Compostos organolantanídeos contendo o ligante pirazinamida: síntese, caracterização e atividade catalítica na polimerização do etileno

In this work we report the synthesis of some organolanthanide compounds which were identified as LnCl2Cp(PzA)2, Ln = Nd, Sm, Eu and Tb, Cp = cyclopentadienyl and PzA = pirazinamide, by elemental analyses, complexometric titration with EDTA, thermal analyses and IR spectra. Thermal analysis and infrared spectra indicated that the coordination of the pyrazinamide to the lanthanide ions was made by the O atom of the carbonyl group and by one or both N atoms of the pyrazinamide ring. This class of compound showed catalytic activity of ca. 4.0 to 6.4 kgPE molLn-1 h-1 bar-1, in ethylene polymerization, using methylaluminoxane as cocatalyst. The resulting polyethylene presented low crystallinity (20%).

Síntese, caracterização e estudo das propriedades catalíticas e magnéticas de nanopartículas de Ni dispersas em matriz mesoporosa de SiO2

Nickel nanoparticles supported on amorphous silica ceramic matrix were synthesized by the polymeric precursor method. The nanostructure was characterized by NMR, BET, XRD, SEM, TEM, and flame atomic absorption spectrometry techniques. It was observed a dependence of the crystallite size on the thermal annealing, under a N2 atmosphere. The materials presented a high catalytic activity and selectivity upon the beta-pinene hydrogenation reaction. The magnetic hystereses were also correlated with the morphology of the processed material.

Obtenção e caracterização de blendas colágeno-quitosana

Biodegradable polymer blends were obtained using collagen and chitosan. Membranes of collagen and chitosan in different proportions (3:1, 1:1 and 1:3) were prepared by mixing their acetate solutions (pH 3.5) at room temperature. The blends were characterized by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), Fourier Transform infrared (FTIR) spectroscopy, specific viscosity, water absorption and stress-strain assays. The results showed that chitosan did not interfere in the structural arrangement of the collagen triple helix and the properties of the blends can be controlled by varing the proportion of the collagen and the chitosan.

Distribuição de metais e caracterização das constantes de troca entre espécies metálicas e frações húmicas aquáticas de diferentes tamanhos moleculares

In this work the metal distribution and exchange constants between metal species and aquatic humic fractions with different molecular sizes were studied. The aquatic humic substances (AHS) were extracted by XAD-8 resin from water sample collected from Itapitanguí river, São Paulo State, Brazil. The AHS were fractionated in six fractions with different molecular sizes (>100 - <5 kDa) and characterized by several techniques. Molar ratios H/C suggested higher aromaticity for fractions F1 and F6 whereas molar ratios C/N didn´t show any differences regarding the humification degree between the fractions. The UV-Vis absorbance a254/a436 ratio showed higher results for F4 and F5, probably by less condensed features. FTIR studies showed high similarity in the functional groups in the fractions. The highest percentage of traces of Co, Al, Fe, Mn, Cu, Zn and Ni (determined by ICP-AES) was preferably complexed by fractions F3 and F4 with a greater amount of dissolved organic carbon (DOC). In addition, the exchange constants, determined by ultrafiltration method, showed complexes AHS-Fe and AHS-Al with higher stability than complexes AHS-Co in all fractions.

Caracterização e classificação do resíduo sólido "pó do balão", gerado na indústria siderúrgica não integrada a carvão vegetal: estudo de um caso na região de Sete Lagoas/MG

This research was developed by considering that the solid waste produced in the process of pig iron production represents the loss of raw materials and the increase in environmental problem. The charcoal based mini blast-furnace off gases dust named CHARCOK was collected from SIDERPA ¾ Siderúrgica Paulino Ltda, located in Sete Lagoas, Minas Gerais. The Charcok was characterized and classified according to ABNT (Associação Brasileira de Normas Técnicas) standard. The results showed that the Charcok should be classified as Class I Wastes ¾ "Hazard Wastes" because of its high concentration of phenols (54.5mg C6H5OH/kg). The Charcok had high concentration of iron and charcoal which can be used as energy source.

Formação e caracterização óptica de filmes automontados de POMA/PPV

A study is presented of the formation and optical properties of polymeric heterostructures from poly(p-phenylene vinylene) (PPV) and poly(o-methoxyaniline) (POMA) produced via the self-assembly technique. POMA layers were obtained in a non self-limiting process from its emeraldine salt, semiconducting form in HCl solution. Thermal conversion of PPV was performed at low temperatures with the substitution of the counter-ion Cl in the PPV precursor by a long sulfonic chain, the dodecylbenzenesulfonate (DBS) ion. The optical properties of PPV films converted in this way are not affected by POMA, which can be used as transparent electrode of PPV luminescent devices.

Síntese e caracterização de um composto VOPO4-DMA

A layered matrix, alpha-VOPO4.2H2O was used as host species to produce a VOPO4.dimethylacetamide intercalation compound. The oxovanadium matrix and the synthesized hybrid were characterized by elemental analysis, infrared spectroscopy, thermogravimetry, X-ray diffractometry and SEM microscopy. The X-ray diffraction patterns show that the VOPO4.dimethylacetamide compound is amorphous, but can be turned lamellar after a solubilization-crystallization process. The SEM micrographs obtained for the VOPO4-dimethylacetamide hybrid matrix show that the microstructure of VOPO4.2H2O is changed after reaction, with a delamination of the oxovanadium matrix.

