Síntese, sinterização e caracterização de ferritas à base de Ni-Zn

Were synthesized different ferrites NixZn1-xFe2O4 (0,4 ≤ x ≤ 0,6) compositions by using citrate precursor method. Initially, the precursors citrates of iron, nickel and zinc were mixed and homogenized. The stoichiometric compositions were calcined at 350°C without atmosphere control and the calcined powders were pressed in pellets and toroids. The pressed material was sintered from 1100º up to 1200ºC in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, SEM and vibrating sample magnetometer (VSM). All sintered samples were characterized using XRD, SEM, VSM and measurements of magnetic permeability and loss factor were obtained. It was formed pure ferromagnetic phase at all used temperatures. The Rietveld analyses allowed to calculate the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (12-20 nm) to the calcined powder. By SEM, the sintered samples shows grains sizes from 1 to 10 μm. Sintered densities (ρ) were measured by the Archimedes method and with increasing Zn content, the bulk density decrease. The better magnetization results (105-110 emu/g) were obtained for x=0,6 at all sintering temperatures. The hysteresis shows characteristics of soft magnetic material. Two magnetization processes were considered, superparamagnetism at low temperature and the magnetic domains formation at high temperatures. The sintered toroids presents relative magnetic permeability (μr) from 7 to 32 and loss factor (tanδ) of about 1. The frequency response of toroids range from 0,3 kHz to 0,2 GHz. The composition x=0,5 presents both greater μr and tanδ values and x=0,6 the most broad range of frequency response. Various microstructural factors show influence on the behavior of μr and tanδ, such as: grain size, porosity across grain boundary and inside the grain, grain boundary content and domain walls movement during the process of magnetization at high frequency studies (0,3kKz 0,2 GHz)

Nanoparticles of octakis [3-(3-amino-1,2,4-triazole)propyl] octasilsesquioxane as ligands for Cu(II), Ni(II), Cd(II), Zn(II), and Fe(III) in aqueous solution

Nanoparticles of octakis[3-(3-amino-1,2,4-triazole)propyl]octasilsesquioxane (ATZ-SSQ) were tested as ligands, for transition-metal ions in aqueous solution with a special attention to sorption isotherms, ligand-metal interaction, and determination of metal ions in natural waters. The adsorption potential of the material ATZ-SSQ was compared with related [3(3-amino-1,2,4-triazole)propyl]silica gel (ATZ-SG). The adsorption was performed using a batchwise process and both organofunctionalized surfaces showed the ability to adsorb the metal ions from aqueous solution. The Langmuir model was used to simulate the sorption isotherms. The results suggest that the sorption of these metals on ATZ-SSQ and ATZ-SG occurs mainly by surface complexation. The equilibrium condition is reached at time lower than 3 min for ATZ-SSQ, while for ATZ-SG is only reached at time of 25 min. The maximum metal ion uptake values for ATZ-SSQ were higher than the corresponding values achieved with the ATZ-SG. In order to obtain more information on the ligand-metal interaction of the complexes on the surface of the ATZ-SSQ nanomaterial, ESR study with various degrees of copper loadings was carried out. The ATZ-SSQ was tested for the determination (in flow using a column technique) of the metal ions present in natural waters. (C) 2007 Elsevier B.V. All rights reserved.

Preparação de membranas de acetato de celulose organomodificadas para adsorção dos íons Cu(II), Cd(II), Mn(II) e Ni(II)

Cellulose acetate polymeric membranes had been prepared by a procedure of two steps, combining the method of phase inversion and the technique of hydrolysis-deposition. The first step was the preparation of the membrane, and together was organomodified with tetraethylortosilicate and 3-aminopropyltrietoxysilane. Parameters that exert influence in the complexation of the metallic ion, as pH, time of complexation, metal concentration, had been studied in laboratory using tests of metal removal. The membranes had presented resistance mechanics and reactivity to cations, being able to be an alternative for the removal, daily pay-concentration or in the study of the lability of metals complexed.

