Preparo de filmes-suporte para microscópio eletrônico

Working with low voltage microscope (R.C.A., EMC-2, of 30KV.) the authors verified that parlodion and Formvar films are quickly destroyed by intense heating under the electron beam. They have tried to employ oxide films, as Al2O3 and SiO, more resistant to heat. Al2O3 films are prepared by anodic oxidation of thin aluminium sheets, under 8 to 10 volts in a 3% ammonium citrate solution and subsequent aluminium dissolution in a O.25% HgCl2 solution. These films are very suitable when prepared with highly pure aluminium of extremely homogeneous surface. Best results were obtained with SiO films, evaporated in high vacuum over Parlodion films mounted on metallic grids. Employing 1 or 1.5 mg of SiOm highly homogeneous and resistant films are obtained, having little inferior transparence than the Parlodion ones. Pure SiO films (1.5 mg) are obtained by elimination of the Parlodion under slow heating until 250°C; they are greatly transparent but little resistant to water, thus beeing indicated in dry preparations. For particles which deposite in a chain-like form around thin fibers, the authors employ the mounting on Parlodion fibers, obtained by heating Parlodion films on microscope grids about 190°C.

Influence of the use of acids and films in post-harvest lychee conservation

Lychee (Litchi chinensis Sonn.) has a high commercial value; however, it has a short shelf-life because of its rapid pericarp browning. The objective of this study was to evaluate the shelf-life of 'Bengal' lychee fruits stored after treatment with hydrochloric acid and citric acid, associated with cassava starch and plastic packaging. Uniformly red pericarp fruits were submitted to treatments: 1-(immersion in citric acid 100 mM for 5 minutes + cassava starch 30 g L-1 for 5 minutes), 2-(immersion in hydrochloric acid 1 M for 2 minutes + starch cassava 30 g L-1 for 5 minutes), 3-(immersion in citric acid 100 mM for 5 minutes + polyvinyl chloride film (PVC, 14 µm thick)) and 4-(immersion in hydrochloric acid 1 M for 2 minutes + PVC film). During 20 days, the fruits were evaluated for mass loss, pericarp color, pH, soluble solids and titratable acidity, vitamin C of the pulp and pericarp and activities of polyphenol oxidase and peroxidase of the pericarp. The treatment with hydrochloric acid associated with PVC was the most effective in maintaining the red color of the pericarp for a period of 20 days and best preservation of the fruit. The cassava starch associated with citric acid, and hydrochloric acid did not reduce the mass loss and did not prevent the browning of lychee fruit pericarp.

Recuperação de metais de catalisadores usados de hidrotratamento (NiMo E CoMo/AL2O3)

This work presents a detailed study of the leaching behavior of deactivated hydrotreating catalysts (CoMo, NiMo/Al2O3) in presence of oxalate and NH4+ ions in various media. The yield of metals recovery may be optimized by adjusting several experimental parameters (time, temperature, etc). Leaching is limited by physical factors (diffusional effects caused by coke) and by the existence of silicate/spinel-like species which are poorly soluble in leaching solutions. Coke may be eliminated by an oxidation step at temperatures between 300-400ºC. Above 400ºC, solubilization of Ni and Co is drastically reduced. 50-90% wt of sulphate species and 15-30% wt of phosphate ions are solubilized during leaching. Silicon (as SiO2) is not solubilized. The best Ni-Co-Mo recoveries are in the 70-90% wt range; Fe recovery may be quantitative, whereas Al leaching may be lower than 5% wt.

Caracterização de catalisadores Cu/CeO2/Al2O3 por redução a temperatura programada e atividade para oxidação de CO

The kinetic parameters for the CO oxidation reaction using copper/alumina-modified ceria as catalysts were determined. The catalysts with different concentrations of the metals were prepared using impregnation methods. In addition, the reduction-oxidation behaviour of the catalysts were investigated by temperature-programmed reduction. The activity results show that the mechanism for CO oxidation is bifunctional : oxygen is activated on the anionic vacancies of ceria surface, while carbon monoxide is adsorbed preferentially on the higher oxidation copper site. Therefore, the reaction occurs on the interfacial active centers. Temperatures-programmed Reduction patterns show a higher disperdion when cerium oxide is present.

