Preparo de óxido de nióbio suportado em alumina por deposição química em fase vapor: caracterização por espectroscopia vibracional e termogravimetria

Alumina supported niobium oxide was prepared by chemical vapor deposition (CVD) of NbCl5. The alumina was calcined and pretreated at differents temperatures in order to vary the density of OH groups on the surface which was determined by thermogravimetric analysis. A good correlation was found between the amount of anchored niobium and the total number of anionic sites (oxide and hydroxyl groups) on the surface of the alumina. The infrared spectra on the OH stretching region indicate that OH groups coordinated to at least one tetrahedral aluminum were more reactive towards NbCl5.

Influência da adição de defloculante, ligante e partículas de alumina no comportamento reológico de suspensões a base de frita e caulim

Enamel suspensions were characterized according to their rheological behavior. The suspensions presented a pseudoplastic behavior, yield stress and thixotropy, with or without the presence of deffloculant. Added carboxymethylcellulose increases the apparent viscosity of enamel suspensions and interacts complexly with the deffloculant, here sodium silicate. Addition of crystalline particles of two types of alumina, used to improve the wear resistance of ceramic glazes, also change strongly the rheological behavior of the suspensions. Added high specific area, irregular alumina particles produce a higher increase of the apparent viscosity of enamel suspensions compared to rounded ones.

Influência do pH sobre a estabilidade de suspensões de alumina estabilizadas eletroestericamente

In this work, aqueous suspensions of aluminas with different particle sizes were evaluated. The effect of pH on the electrosteric stabilization using PMAA-NH4 (ammonium polymethacrylate) as deflocculant was studied. The amount of deflocculant was optimized and rheologic properties were determined at four different pH values. Sedimentation was also evaluated. For suspensions with pH 4, an electrostatic mechanism of stabilization was observed, probably due to a flat adsorption of PMMA- on the alumina surface, leading to a small efficiency in relation to steric stabilization. For a suspension with pH 12, the steric mechanism of stabilization prevails. Suspensions with pH 7 and 9 present a higher flocculation degree. In relation to particle size, A-1000 samples present a smaller particle size, leading to a smaller interparticle distance (IPS), making stabilization more difficult.

On-line preconcentration system using a microcolumn packed with Alizarin Red S-modified alumina for zinc determination by flame atomic absorption spectrometry

A simple and sensitive on-line flow injection system for determination of zinc with FAAS has been described. The method is based on the separation and preconcentration of zinc on a microcolumn of immobilized Alizarin Red S on alumina. The adsorbed analyte is then eluted with 250 µL of nitric acid (1 mol L-1) and is transported to flame atomic absorption spectrometer for quantification. The effect of pH, sample and eluent flow rates and presence of various cations and anions on the retention of zinc was investigated. The sorption of zinc was quantitative in the pH range of 5.5-8.5. For a sample volume of 25 mL an enrichment factor of 144 and a detection limit (3S) of 0.2 µg L-1 was obtained. The precision (RSD, n=7) was 3.0% at the 20 µg L-1 level. The developed system was successfully applied to the determination of zinc in water samples, hair, urine and saliva.

Análises térmicas e processo de sinterização da cerâmica KSr2Nb5O15 dopada com CuO

KSr2Nb5O15 is a ferroelectric material. The sintering process of the KSr2Nb5O15 ceramic doped with different amounts of CuO was investigated in this research. It was found that CuO is effective as promoter of the densification process of the KSN ceramic. The developed microstructures were different due to the amount of CuO and secondary phases were observed in the microstructures. However, the results of X - ray diffraction showed that only the tetragonal tungsten bronze (TTB) structure was identified in all the investigated ceramic systems. The thermal behavior of CuO and also of the CuO - KSN phase mixture was investigated by thermal analysis.

Palladium-supported catalysts in methane combustion: comparison of alumina and zirconia supports

Palladium catalysts supported on alumina and zirconia were prepared by the impregnation method and calcined at 600 and 1000 ºC. Catalysts were characterized by BET measurements, XRD, XPS, O2-TPD and tested in methane combustion through temperature programmed surface reaction. Alumina supported catalysts were slightly more active than zirconia supported catalysts, but after initial heat treatment at 1000 ºC, zirconia supported palladium catalyst showed better performance above 500 ºC A pattern between temperature interval stability of PdOx species and activity was observed, where better PdOx stability was associated with more active catalysts.

Sodium dodecyl sulfate coated γ-alumina support modified by a new Schiff base for solid phase extraction and flame-AAS determination of lead and copper ions

A simple and fast approach for solid phase extraction is herein described, and used to determine trace amounts of Pb2+ and Cu2+ metal ions. The solid phase support is sodium dodecyl sulfate (SDS)-coated γ-alumina modified with bis(2-hydroxy acetophenone)-1,6-hexanediimine (BHAH) ligand. The adsorbed ions were stripped from the solid phase by 6 mL of 4 M nitric acid as eluent. The eluting solution was analyzed by flame atomic absorption spectrometry (FAAS). The sorption recovery of metal ions was investigated with regard to the effects of pH, amount of ligand, γ-alumina and surfactant and the amount and type of eluent. Complexation of BHAH with Pb2+ or Cu2+ ions was examined via spectrophotometry using the HypSpec program. The detection limit for Cu2+ was 7.9 µg L-1 with a relative standard deviation of 1.67%, while that for Pb2+ was 6.4 µg L-1 with a relative standard deviation of 1.64%. A preconcentration factor of 100 was achieved for these ions. The method was successfully applied to determine analyte concentrations in samples of liver, parsley, cabbage, and water.

