2-Cl-BP is 2-chlorobenzylidenepyruvate, have been synthesized. Thermogravimetry and derivative thermogravimetry (TG/DTG), simultaneous thermogravimetry and differential thermal analysis (TG-DTA), X-ray powder diffractometry, infrared spectroscopy, elemental analysis, and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds.

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Thermogravimetry, Differential Scanning Calorimetry and other analytical techniques (Energy Dispersive X-ray Analysis; Scanning Electron Microscopy; Mapping Surface; X-ray Diffraction; Inductively Coupled Plasma Atomic Emission Spectroscopy and Cold Vapor Generation Atomic Absorption Spectroscopy) have been used to study the reaction of mercury with platinum foils. The results suggest that, when heated, the electrodeposited Hg film reacts with Pt to form intermetallic compounds each having a different stability, indicated by at least three mass loss steps. Intermetallic compounds such as PtHg4, PtHg and PtHg2 were characterized by XRD. These intermetallic compounds were the main products formed on the surface of the samples after partial removal of bulk mercury via thermal desorption. The Pt(Hg) solid solution formation caused great surface instability, attributed to the atomic size factor between Hg and Pt, facilitating the acid solution's attack to the surface.

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Solid-state Ln(Bz)(3)center dot H(2)O compounds where Ln stands for trivalent yttrium or lanthanides and Bz is benzoate have been synthesized. Simultaneous thermogravimetry-differential thermal analysis (TG-DTA), X-ray powder diffractometry, infrared spectroscopy and chemical analysis were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, thermal stability and thermal decomposition of the isolated compounds.

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Solid compounds of general formula ML(2) . nH(2)O [where M is Mg, Ca, Sr or Ba; L=4 methoxybenzylidenepyruvate (4-MeO-BP); n = 4, 1 or 0] have been synthetized. Thermogravimetry (TG), derivative thermogravimetry (DTG), differential scanning calorimetry (DSC), x-ray diffraction powder patterns and elemental analysis have been used to characterize the compounds. The thermal stability of these compounds as well as that of the decomposition products were studied using Pt or Al2O3 crucibles in an air or a CO2 atmosphere.

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Tin(II) complexes with 8-hydroxyquinolinate in solid state have been obtained by adding aqueous ammonium to a solution containing stannous chloride and 8-hydroxiquinoline in medium of HCl and acetone up to pH 5 and 9, respectively. The products obtained show the same composition, Sn(C9H6ON)(2); however there are some differences regarding both the thermal behaviour in an oxidant atmosphere and morphology. These products were characterised by elemental and complexometric analysis, TG and DTA curves, infrared and X-ray diffractometry. TG curves show, above 448 K, the partial oxidation on air atmosphere of Sn(II) complexes to Sn(IV) complexes, SnO(C9H6ON)(2). This behaviour does not depend only on pH in which the compounds were obtained but also on the heating rate in TG curves. Sn(II) complexes volatilise almost completely on nitrogen atmosphere and partially on air atmosphere depending on the oxidation degree of the compound.

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In situ solid state oxidation reaction for an alternative La1-xSrxMnO3 (x = 0, 0.1, 0.2 and 0.3) formation is reported. Samples have been obtained by using strontium peroxide, lanthanum and manganese (III) oxide reagents. Strontium peroxide has induced the oxidation of Mn+3 to Mn+4. Lanthanum strontium-doped manganite was obtained without secondary phase formation. La0.825Sr0.175MnO3 showed two structural transitions. The first from 88 to 373 K and the second at 1073 K. which are explained by Jahn-Teller effect at low temperature and cation displacement at high temperature. (C) 2001 Elsevier B.V. B.V. All rights reserved.

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The reactions of the pseudohalide-bridged dimer [Pd(N,C-dmba)(mu -SCN)](2) (1) (dmba = N,N-dimethylbenzylamine) with cis-Ph2PCH=CHPPh2 (cis-dppet) (1:1 molar ratio) and of [Pd(N,C-dmba)(mu -NCO)](2) (2) with Ph2PCH2CH2PPh2 (dppe) (1:2 molar ratio) gave mononuclear [Pd(C-dmba)(SCN)(cis-dppet)].H2O (1a) and [Pd(C-dmba)(NCO)(dppe)] (2a), respectively, with the diphosphines acting as chelating ligands. Reaction of (2) with Fe(C5H4PPh2)(2) (dppf) (1:1 molar ratio) yielded [{Pd(N,C-dmba)(NCO)}(2)(mu -dppf)] (2b), a bimetallic species containing two palladium atoms bridged by the diphosphine, whereas reaction in a 1:2 molar ratio gave the mononuclear [Pd(N,C-dmba)(dppf)][NCO]. CH2Cl2 (2c), with the diphosphine acting as a chelating ligand. The compounds have been characterized by elemental analysis, i.r., P-31{H-1}, C-13- and H-1-n.m.r. spectroscopies. Conductivity measurements together with spectroscopic data showed that (1a) and (2a) do not have the same structure in the solid state and in MeCl solution, whereas for compounds (2b) and (2c) no structural changes were observed when the solids were dissolved in MeCl.