Determinação direta de crômio em açúcar e leite por espectrometria de absorção atômica com atomização eletrotérmica em forno de grafite

A fast and direct method for the determination of Cr in milk and cane sugar suspensions using graphite furnace atomic absorption spectrometry with Zeeman-effect background correction is described. No sample pre-treatment was necessary, minimizing the risk of contamination. The concentration of chromium in cane sugar was evaluated using Cr reference solutions prepared in 1% v/v HNO3 solution. The milk samples were introduced into the furnace with a mixture of amines for avoiding the autosampler blockage and foaming of milk. Chromium determination in milk was based on the standard additions method (SAM). The limit of detection and characteristic mass for cane sugar sample (30 muL) were 0,13 ng/ml and 4,3 pg, and for milk sample (10 muL) were 0,23 ng/ml and 7,8 pg, respectively. The graphite tube lifetime was 300 firings for sugar-cane sample and 100 firings for milk sample. The heating program was implemented in 68 s.

Biocerâmicas: tendências e perspectivas de uma área interdisciplinar

The need for new materials to substitute injured or damaged parts of the human body has led scientists of different areas to the investigation of bioceramics since the 70's, when other materials in use started to show implantation problems. Bioceramics show some advantages like being the material that best mimics the bone tissue but also, present low mechanical strength due to its ceramic nature. This paper presents a general view about the topic.

Análise por difração de raios x de filmes de óxidos cerâmicos compostos por IrO2/TiO2/CeO2

Independent of the sample form (powder or film), XRD analysis of Ir0,3Ti(0,7-x)Ce xO2, (nominal) mixtures, for x=0, shows the formation of a solid solution phase between IrO2 and TiO2, as well as the rutile phases of IrO2 and TiO2. The presence of the anatase phase of TiO2 is also confirmed. The introduction of 30 mol% CeO2 in the mixture reveals the presence of the CeO2 and Ce2O3 phases, besides the already mentioned ones, in the powder. In the film form, however, an amorphous phase is identified. When all of the TiO2 is substituded by CeO2, for both sample forms, the only phases found are IrO2, CeO2 and Ce2O3. This result suggests cerium oxides are not capable of forming solid solutions with either IrO2 or (Ir,Ti)O2 acting solely as a dispersant matrix for these phases. These results are consistent with the much higher electrochemically active surface area when CeO2 is introduced in the binary Ti/Ir0,3Ti0,7O2 mixture. It was possible to establish a relationship between the electrochemical stability of the supported films and their crystalline structure. The unexpected presence of TiO2 and Ti2O3 in the Ti/Ir0,3Ce0,7O2 (film sample) is attributed to oxidation of the Ti support during the calcination step.

Reação de geração de oxigênio em eletrodos de Mn2O3 suportados em aço inoxidável

A study of the kinetics of oxygen evolution in alkaline conditions from ceramic films of Mn2O3 supported on stainless steel was carried out. This study has been done through the determination of transfer coefficients, Tafel slopes and exchange currents using potentiodynamic and quasi-potentiostatic measurements. The activation energy was determined as a function of the overpotential and, additionally, the electrode active surface was estimated. The results are consistent with data already published for other electrodes, implying that the methods used in this work were reliable and precise.

Interações entre corantes e argilas em suspensão aquosa

Adsorption of cationic dyes on clays can be used as a model for the interactions between organic compounds and these minerals. Cationic dyes like methylene blue are used to study these interactions because of the spectroscopic changes observed when their molecules are adsorbed on clay surfaces. Depending on the structure and layer charge of the clay particles several processes may occur, like adsorption of dye monomers and aggregates on the external and internal surfaces of the clay tactoids, migration towards internal surfaces, protonation, etc. Under certain conditions the deaggregation-aggregation of the clay particles are accelerated trapping dye species during these processes. A general scheme is proposed for the processes occurring between clays and dyes in aqueous suspensions, which can be used to explain the behaviour of specific systems.

Preparação e caracterização de pós cerâmicos de aluminatos de lítio

The preparation of gamma-LiAlO2 by coprecipitation and sol-gel synthesis was investigated. Ceramic powders obtained by coprecipitation synthesis were prepared from aqueous solutions of aluminum and lithium nitrates using sodium hydroxide as precipitant agent. By sol-gel synthesis, the ceramic powders were prepared from hydrolysis of aluminum isopropoxide. The materials obtained by two routes of synthesis were dried at 80ºC and calcined at 550, 750, 950 and 1150ºC. The characterization was done by X-ray diffraction, infrared spectroscopy, emission and absorption atomic spectrometry, helium picnometry, specific surface area (BET method) and scanning electronic microscopy. Mixtures of crystalline phases were obtained by coprecipitation synthesis: 80ºC- LiAl2(OH)7.2H2O + Al(OH)3; 550 and 750ºC- alpha-LiAlO2 + eta-Al2O3; 950 and 1150ºC- gamma-LiAlO2 + LiAl5O8. Chemical analysis showed molar ration Al/Li @ 3. Crystalline single-phases were obtained by sol-gel synthesis above 550ºC: 550ºC-alpha-LiAlO2; 750, 950 and 1150ºC-gamma-LiAlO2. These powders presented molar ration Al/Li @ 1. Thus, gamma-LiAlO2 crystalline phase was obtained at 750ºC by sol-gel synthesis while by coprecipitation synthesis, a mixture of crystalline phases was obtained. These results showed the superiority of the sol-gel synthesis for the preparation of pure gamma-LiAlO2.

