Microwave Hydrothermal Synthesis and Photocatalytic Performance of ZnO and M:ZnO Nanostructures (M = V, Fe, Co)

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Expression, purification and spectroscopic analysis of an HdrC: An iron-sulfur cluster-containing protein from Acidithiobacillus ferrooxidans

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

A thermal analysis study of some transition-metal dithizonates

Solid dithizonates of Fe(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Pb(II), have been prepared. Thermogravimetry (TG), derivative thermogravimetry (DTG), differential scanning calorimetry (DSC), X-ray diffraction powder patterns and elemental analysis have been used to characterize and study the thermal stability and thermal decomposition of these compounds.

Electrodeposition of amorphous Fe-Cr-P-Ni-C alloys. Morphological and structural characteristics

The effect of bath composition and electroplating conditions on structure, morphology and composition of amorphous Fe-Cr-P-Ni-C deposits on Cu substrate was investigated. The deposition efficiency of Fe-Ni-P-C alloy increased significantly with the addition of formic acid, but decreased with the addition of Cr to the plating bath. The increase of charge density activates the inclusion of Cr in the deposit. However, above a specific value of charge density, which depends on deposition current density, the Cr content in the deposit decreases. SEM analysis showed that the increase of Ni, Cr or charge deposition promotes susceptibility to microcracking.

Evaluation of the combined solar TiO2/photo-Fenton process using multivariate analysis

The effect of combining the photocatalytic processes using TiO 2 and the photo-Fenton reaction with Fe3+ or ferrioxalate as a source of Fe2+ was investigated in the degradation of 4-chlorophenol (4CP) and dichloroacetic acid (DCA) using solar irradiation. Multivariate analysis was used to evaluate the role of three variables: iron, H2O2 and TiO2 concentrations. The results show that TiO2 plays a minor role when compared to iron and H2O2 in the solar degradation of 4CP and DCA in the studied conditions. However, its presence can improve TOC removal when H2O2 is totally consumed. Iron and peroxide play major roles, especially when Fe(NO3)3 used in the degradation of 4CP. No significant synergistic effect was observed by the addition of TiO 2 in this process. On the other hand, synergistic effects were observed between FeOx and TiO2 and between H 2O2 and TiO2 in the degradation of DCA. © IWA Publishing 2004.

Comparative studies of the sample decomposition of green and roasted coffee for determination of nutrients and data exploratory analysis

The contents of some nutrients in 35 Brazilian green and roasted coffee samples were determined by flame atomic absorption spectrometry (Ca, Mg, Fe, Cu, Mn, and Zn), flame atomic emission photometry (Na and K) and Kjeldahl (N) after preparing the samples by wet digestion procedures using i) a digester heating block and ii) a conventional microwave oven system with pressure and temperature control. The accuracy of the procedures was checked using three standard reference materials (National Institute of Standards and Technology, SRM 1573a Tomato Leaves, SRM 1547 Peach Leaves, SRM 1570a Trace Elements in Spinach). Analysis of data after application of t-test showed that results obtained by microwave-assisted digestion were more accurate than those obtained by block digester at 95% confidence level. Additionally to better accuracy, other favorable characteristics found were lower analytical blanks, lower reagent consumption, and shorter digestion time. Exploratory analysis of results using Principal Component Analysis (PCA) and Hierarchical Cluster Analysis (HCA) showed that Na, K, Ca, Cu, Mg, and Fe were the principal elements to discriminate between green and roasted coffee samples. ©2007 Sociedade Brasileira de Química.

Voltammetric determination of ethyl acetate in ethanol fuel using a Fe 3+/Nafion®-coated glassy carbon electrode

A voltammetric method for the determination of ethyl acetate in ethanol fuel using a Fe3+/Nafion®-coated glassy carbon electrode (GCE) is proposed. The ethyl acetate present in the ethanol fuel was previously converted to acetohydroxamic acid via pretreatment with hydroxylamine chloride. The acetohydroxamic acid promptly reacted with the iron (III) present in the film, producing iron (III) acetohydroxamate, which presents a well-defined voltammetric peak current at -0.02 V. Optimization of the voltammetric parameters for the cyclic, linear sweep, square wave, and differential pulse modalities was carried out for this chemically-modified electrode. Square wave voltammetry afforded the best response for acetohydroxamic acid detection. The analytical curve for this species was linear from 9 to 100 μmol L 1 according to the following equation: ip (μA) = 0.27 + 2.55Cacetohydroxamic acid (μmol L 1), with linear correlation coefficient equal to 0.993. The technique presented limit of detection equal to 5.3 μmol L 1 and quantification limit of 17.6 μmol L 1. The proposed method was compared to the official method of ethyl acetate analysis (Gas Chromatography), and a satisfactory correlation was found between these techniques. © 2012 Elsevier Ltd. All rights reserved.