Efeito da ativação mecânica de uma formulação de talco/caulim/alumina sobre o mecanismo e a cinética de formação de cordierita

In this study, the influence of mechanical activation by intensive ball milling of a stoichiometric mixture of talc, kaolin, and alumina on the mechanism and kinetics of cordierite (2MgO·2Al2O3·5SiO2) formation was evaluated. The raw materials were characterized by chemical analysis, X-ray diffraction (XRD), laser diffraction, and helium pycnometry. The kinetics and mechanism of cordierite formation were studied by XRD, differential thermal analysis, and dilatometry in order to describe the phase formation as a function of temperature (1000-1400 ºC), time of thermochemical treatment (0-4 h), and grinding time of the mixture (0-45 min). Finally, the optimal conditions of the thermochemical treatment that ensured the formation of cordierite were determined: milling time of 45 min and thermal treatment at 1280 ºC for 1 h.

COMPARAÇÃO E CONSTRUÇÃO DE REATORES DE "MILD" E "HARD ANODISATION" PARA FABRICAÇÃO DE ALUMINA ANÓDICA POROSA

The mild anodization (MA) reactor is exemplified for its operational simplicity and its excellent control over the experimental parameters that are involved in the anodization process. This method provides porous anodic alumina films with a regular cell-arrangement structure. This offers a better cost-benefit ratio than the other equipment configurations that are used to fabricate nanoporous structures (i.e., ion beam lithography). Conversely, the hard anodization (HA) reactor produces oxides at a rate that is 25 to 35 times faster than the MA reactor. The produced oxides also have greater layer thicknesses and interpore distance, and with a uniform nanopore spatial order (> 1000). In contrast to MA reactors, the construction of an HA reactor requires special components to maintain anodisation at a high potential regime. Herein, we describe and compare both reactors from a technical viewpoint.

Enterobactérias Patogênicas: seu isolamento das águas superficiais por meio de precipitação química

Enterobacteria of pathogenic group were isolated directly of superficial waters using Alumina Milk as precipitate, being 23 Salmonella, 19 Shigella and 17 Proteus from 18 samples which were collected in brooks and rivers of São Paulo, Brazil.

Ocorrência de montmorilonita em alguns solos desenvolvidos do arenito de Botucatu

Este trabalho foi realizado com o objetivo de estudar a ocorrência de montmorilonita em solos desenvolvidos do arenito de Botucatu no município de Piracicaba. Tais solos são os seguintes: Regossol (série Ribeirão Claro), Podzólico Vermelho Amarelo-variação Laras (série Ibitiruna) e Regossol "intergrade". para Podzólico Vermelho Amarelo. Foram selecionados cinco perfis, sendo dois pertencentes ao Regossol (perfis P1, e Ρ2), dois ao Podzólico (perfis P3 e P4) e um ao Regossol "intergrade" (perfil Ρ5). As amostras dos cinco perfis, em número de 33, foram tratadas convenientemente para se processar a eliminação de sais solúveis e agentes cimentantes (matéria orgânica, óxidos de ferro livres, etc), e assim facilitar o estudo da fração argila. Nesta fração foram feitas as determinações químicas (% de K2O, silica, alumina e C.T.C.) e mineralógicas (raios X e análise térmica diferencial). Também determinações granulométricas e químicas foram realizadas em todas as amostras. Os perfis Ρ1 e P2, que não apresentaram rocha consolidada, tiveram a caolinita como mineral dominante (acima de 50%). Os perfis Ρ3, Ρ4 e Ρ5, que apresentaram como material de origem a rocha arenítica consolidada, tiveram a montmorilonita como mineral dominante, apresentando todavia, diferenças quanto ao teor desse mineral. Assim, o Podzólico Vermelho Amarelo-variação Laras, que possui o arenito de Botucatu de estratificação plano-paralela como material originário, teve um teor médio de montmorilonita de 35%, enquanto que o Regossol "intergrade" para Podzólico Vermelho Amarelo, com o mesmo arenito, mas de estratificação cruzada como material originário apresentou um teor médio de montmorilonita de 57%. A presença da montmorilonita nestes dois solos se deve a uma herança do material originário e não à formação local, por intemperização. Neste caso, o material originário deve ter tido, em outras épocas, condições favoráveis para a formação deste mineral, ou seja, clima semi-árido, riqueza de Ca, Mg, Na, baixa relação Si/Al e baixo teor de H. Pelos resultados obtidos, os perfis Ρ1 e P2), parecem não pertencer ao arenito de Botucatu. Infelizmente, devido à falta de dados mineralógicos da rocha do arenito de Botucatu de outras regiões do Estado, não foi possível verificar se a ocorrência da montmorilonita é ou não comum neste arenito. Outras pesquisas devem ser executadas visando este objetivo.