Comparison of the univariate and multivariate methods in the optimization of experimental conditions for determining Cu, Pb, Ni and Cd in biodiesel by GFAAS

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

Development of a method to determine Ni and Cd in biodiesel by graphite furnace atomic absorption spectrometry

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

Determinação de Ba, Cd, Cr, Cu, Ni, Pb, Sn e Zn em Tainha (Mugil brasiliensis) nos estuários potiguares

Heavy metals can cause problems of human poisoning by ingestion of contaminated food, and the environment, a negative impact on the aquatic fauna and flora. And for the presence of these metals have been used for aquatic animals biomonitoramento environment. This research was done in order to assess the environmental impact of industrial and domestic sewage dumped in estuaries potiguares, from measures of heavy metals in mullet. The methods used for these determinations are those in the literature for analysis of food and water. Collections were 20 samples of mullet in several municipality of the state of Rio Grande do Norte, from the estuaries potiguares. Were analyzed the content of humidity, ash and heavy metals. The data were subjected to two methods of exploratory analysis: analysis of the main components (PCA), which provided a multivariate interpretation, showing that the samples are grouped according to similarities in the levels of metals and analysis of hierarchical groupings (HCA), producing similar results. These tests have proved useful for the treatment of the data producing information that would hardly viewed directly in the matrix of data. The analysis of the results shows the high levels of metallic species in samples Mugil brasiliensis collected in Estuaries /Potengi, Piranhas/Açu, Guaraíra / Papeba / Arês and Curimataú

Estudo do desempenho de catalisadores tipo Ni/CexM1-xO2 (M = Zr ou Mn) na reação de oxidação parcial do metano

One of the main applications of methane is in the production of syngas, a mixture of hydrogen and carbon monoxide. Procedures used in this process are steam reforming, CO2 reforming, partial oxidation and autothermal reforming. The present study evaluated and compared the behavior of nickel catalysts supported on mixed oxides of cerium and manganese in the partial oxidation of methane with that of nickel catalysts supported on mixed oxides of cerium and zirconium. Mixed oxides of cerium and zirconium or cerium and manganese were synthesized using two different preparation methods, the polymeric precursor based on Pechini method and combustion reaction using a microwave. This was followed by impregnation with nickel content of 15 %. Samples were calcined at 300, 800 and 900 °C and characterized by specific surface area (SSA), X-ray fluorescence (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM), temperature programmed reduction (TPR) and the reaction of partial oxidation of methane. The specific areas of samples decrease with the rise in calcination temperature and after nickel impregnation. Metal-cerium solid solution was formed and the presence of other manganese species outside the solid solution structure was confirmed in the compound with the highest amounts of manganese oxides showed. With regard to scanning electron microscopy, supports based on cerium and zirconium prepared by Pechini method exhibited agglomerated particles without uniform geometry or visible pores on the surface. However, compounds containing manganese presented empty spaces in its structure. Through synthesis by combustion reaction, morphology acquired independently of the proposed composition demonstrated greater porosity in relation to Pechini synthesis. Although catalysts were prepared using different synthesis methods, the insertion of nickel showed very similar reduction profiles (TPR). In relation to nickel catalysts supported on mixed oxide of cerium and zirconium, there is an initial reduction of NiO species that present certain interaction with the support. This is followed by the reduction of Ce4+ in Ce3+ surface, with subsequent bulk reduction. For catalysts containing manganese, a reduction of nickel oxide species occurs, followed by two stages of reduction for species Mn2O3 in Mn3O4 and Mn3O4 in MnO, with subsequent reduction of bulk. With respect to partial oxidation reactions, the nickel catalyst supported on mixed oxide of cerium and zirconium, prepared using the Pechini method, exhibited CH4 conversion of approximately 80 %, with conversion of 81 % when prepared by combustion. This behavior continued for 10 hours of reaction. Manganese content was also found to directly influence catalytic activity of materials; the greater the manganese oxide content, the faster deactivation and destabilization occurred in the catalyst. In both synthesis methods, the nickel catalyst supported on mixed oxide of cerium and zirconium maintained an H2/CO ratio very close to 2 during the 10 hours of partial oxidation reaction. Samples containing manganese displayed smaller H2/CO ratios and lower performance in partial oxidation.

