Electro-precipitation of Fe(3)O(4) nanoparticles in ethanol

The preparation of superparamagnetic magnetite (Fe(3)O(4)) nanoparticles by electro-precipitation in ethanol is proposed. Particle average size can be set from 4.4 to 9 nm with a standard deviation around 20%. Combination of wide-angle X-ray scattering (WAXS), Electron energy loss spectroscopy (EELS) and Mossbauer spectroscopy characterizations clearly identifies the particles as magnetite single-crystals (Fe(3)O(4)). (C) 2008 Elsevier B.V. All rights reserved.

Evaluation of different rhodium modifiers and coatings on the simultaneous determination of As, Bi, Pb, Sb, Se and of Co, Cr, Cu, Fe, Mn in milk by electrothermal atomic absorption spectrometry

Different kinds of modifiers and coatings on the integrated platform of transversely heated graphite atomizer (THGA) have been tested for the simultaneous determination of two group of elements: the first, the more volatile, formed by arsenic, bismuth, lead, antimony and selenium; the second, the less volatile, formed by cobalt, chromium, cupper, iron and manganese in milk by electrothermal atomic absorption spectrometry. Different Rh-modifiers were studied, such as Rh-coated platforms (Rh), carbide plus rhodium coated platforms (W-Rh, Zr-Rh), carbide-coated platforms (W and Zr) with co-injection of RhCl3, solutions and uncoated platforms with injection of solutions of Pd(NO3)(2), Mg(NO3)(2), and RhCl3. Milk samples were diluted 1:10 in 1.0% HNO3 and injected into the tube. The mass of modifier deposited and co-injected in the tube and the use of end capped tubes were also evaluated in order to improve the electrothermal behavior of analytes. Integrated platform pretreated with W plus co-injection RhCl3 for first group and pretreated with W-Rh for second group were elected. For 20 mu L injected samples the analytical curves in the 5.0-20.0 mu g L-1 concentration range have good linear correlation coefficients (r > 0.998). Relative standard deviations (n = 12) are < 6% and the calculated characteristic masses are between 5 pg and 62 pg.

Protective effect of safranine on the mitochondrial damage induced by Fe(II)citrate: Comparative study with trifluoperazine

In this study, we show that safranine at the concentrations usually employed as a probe of mitochondrial membrane potential significantly protects against the oxidative damage of mitochondria induced by Fe(II)citrate. The effect of safranine was illustrated by experiments showing that this dye strongly inhibits both production of thiobarbituric acid-reactive substances and membrane potential decrease when energized mitochondria were exposed to Fe(II)citrate in the presence of Ca 2+ ions. Similar results were obtained with the lipophylic compound trifluoperazine. It is proposed that, like trifluoperazine, safranine decreases the rate of lipid peroxidation due to its insertion in the membrane altering the physical state of the lipid phase.

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.

Estudo da dissolução oxidativa microbiológica de uma complexa amostra mineral contendo pirita (FeS2), pirrotita (Fe 1-XS) e molibdenita (MoS2)

This work aims to study the oxidation of a complex molybdenite mineral which contains pyrite and pyrrotite, by Acidithiobacillus ferrooxidans. This study was performed by respirometric essays and bioleaching in shake flasks. Respirometric essays yielded the kinetics of mineral oxidation. The findings showed that sulfide oxidation followed classical Michaelis-Menten kinetics. Bioleaching in shake flasks allowed evaluation of chemical and mineralogical changes resulting from sulfide oxidation. The results demonstrated that pyrrotite and pyrite were completely oxidized in A. ferrooxidans cultures whereas molybdenite was not consumed. These data indicated that molybdenite was the most recalcitrant sulfide in the sample.