Conservação da qualidade de caqui 'Fuyu' em ambiente refrigerado pela combinação de 1-MCP e atmosfera modificada

O presente estudo analisou os efeitos do inibidor da ação do etileno 1-MCP (1-metilciclopropeno), da AM (atmosfera modificada) e do oxidante de etileno KMnO4 (permanganato de potássio) sobre a qualidade de caqui 'Fuyu' após a armazenagem refrigerada. Os fatores 1-MCP, AM e KMnO4 foram combinados de quatro maneiras, correspondendo aos seguintes tratamentos: T1) Controle + AM + KMnO4;T2) 1-MCP + AM + KMnO4; T3) 1-MCP + AM, e T4) 1-MCP + AA (AA=atmosfera do ar). Frutos maduro-firmes com coloração da casca predominantemente amarela foram colhidos em sete pomares comerciais no nordeste do Estado do Rio Grande do Sul. Parte dos frutos foi exposta a 0.3 µL L-1 de 1-MCP por 12 h em 24 h após a colheita. A seguir, os frutos foram armazenados sob AA ou sob AM induzida por bolsas de polietileno (0,04 mm de espessura), por 20; 40; 60 ou 80 dias a -0,1±0,8ºC. Dois sachês contendo 8,5 g de Alumina-KMnO4foram adicionados em cada uma das bolsas de polietileno dos tratamentos um e dois, antes de elas serem vedadas. Os frutos de cada período de armazenagem refrigerada foram analisados após 0; 3; 6 ou 9 dias de prateleira sob AA a 22±1ºC. O tratamento 1-MCP retardou o amolecimento da polpa, mas não afetou consistentemente o desenvolvimento de 'estrias' e manchas pretas na superfície dos frutos armazenados sob AM contendo KMnO4. A incidência de 'estrias' e manchas pretas em frutos tratados com 1-MCP e armazenados sob AM foi significativamente menor que a de frutos tratados com 1-MCP e armazenados sob AA. Houve efeitos aditivos do 1-MCP e AM na conservação da firmeza e na redução de danos por frio manifestados pela formação de textura gel-firme e manchas translúcidas na casca. O uso de KMnO4 não aumentou a conservação da qualidade dos frutos quando tratados com 1-MCP e armazenados sob AM. O desenvolvimento dos distúrbios da epiderme dependeu do pomar e de períodos de armazenagem e prateleira. No entanto, os benefícios da combinação de 1-MCP e AM sobre a redução desses distúrbios e do amolecimento dos frutos foram consistentes para todos os pomares. Os resultados indicam que a combinação de 1-MCP e AM é um método efetivo para retardar a deterioração de caqui 'Fuyu' durante e após a armazenagem refrigerada.

Síntesis de espirobrasinoesteroides análogos de la 6-desoxocastasterona

The synthesis of two new spirostanic analogs of the natural occurring brassinosteroid 6-desoxocastasterone (1) is described. The scheme consists in the formation and elimination of tigogenin mesylate followed by catalytic dihydroxylation of the resulting D2-steroid (3) and acetylation of the 2a, 3a-diol introduced.Treatment diacetate (5) with NaNO2/BF3.Et2O and chromatography in alumina led to a 23-keto (6) which on reduction produced the 23S alcohol (8) as major product. Saponification of the 2a, 3a-diacetoxy-23-keto compound (6) and the 2a,3a-diacetoxy-23-hydroxy compound (8) led to the spirobrasinosteroids (7) and (9).13C NMR and ¹H RMN characteristics derived from substitution at C23 are briefly discussed.

Study of the optical properties of TeO2-PbO-TiO2 glass system

We describe the preparation and some optical properties of high refractive index TeO2-PbO-TiO2 glass system. Highly homogeneous glasses were obtained by agitating the mixture during the melting process in an alumina crucible. The characterization was done by X-ray diffraction, Raman scattering, light absorption and linear refractive index measurements. The results show a change in the glass structure as the PbO content increases: the TeO4 trigonal bipyramids characteristics of TeO2 glasses transform into TeO3 trigonal pyramids. However, the measured refractive indices are almost independent of the glass composition. We show that third-order nonlinear optical susceptibilities calculated from the measured refractive indices using Lines' theoretical model are also independent of the glass composition.

Decomposição catalítica de óleo de soja em presença de diferentes zeólitas

The catalytic decomposition of soybean oil was studied in a fix bed reactor at 673 and 773 K and using amorphous silica-alumina and the zeolites USY, H-Mordenite and H-ZSM-5 as catalysts. Both the selectivity and the catalytic activity were determined by studying the product composition resulting from the chemical reactions. Physicochemical characteristics of the catalysts were obtained by X-ray fluorescence, Fourier Transform infrared spectroscopy, 29Si and 27Al Nuclear Magnetic Ressonance and textural analysis. The zeolites USY and H-ZSM-5, showing higher Brönsted acidity, yielded products with higher concentration in aromatic hydrocarbons, whereas with both H-Mordenite and amorphous silica-alumina the main products were paraffins.