NI-GMRES precondicionado

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior

Shear bond strength of aesthetic materials bonded to Ni-Cr alloy

Objectives. This study was undertaken to evaluate the shear bond strength of four materials used as aesthetic material bonded to Ni-Cr alloy.Methods. Sixty-eight alloy discs were prepared and divided equally into four groups, and received four treatments for veneering: conventional feldspathic porcelain (Noritake EX-3) and three light-cured prosthodontic composite resins (Artglass, Solidex and Targis). The aesthetic materials were applied after metal structure conditioning in accordance with the manufacturers' recommendations. The specimens were stored in distilled water at 37 degreesC for 7 days. A universal testing machine was used to measure the shear bond strength of the specimens at a cross head speed of 0.5 mm/min. Fractured specimens were examined by using both optical and scanning electron microscope.Results. The analysis of variance and Tukey's test showed that the strongest mean shear bond was obtained with Noritake EX-3 (mean shear bond strength 42.90 +/- 7.82 MPa). For composites, the highest mean shear bond strength was observed for Targis (12.30 +/- 1.57 MPa); followed by Solidex (11.94 +/- 1.04 MPa) and Artglass (10.04 +/- 0.75 MPa). Optical analysis of the fractured surf aces indicated that for Targis and Noritake EX-3 all failures were a mixture of both cohesive and adhesive patterns. As for Artglass and Solidex, the fractures were mainly adhesive in nature.Conclusions. The Solidex system was equivalent to the Targis system in bond strength and exhibited greater strength than the Artglass system. The porcelain fused-to-metal showed considerably higher shear bond strength than the three metal-resin bonding techniques. (C) 2003 Elsevier B.V. Ltd. Ali rights reserved.

Adhesive Bonding of Resin Composite to Various Ni-Cr Alloy Surfaces Using Different Metal Conditioners and a Surface Modification System

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

Application of cellulose modified with p-aminobenzoic groups in preconcentration system for determination of Cu, Fe, Ni, and Zn in fuel ethanol samples by flame atomic absorption spectrometry

Cellulose chemically modified with p-aminobenzoic groups, abbreviated as Cel-PAB, was used for preconcentration of copper, iron, nickel, and zinc from ethanol fuel, normally used in Brazil as engine fuel. The surface characteristics and the surface area of the cellulose were obtained before and after chemical modification using FT-IR, elemental analysis, and surface area analysis (B.E.T.). The retention and recovery of the analyte elements were studied by applying batch and column techniques.

Determination of Cd(II), Cu(II) and Ni(II) in aqueous samples by ICP-OES after on-line preconcentration in column packed with silica modified with 2-aminothiazole

This work describes the synthesis and characterization of 2-aminothiazole modified silica gel (SiAT) and the studies of adsorption and pre-concentration (in batch and using a flow-injection system coupled with optical emission spectrometer) of Cd(II), Cu(II) and Ni(II) in aqueous medium. The adsorption capacity for each metal ions in mmolg(-1) was: Cu(II) = 1.18, Ni(II) = 1.15 and Cd(II) = 1.10. The results obtained in the flow experiments showed about 100% of recovering of the metal ions adsorbed in a mini-column packed with 100 mg of SiAT, using 100 mu L of 2.0 mol L-1 HCl solution as eluent. The quantitative sorption-desorption of the metal ions made possible the application of a flow-injection system in the pre-concentration and quantification by ICP-OES of metal ions at trace level in natural water samples.

Determination of Cu, Ni, and Zn in fuel ethanol by FAAS after enrichment in column packed with 2-aminothiazole-modified silica gel

This work describes the synthesis and characterization of 2-aminothiazole-modified silica gel (SiAT), as well as its application for preconcentration (in batch and column technique) of Cu(II), Ni(II) and Zn(II) in ethanol medium. The adsorption capacities of SiAT determined for each metal ion were (mmol g(-1)): Cu(II)=1.20, Ni(II)=1.10 and Zn(II)=0.90. In addition, results obtained in flow experiments, showed a recovery of ca. 100% of the metal ions adsorbed in a column packed with 500 mg of SiAT. The eluent was 2.0 mol L-1 HCl. The sorption-desorption of the studied metal ions made possible the development of a preconcentration method for metal ions at trace level in fuel ethanol using flame AAS for their quantification.