Influence of voids in the hybrid layer based on self-etching adhesive systems: a 3-D FE analysis

The presence of porosities at the dentin/adhesive interface has been observed with the use of new generation dentin bonding systems. These porosities tend to contradict the concept that etching and hybridization processes occur equally and simultaneously. Therefore, the aim of this study was to evaluate the micromechanical behavior of the hybrid layer (HL) with voids based on a self-etching adhesive system using 3-D finite element (FE) analysis. Three FE models (Mr) were built: Mr, dentin specimen (41x41x82 μm) with a regular and perfect (i.e. pore-free) HL based on a self-etching adhesive system, restored with composite resin; Mp, similar to M, but containing 25% (v/v) voids in the HL; Mpp, similar to Mr, but containing 50% (v/v) voids in the HL. A tensile load (0.03N) was applied on top of the composite resin. The stress field was obtained by using Ansys Workbench 10.0. The nodes of the base of the specimen were constrained in the x, y and z axes. The maximum principal stress (σmax) was obtained for all structures at the dentin/adhesive interface. The Mpp showed the highest peak of σmax in the HL (32.2 MPa), followed by Mp (30 MPa) and Mr (28.4 MPa). The stress concentration in the peritubular dentin was high in all models (120 MPa). All other structures positioned far from voids showed similar increase of stress. Voids incorporated into the HL raised the σmax in this region by 13.5%. This behavior might be responsible for lower bond strengths of self-etching and single-bottle adhesives, as reported in the literature.

A simple method based on HR-CS FAAS for multi-element determination of Cu, Fe, Mn and Zn in medicinal plants

A simple method to determine Cu, Fe, Mn and Zn in single aliquots of medicinal plants by HR-CS FAAS is proposed. The main lines for Cu, Mn and Zn, and the alternate line measured at the wing of the main line for Fe at 248.327 nm allowed calibration within the 0.025 - 2.0 mg L-1 Cu, 1.0 - 20.0 mg L-1 Fe, 0.05 - 2.0 mg L-1 Mn, 0.025 - 0.75 mg L-1 Zn ranges. Nineteen medicinal plants and two certified plant reference materials were analyzed. Results were in agreement at a 95% confidence level (paired t-test) with reference values. Limits of detection were 0.12 μg L-1 Cu, 330 μg L-1 Fe, 1.42 μg L-1 Mn and 8.12 μg L-1 Zn. Relative standard deviations (n=12) were ≤ 3% for all analytes. Recoveries in the 89 - 105% (Cu), 95 - 108% (Fe), 94 - 107% (Mn), and 93 - 110% (Zn) ranges were obtained.

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.

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.

Role of Ca, Fe, Cu and Zn in breast cancer: Study by X-ray fluorescence techniques and immunohistochemical analysis

In recent years, several studies have shown that concentrations of trace elements are altered in neoplastic breast tissues. However, the microenvironment and metabolic changes caused by tumors are complex and still not completely understood. Under this aspect, the combination of different techniques to investigate the role of trace elements in promoting and/or maintaining a tumor is interesting once the combination of information obtained by analytical techniques and immunohistochemical assays, associated with clinicopathological data, may allow a better metabolic understanding of trace elements in breast cancer. In this work, the role of the trace elements Ca, Fe, Cu and Zn in neoplastic breast tissues was investigated by X-ray fluorescence (XRF) techniques and immunohistochemical assays. We determined concentrations of Ca, Fe, Cu and Zn in normal and neoplastic breast tissues using energy dispersive XRF, and these values were used to set the positive or negative expression of elements in normal and neoplastic tissues. These expressions were correlated with the spatial distributions of trace elements (evaluated by micro-XRF) and with immunoexpression of matrix metalloproteinases (MMPs), tissue inhibitors of MMPs and vascular endothelial growth factor. The results revealed that the expression of the trace elements Fe, Cu and vascular endothelial growth factor are related, indicating that higher levels of these elements can be associated with the angiogenic process in breast cancer. Also, associations between Ca, Zn and MMPs expression have been observed, possibly because of the fact that both metals are present in these proteins. © 2013 John Wiley & Sons, Ltd.

Efeito da adição de nanopartículas na biolixiviação da calcopirita ('CU''FE''S IND.2') por Acidithiobacillus ferrooxidans LR

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Biossolubilização da calcopirita ('CU'FE'S IND. 2') na presença de íons cloreto

Pós-graduação em Biotecnologia - IQ

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)