An anisotropic linear elastic boundary element formulation for masonry wall analysis

This work presents an application of a Boundary Element Method (BEM) formulation for anisotropic body analysis using isotropic fundamental solution. The anisotropy is considered by expressing a residual elastic tensor as the difference of the anisotropic and isotropic elastic tensors. Internal variables and cell discretization of the domain are considered. Masonry is a composite material consisting of bricks (masonry units), mortar and the bond between them and it is necessary to take account of anisotropy in this type of structure. The paper presents the formulation, the elastic tensor of the anisotropic medium properties and the algebraic procedure. Two examples are shown to validate the formulation and good agreement was obtained when comparing analytical and numerical results. Two further examples in which masonry walls were simulated, are used to demonstrate that the presented formulation shows close agreement between BE numerical results and different Finite Element (FE) models. © 2012 Elsevier Ltd.

Fe K-edge X-ray absorption spectroscopy study of Pb(Fe2/3W 1/3)O3-PbTiO3 multiferroic ceramics

The present paper is a comprehensive study concerning Fe K-edge X-ray absorption spectroscopy (XAS) measurements, which were performed to characterize the local structure of (1 - x)Pb(Fe2/3W1/3)O 3-xPbTiO3 samples as a function of temperature and PbTiO3 content. Results obtained by the fits of extended X-ray absorption fine structure consist with rhombohedral symmetry for Pb(Fe 2/3W1/3)O3 composition at temperatures lower than room temperature. This result is in apparent disagreement with X-ray and neutron diffraction characterization which have been reported. This apparent disagreement is related to the fact that XAS probes the short-range order, whereas X-ray diffraction provides structural information about the average structure. Moreover, as the PbTiO3 content increases, a disorder has been detected at local structure of the FeO6 octahedron. Analysis of X-ray absorption near edge structure spectra did not show modifications in intensity nor energy of transitions. © 2013 American Institute of Physics.

Concentrations of Cu, Fe, Mn, and Zn in tropical soils amended with sewage sludge and composted sewage sludge

Sewage sludge may be used as an agricultural fertilizer, but the practice has been criticized because sludge may contain trace elements and pathogens. The aim of this study was to compare the effectiveness of total and pseudototal extractants of Cu, Fe, Mn, and Zn, and to compare the results with the bioavailable concentrations of these elements to maize and sugarcane in a soil that was amended with sewage sludge for 13 consecutive years and in a separate soil that was amended a single time with sewage sludge and composted sewage sludge. The 13-year amendment experiment involved 3 rates of sludge (5, 10, and 20 t ha-1). The one-time amendment experiment involved treatments reflecting 50, 100, and 200 % of values stipulated by current legislation. The metal concentrations extracted by aqua regia (AR) were more similar to those obtained by Environmental Protection Agency (EPA) 3052 than to those obtained by EPA3051, and the strongest correlation was observed between pseudo(total) concentrations extracted by AR and EPA3052 and bioavailable concentrations obtained by Mehlich III. An effect of sewage sludge amendment on the concentrations of heavy metals was only observed in samples from the 13-year experiment. © 2012 Springer Science+Business Media B.V.

Testing extractants for Cu, Fe, Mn, and Zn in tropical soils treated with sewage sludge for 13 consecutive years

In this paper, we report on a field experiment being carried out in a Typic Eutrorthox. The experiment was initiated in the 1997-98 agricultural season as a randomized block design with four treatments (0, 5, 10, and 20 t ha -1) of sewage sludge and five replicates. Compound soil samples were obtained from 20 subsamples collected at depths of 0-0.1 and 0.1-0.2 m. Cu, Fe, Mn, and Zn concentrations were extracted with DTPA pH 7.3; 0.1 mol L -1 HCl, Mehlich-I, Mehlich-III, and 0.01 mol L-1 CaCl 2. Metal concentrations were determined via atomic absorption spectrometry. Diagnostic leaves and the whole above-ground portion of plants were collected to determine Cu, Fe, Mn, and Zn concentrations extracted by nitric-perchloric digestion and later determined via atomic absorption spectrometry. Sewage sludge application caused increases in the concentrations of soil Cu, Fe, and Mn in samples taken from the 0-0.1 m depth evaluated by the extractants Mehlich-I, Mehlich-III, 0.01 mol L-1 HCl and DTPA pH 7.3. None of the extractants provided efficient estimates of changes in Mn concentrations. The acid extractants extracted more Cu, Fe, Mn, and Zn than the saline and chelating solutions. The highest concentrations of Cu, Fe, and Zn were obtained with Mehlich-III, while the highest concentrations of Mn were obtained with HCl. We did not observe a correlation between the extractants and the concentrations of elements in the diagnostic leaves nor in the tissues of the whole maize plant (Zea mays L.). © 2013 Springer Science+Business Media Dordrecht.