Catalisadores Ni/Al2O3 promovidos com molibdênio para a reação de reforma a vapor de metano

Mo-promoted Ni/Al2O3 catalysts for the methane steam reforming reaction were studied in this work. The Ni/Al2O3 catalysts were prepared by precipitation and molibdenum was added by impregnation up to 2%wt. The solids were tested using a micro-reactor under two H2Ov/C conditions and were characterized by ICP-OES, XRD, N2 adsoption, H2 chemisorption and TPR. NiO and NiAl2O4 phases were observed and the metallic area decreased with the increase of the Mo content. From the catalytic tests high stability was verified for H2Ov/C=4.0. On the other hand, only the catalyst containing 0,05% Mo stayed stable during 30 hours of the test at H2Ov/C=2.0.

Estudo microestrutural do catalisador Ni/gama-Al2O3: efeito da adição de CeO2 na reforma do metano com dióxido de carbono

The carbon dioxide reforming of methane was carried out over nickel catalysts supported on the gamma-Al2O3/CeO2 system prepared by wet impregnation. With the increase of the CeO2 weight in the catalyst, a higher stability was observed in the catalytic activity, together with an excellent resistance to carbon deposition and a better Ni dispersion. The catalysts were characterized by means of surface area measurements, TPR, H2 chemisorption, XRD, SEM, EDX, XPS and TEM. An interaction between Ni and CeO2 was observed to the Ni/CeO2 sample after activation in a H2 atmosphere above 300 ºC. Such behavior has a significantly influence on the catalytic activity.

Efeito do teor metálico em catalisadores Co/Al2O3 aplicados à reação de reforma a vapor de etanol

The development of cobalt catalysts to produce hydrogen from ethanol is the goal of this investigation. Co/Al2O3 catalysts were prepared by impregnation and characterized by atomic absorption, nitrogen adsorption, X-ray diffraction, Raman spectroscopy, temperature programmed reduction and carbon analysis. The catalysts contained Co3O4 oxide and Co3+ and Co2+ species interacting with alumina. The cobalt load affects the crystal size and the crystalline structure and higher Co loads influence the reaction mechanism, changing the selectivity of the catalysts, decreasing the amount of CO produced and avoiding the formation of products catalyzed by the support. The ethanol conversion was 50-70% with 10-<1% of CO in the hydrogen.

Catalisador Pd/gama-Al2O3: efeito do tamanho de partícula na atividade catalítica para combustão do CH4

Methane, the main constituent of natural gas (> 85%), is employed in large scale as an energy source (thermoelectric power plants, automobiles, etc). However, significant quantities of this gas contribute to the greenhouse effect. The catalytic combustion of methane can minimize these emissions. Palladium is one of the metals that shows the highest activity, depending on the different active forms of the metal. In this article, we focus on the influence of particle size and pretreatment on the catalytic performance of palladium in the methane combustion reaction.

Use of thin films obtained by plasma polymerization for grain protection and germination enhancement

In this work, preliminary results of the use of hydrophobic thin films obtained by plasma deposition to protect grains and seeds are presented: grains coated by the films did not present biological degradation when stored in a saturated water vapor environment, but had their germination accelerated in the presence of water. A model that explains the difference of behavior of the films when exposed to water in vapor form or in liquid form, based on the formation of microchannels within the film that lead to water uptake in seeds, is presented. The model was successfully tested using quartz crystal measurements, which showed that the microchannels within the films can favor the adsorption and permeation of water when the films are immersed in water.

Produção de hidrogênio a partir da reforma a vapor de etanol utilizando catalisadores Cu/Ni/gama-Al2o3

Cu/Ni/gamma-Al2O3 catalysts were prepared by an impregnation method with 2.5 or 5% wt of copper and 5 or 15% wt of nickel and applied in ethanol steam reforming. The catalysts were characterized by atomic absorption spectrophotometry, X-ray diffraction, temperature programmed reduction with hydrogen and nitrogen adsorption. The samples showed low crystallinity, with the presence of CuO and NiO, both as crystallites and in dispersed phase, as well as of NiO-Al2O3. The catalytic tests carried out at 400 ºC, with a 3:1 water/ethanol molar ratio, indicated the 5Cu/5Ni/Al2O3 catalyst as the most active for hydrogen production, with a hydrogen yield of 77% and ethanol conversion of 98%.