Caracterização de cinza de casca de arroz para uso como matéria-prima na fabricação de refratários de sílica

The characterization of rice husk ash, a deriving by-product of the burning of the rice husk during the rice processing is the object of this study. This by-product, for being rich in silica, can be an important raw material for the production of siliceous ceramics, such as thermal insulators and refractory. A combination of surface analysis, thermal analysis and microscopy analysis techniques was used for the characterization. The characterized by-product presented as main component the silica, under amorphous form, with a maximum content of alkalis around 1%, features that become it potentially interesting for the production of ceramic materials.

Resistência química de vitro-cerâmicos pertencentes a sistemas Li2O-ZrO2-BaO-SiO2 frente ao tratamento com soluções ácidas e básicas

The chemical durability of the Li2O-ZrO2-BaO-SiO2 system was examined by determination of the Vickers hardness. The dependence of hardness and of the chemical resistance with BaO addition was investigated. The experimental results indicate that the hardness increases with the BaO content. The samples surface's morphology submitted to the chemical treatment in acidic (H2SO4) and basic (KOH) solution was accompanied by scanning electron microscopy. The chemical durability of the materials with BaO showed better than the glass ceramic without this content. These materials treated with H2SO4 solution showed a preferential attack to the silica rich sites.

Células a combustível de baixa potência para aplicações estacionárias

A paradigmatic shift in developing fuel cell for stationary applications has been occurring in the last ten years. Previously, 100 kW class to a few MW class power plants were preferred but recently, the development has drifted towards units of only a few kW. The motivation is the present market situation, which favors disperse residential electric power generation from natural or liquefied gas. Membrane-type fuel cells are very promising for this application, due to their present state of development in the automobile industry. More recently, small ceramic fuel cells (SOFC) has also been found to be adequate for this application. Considering a family of 4 members, 1 kW (electric) units seem to be optimal for individual residences. This presentation discusses briefly the Brazilian scenario with respect to these units.

Nano vitrocerâmica de escória de aciaria

The manufacture of glass-ceramics is an alternative route for the commercial use of metallurgical slags. Such types of glass-ceramics may find commercial applications owing to their low cost, good mechanical properties and superior visual aspect. Besides, due to the elimination of that industrial residue from the environment and also due to the possibility of replacement of natural stones such as marbles and granites, the use of slags is an activity with strong ecological appeal. While the use of blast-furnace slags for the production of glass-ceramics is well known, the utilization of steel making slags constitutes a challenge, because these materials possess low concentration of SiO2. In this work a novel composition for producing glasses and glass-ceramics from a steelmaking slag is presented. The crystal nucleation kinetics, the characterization of the resulting microstructures for two different thermal treatments and mechanical properties of the glass-ceramics are discussed. A glass-ceramic having a marble aspect, fine volumetric crystallization, high degree of crystallization and improved mechanical strength was obtained.

Estudo do efeito da quantidade de óxido de ferro em cinzas pesadas de carvão mineral na obtenção de vitrocerâmicos

Bottom ash has been used as raw material to glass and glass ceramic production because it is a source of SiO2 and Al2O3. However, the high concentration of iron (about 10% wt.) difficulty the control of the nucleation and the crystallization processes. The iron content was reduced by magnetic process, where the magnetite phase was mainly removed. In order to compare glass ceramics obtained from original and low iron bottom ashes, microstructural and dilatometric characterizations were performed.

Síntese, caracterização e estudo das propriedades catalíticas e magnéticas de nanopartículas de Ni dispersas em matriz mesoporosa de SiO2

Nickel nanoparticles supported on amorphous silica ceramic matrix were synthesized by the polymeric precursor method. The nanostructure was characterized by NMR, BET, XRD, SEM, TEM, and flame atomic absorption spectrometry techniques. It was observed a dependence of the crystallite size on the thermal annealing, under a N2 atmosphere. The materials presented a high catalytic activity and selectivity upon the beta-pinene hydrogenation reaction. The magnetic hystereses were also correlated with the morphology of the processed material.

Dimensão fractal de ácidos húmicos em diferentes condições experimentais

The determination of fractal dimension (D) of humic particles was achieved by the turbidimetric technique where diluted suspensions of humic acids, in different experimental conditions, were analyzed by spectrophotometry UV-Vis. The slope of the lines (beta) was taken from the graphics (logtauvs loglambda) to obtain D. The results show that the values of D changed according to pH (3.0, 5.0 and 7.0), temperature (25 and 5 ºC) and shaking (magnetic and horizontal). In general, the value of D decreased with the increment of pH, increase of shaking and decrease of temperature.

Caracterização e estabilidade físico-química de sistemas poliméricos nanoparticulados para administração de fármacos

Polymeric nanoparticle systems such as nanocapsules and nanospheres present potential applications for the administration of therapeutic molecules. The physico-chemical characteristics of nanoparticle suspensions are important pre-requisites of the success of any dosage form development. The purpose of this review is to present the state of the art regarding the physico-chemical characterization of these drug carriers, in terms of the particle size distribution, the morphology, the polymer molecular weight, the surface charge, the drug content and the in vitro drug release profiles. Part of the review is devoted to the description of the techniques to improve the stability of colloidal systems.

Desenvolvimento de um dispositivo para obtenção de monocristais de ligas à base de cobre

This paper describes the drawing, construction and optimization of a device, which can be used to obtain single crystals of different metallic materials with melting point from 550 to 1050 ºC. Components of ease obtaining and of low cost were used. The device was based on the modified Bridgman technique and it was used to obtain single crystals of copper-based alloys. The temperature axial profiles and a difference less then 1% in the temperature between the wall and the center of the ceramic tube in the critical region for obtaining single crystals of good quality indicated that the oven presents a good thermal stability. Single crystals of CuZnAl and CuAlAg alloys of good quality were growth and characterized using optical microscopy and Laüe X-ray back reflection.