Síntese e caracterização de cátodos de perovskitas 'La IND.0,6''Sr IND.0,4''Fe IND.y''Co IND.1-y''O IND.3-'delta'', para células a combustível de eletrólito sólido (SOFC) operando em temperaturas intermediárias

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Thermal decomposition and stability in a series of heterobimetallic carbonyl compounds of the type [Fe(CO)4(HgX)2] (X=Cl, Br, I)

Foram preparados compostos carbonílicos heterobimetálicos do tipo [Fe(CO)₄(HgX)₂] ( X= Cl, Br, I), contendo ligação metal-metal, objetivando investigar suas estabilidades térmicas em função do halogênio coordenado aos átomos de mercúrio. A caracterização destes complexos foi feita usando-se de técnicas espectroscópicas de infravermelho e ressonância magnética nuclear, além de análise elementar. O produto final das termodecomposições foi identificado através de espectroscopia no infravermelho e difratograma de raios-X, método de pó.

Análise da influência dos solutos Zr e Ti sobre as propriedades mecânica, elétrica e de termorresistência de uma liga Al-Cu-Fe-Si destinada a Tx e a Dx de energia elétrica

O contexto energético mundial apresenta um aumento constante do consumo de energia elétrica no último século, desta forma exigindo a pesquisa de novos materiais para a aplicação em cabos e fios condutores de eletricidade. A partir destas demandas por novos materiais, desenvolveu-se uma análise da influência dos solutos zircônio e titânio na modificação de características importantes de uma liga Al-Cu-Fe-Si, destinada a ser o meio condutor de energia elétrica, almejando obter propriedades termorresistentes. Para a realização deste estudo, as ligas foram obtidas por fundição direta em lingoteira metálica em formato “U”, a partir do Al-EC, fixando-se na liga-base os teores de 0,05% Cu, [0,24 a 0,28]% Fe e 0,7% de Si, e em seguida, inserindo-se os teores de 0,26% Zr e 0,26% Ti. O experimento foi dividido em duas etapas, ETAPA A e ETAPA B, respectivamente, com o intuito de se avaliar as características mecânicas, elétricas e estruturais das ligas. Os corpos de prova após laminação a frio (nos diâmetros 2,7; 3,0; 3,8 e 4,0 mm) foram analisados sem tratamento térmico (STT) e com tratamento térmico (CTT): 230 ºC por uma hora, de acordo com o protocolo COPEL, 310 ºC e 390 ºC por uma hora, visando avaliar a ermorresistência em temperaturas mais elevadas, a estabilidade térmica e analisar as microestruturas desenvolvidas em tais tratamentos térmicos (TT). Verificou-se que o Ti tem maior capacidade de refinar o grão em relação ao Zr, que apresenta grãos menos refinados, porém com melhores propriedades físicas e apresentando-se termorresistente.

Efeito de adições de Ni e Mg sobre o comportamento térmico, mecânico e elétrico de ligas Al-Cu-Fe solidificadas unidirecionalmente

Este trabalho estudou a influência dos teores dos solutos Mg e Ni na modificação das propriedades térmicas, elétricas e mecânicas de uma liga Al-Cu-Fe para aplicação como condutor de energia elétrica. Para a realização do presente estudo, as ligas foram obtidas por fundição unidirecional horizontal, a partir da base do alumínio de pureza comercial com adição dos teores 0,05%p Cu e [0,24 a 0,28]%p Fe. Tal base foi modificada em uma primeira etapa com teores de 0,45, 0,60 e 0,80%p Mg. As ligas obtidas com estes teores tiveram suas propriedades estudadas para que se selecionasse um teor de Mg para posterior adição de Ni à liga. O estudo destas propriedades na primeira etapa passou pela análise das propriedades térmicas: velocidade de solidificação (V_L) e taxa de resfriamento (Ṫ). A caracterização elétrica estudou a propriedade condutividade elétrica (φ) e o levantamento das propriedades mecânicas: limite de resistência à tração (σ) e microdureza Vickers (HV). A liga com adição de Ni passou por tratamentos térmicos de envelhecimento, por 1, 4 e 8h. Estas amostras foram analisadas em um microscópio eletrônico de varredura - MEV pelos sinais de elétrons retroespalhados – ERE e espectroscopia de energia dispersiva – EDS. Como resultados do estudo, encontrou-se que adições de Mg influenciaram significativamente a viscosidade das ligas, elevando as velocidades de solidificação nos instantes finais. Os ensaios de microdureza das amostras envelhecidas mostraram que houve um acréscimo significativo de dureza na quarta hora de envelhecimento, da mesma forma que as análises de EDS mostraram que a concentração de Ni também elevou-se nesta condição de tratamento.