Decomposição térmica de espumas de poliuretano para fabricação de vitrocerâmica celular de Li2O-ZrO2-SiO2-Al2O3 (LZSA)

Characterization of the thermal decomposition of polyurethane (PUR) foams was performed by Fourier-transformed infrared (FT-IR) spectroscopy and thermogravimetric analysis (TGA). Three main weight loss paths were observed by TGA, the residue being lower than 3 wt.% for 3 different PUR foams analyzed. FT-IR spectra indicated CO2, CO, NH3 and isocyanides as main decomposition products. PUR foams of different cell sizes were immersed in a slurry of the parent glass ceramic of composition Li2O-ZrO2-SiO2-Al 2O3 (LZSA) and submitted to heat treatment. The LZSA cellular glass ceramics obtained after sintering and crystallization resembled the original morphology of the PUR foams.

Cinética de redução do catalisador CuO/ZnO/Al2O3

The reduction kinetics of a CuO/ZnO/Al2O3 catalyst by hydrogen was investigated isothermally and by temperature programmed reduction (TPR). Two reducible Cu2+ species were detected; the first one was identified as CuO bulk and the other as Cu2+ strongly interacting with alumina, possibly in the form of copper aluminate. The activation energies for the reduction of these two species were 60 and 90 kJ mol-1, respectively, and the reaction order with respect to hydrogen was one. The isothermal reduction data showed that the isotropic growth model is the most appropriate to describe the reaction rate data for both Cu2+ species.

Plasma polymerized acetaldehyde thin films for retention of volatile organic compounds

The aim of this work is the production and characterization of plasma polymerized acetaldehyde thin films. These films show highly polar species, are hydrophilic, organophilic and easily adsorb organic reactants with CO radicals but only allow permeation of reactants with OH radicals. The good step coverage of films deposited on aluminum trenches is useful for sensor development. Films deposited on hydrophobic substrates may result in a discontinued layer, which allows the use of preconcentration in sample pretreatment. Deposition on microchannels showed the possibility of chromatographic columns and/or retention system production to selectively detect or remove organic compounds from gas flows.

Preparation and characterization oF Ru-Sn/Al2O3 catalysts for the hydrogenation of fatty acid methyl esters

Ru-Sn/Al2O3 catalysts with different Sn loadings were prepared by the coimpregnation method. Several characterization techniques such as TPR, pyridine TPD and catalytic tests for dehydrogenation and hydrogenolysis were used to evaluate and compare such catalysts. TPR results indicate that Sn is deposited both onto the support and as species strongly interacting with Ru. Such non selective deposition modifies the acid and metallic functions of the catalysts. Both total acidity and acid strength distribution are affected: total acidity decreases and new sites of lower acid strength are created. Both dehydrogenating and hydrogenolytic activities are strongly diminished by the addition of Sn. Results of catalytic tests for methyl oleate hydrogenation indicate that methyl stearate is the main product, with only minute amounts of oleyl alcohol produced, and that the addition of Sn diminishes the hydrogenation activity.

Citric acid as multifunctional agent in blowing films of starch/PBAT

Citric acid was used as a compatibilizer in the production of starch and PBAT films plasticized with glycerol and processed by blow extrusion. Films produced were characterized by WVP, mechanical properties, FT-IR-ATR and SEM. WPV ranged from 3.71 to 12.73×10-11 g m-1 s-1 Pa-1, while tensile strength and elongation at break ranged from 1.81 to 7.15 MPa and from 8.61 to 23.63%, respectively. Increasing the citric acid concentration improved WVP and slightly decreased film resistance and elongation. The films micrographs revealed a more homogeneous material with the addition of citric acid. However, the infrared spectra revealed little about cross-linking esterification reaction