Um novo modelo para os sítios de interação dos antagonistas H2, baseado na caracterização química dos sítios primário e secundário por QSAR- 3D

A new model for the H2 antagonists binding site is postulated based on adsorption coefficient values of sixteen antagonists, in the affinities constants of the primary and secondary binding sites, and in the chemical characterization of these sites by 3D-QSAR. All study compounds are in the extended conformation and deprotonated form. The lateral validation of the QSARs, CoMFA analysis, affinity constants and chemical similarity data suggest that the antagonists block the proton pump in the H2 receptor interacting with two tyrosines - one in the helix 5, and other in the helix 6.

Caracterização e estabilidade físico-química de sistemas poliméricos nanoparticulados para administração de fármacos

Polymeric nanoparticle systems such as nanocapsules and nanospheres present potential applications for the administration of therapeutic molecules. The physico-chemical characteristics of nanoparticle suspensions are important pre-requisites of the success of any dosage form development. The purpose of this review is to present the state of the art regarding the physico-chemical characterization of these drug carriers, in terms of the particle size distribution, the morphology, the polymer molecular weight, the surface charge, the drug content and the in vitro drug release profiles. Part of the review is devoted to the description of the techniques to improve the stability of colloidal systems.

Preparação e caracterização do complexo cobaloxima e sua utilização na construção de um eletrodo modificado: um experimento eletroquímico no curso de graduação

The present experiment describes the preparation, characterization of n-butyl(pyridil)cobaloxime complex and its electrochemical property. The infrared and uv-visible absorption spectra were used to characterize the complex obtained. The infrared spectrum of the compound showed characteristics bands that indicated the formation of the Co-C chemical bond formation. The electronic absorption spectrum in acetonitrile showed transition bands attributed to p-p*, metal-to-ligand charge transfer, d-d transitions and charge transfer Co-C. The electrochemical property was investigated by the pulse differential voltammetry technique. Two oxidation processes: Co(I)/Co(II) at -423 mV and Co(II)/Co(III) at 752 mV were observed.

Caracterização de amostras comerciais de vermicomposto de esterco bovino e avaliação da influência do pH e do tempo na adsorção de Co(II), Zn(II) and Cu(II)

Some commercial samples of vermicompost from bovine manure (humus) were characterized by thermogravimetry with respect to humidity, organic matter and ash contents, the percentages of which range from 6.55 to 5.35%, 53.01 to 69.96% and 46.44 to 66,14%, respectively. The capacity of adsorption of Cu2+, Zn2+ and Co2+ ions by these samples has been evaluated as a function of pH and time. The contents of several metal ions in the original vermicompost samples have been determined by flame atomic absorption spectrometry after digestion in a microwave oven. The high nitrogen content suggests that the earthworms used in the maturation procedure lead to an efficient degradation of organic matter. The metal retention was affected by both pH and adsorption time. The results also show that adsorption follows the order Cu2+ > Zn2+ > Co2+.

Irradiação de polímeros com feixe de elétrons: caracterização de íons positivos através da técnica de tempo-de-vôo

With the aim of studying the interaction of fast electrons with solid surfaces we have developed an experimental set-up based on electron stimulated desorption (ESD) coupled to time-of-flight (TOF) mass spectrometry. Poly(methyl methacrylate) and poly(vynil chloride) samples have been irradiated by a pulsed electron beam of 1.2 keV and 0.18 µs FWHM. The results show that H+ is the main ionic species to desorb after electron bombardment. In addition, other ionic fragments were also observed and assigned. These results show the potentiality of this technique in the study of ESD of polymers.

Caracterização química do óleo da amêndoa de Sterculia striata St. Hil. et Naud

This paper describes total lipid content, unsaponifiable fraction and the acid, refractive, saponification and iodine indices of the oil of Sterculia striata nuts. The fatty acids, the sterols and the triterpene alcohols were determined. The percentage of cyclopropenoid fatty acids (CPFA), determined by NMR ¹H (15,5%), makes the nuts of this species unsuitable for human consumption.

Síntese, caracterização e propriedades espectroscópicas de criptatos de lantanídeo do tipo [LnÌ(bipy)2py(CO2Et) 2(3+)]

This work reports on the synthesis, characterization (infrared and hidrogen nmr spectra) and photophysical properties (luminescence spectra and emission quantum yield) of the lanthanide cryptates [LnÌ(bipy)2py(CO2Et) 2]3+ with Ln = Eu3+, Tb3+ or Gd3+, which can be applied as efficient Light-Conversion-Molecular-Devices. From emission spectra of [EuÌ(bipy)2py(CO2Et) 2]3+ it was possible to assign C3 symmetry to the metal ion. The spectroscopic studies show a higher emission quantum yield (q=25%) for [TbÌ(bipy)2py(CO2Et) 2]3+ in aqueous solution, whereas the europium cryptate presents q=14%. This is justified by a more efficient energy transfer between triplet and emission levels of terbium (T->5D4).

Biodiesel de soja: taxa de conversão em ésteres etílicos, caracterização físico-química e consumo em gerador de energia

Biodiesel was produced by the transesterification of neutral soybean oil and anhydrous ethanol using NaOH as catalyst. Combinations of biodiesel and diesel in the proportions of 0, 5, 10, 20, 40, 60, 80 and 100% were tested, respectively, as fuel in an energy generator. The average consumption and mixture performance were analysed. The tests showed a reduction in Diesel oil consumption when mixed with up to 20% of biodiesel. The quality characteristics of these fuels were analyzed.