Preparo de filmes-suporte para microscópio eletrônico

Working with low voltage microscope (R.C.A., EMC-2, of 30KV.) the authors verified that parlodion and Formvar films are quickly destroyed by intense heating under the electron beam. They have tried to employ oxide films, as Al2O3 and SiO, more resistant to heat. Al2O3 films are prepared by anodic oxidation of thin aluminium sheets, under 8 to 10 volts in a 3% ammonium citrate solution and subsequent aluminium dissolution in a O.25% HgCl2 solution. These films are very suitable when prepared with highly pure aluminium of extremely homogeneous surface. Best results were obtained with SiO films, evaporated in high vacuum over Parlodion films mounted on metallic grids. Employing 1 or 1.5 mg of SiOm highly homogeneous and resistant films are obtained, having little inferior transparence than the Parlodion ones. Pure SiO films (1.5 mg) are obtained by elimination of the Parlodion under slow heating until 250°C; they are greatly transparent but little resistant to water, thus beeing indicated in dry preparations. For particles which deposite in a chain-like form around thin fibers, the authors employ the mounting on Parlodion fibers, obtained by heating Parlodion films on microscope grids about 190°C.

Age-related worm load and worm fecundity patterns in human populations, as indicated by schistosome circulating antigens

Recently, our group determined the relationship between serum CAA levels and fecal egg counts in two foci with very intense Schistosoma mansoni transmission: Maniema (Zaire), an area endemic for S. mansoni since several decades, and Ndombo (Senegal), where transmission has only been established since a few years. The objective was to study and compare age-related worm load and worm fecundity patterns in these two different endemic settings. Here, we will summarize the most important findings and conclusions of this study.

Análise potenciométrica de redissolução com ultramicroeletrodos: fundamentos e aplicações na determinação de metais traços

The Potentiometric Stripping Analysis (PSA) is described with emphasis on ultramicroelectrode applications with a laboratory developed computer based instrumentation. The technique potentialities as compared with the voltammetric approach are pointed out based on the current literature. Some results of trace metals analysis including zinc, cadmium, lead and copper in vinegar and canned food samples are presented. The mainly advantage found in our laboratory was the technique capability to analyse natural samples with minimum matrix interference and the low level of noise found in our determinations.

Alteração do comportamento eletroquímico do eletrodo de níquel, em ácido sulfúrico diluído, sob diferentes condições de iluminação

In this paper is presented electrochemical evidences of the influence of the light on the electrochemical behavior of nickel electrode in diluted sulfuric acid. The current densities related with the electrooxidation of the metal decreases when the electrode is under illumination. The corrosion potential, Ecorr , shift to a more positive value in this condition. This effect was observed with polychromatic light and with different wavelength glass filters such as 700 nm and 520 nm. It was observed that increasing the temperature of the solution, the current densities related with cathodic and anodic processes, increases instead of decreases. The activation energy related with the electrooxidation of the electrode was higher under illumination than in the dark. It is suggested that this behavior may be related or with a photo-inhibition effect either with dessorption of adsorbed water involved in the electrooxidation mechanism.

Desenvolvimento e caracterização de recobrimentos de Ni-Co e de seus óxidos mistos para a produção de oxigênio por eletrólise alcalina da água

This paper describes the development and characterisation of Ni-Co coatings to be used as anodes in water electrolysis. Chemical oxidation of the surface was performed through thermal treatment at 400ºC for 10 h. The resulting surfaces were analysed by X-ray diffraction, EDX, SEM, cyclic voltammetry and constant current electrolysis. The electrochemical oxidation occurring on bare surfaces during electrolysis promotes the formation of thick oxide layers resulting in loss of activity. In oxidised surfaces the chemical Ni-Co oxide grown during the thermal treatment prevents further oxidation thus retaining their activity towards oxygen evolution. An optimum condition for the growth of mixed oxide with high activity was found for the bath containing 50 g L-1 CoSO4.

Filmes de óxidos anódicos de nióbio: efeito eletrocrômico e cinética da reação de eletro-intercalação

The aim of this work is to study the electrochromism and the reaction kinetics of lithium electrointercalation in anodic niobium oxide films. The oxide grown in an acid environment by application of an alternating potential shows interference colour (iridescence) and when reduced in lithium perclorate/PC solution, the intercalation of Li+ ions and electrons causes a reversible colour change (electrochromism), characterized here by electrochemical and optical measurements. A model where the reaction kinetics is dominated by diffusion of ionic pairs (Li+, e-) in the oxide film permitted the reproduction of current and absorbance temporal dependence, confirming the relationship between the electrochromic and electrochemical reactions. From the results obtained, a relation was established where the colour change is associated to the reduction of Nb+5 to Nb+4 ions with simultaneous cations injection.

Caracterização de filmes finos de Nb2O5 com propriedades eletrocrômicas

The sols for thin electrochromic coatings of Nb2O5 were obtained by synthesis of the niobium butoxide from BuONa and NbCl5. The ~300nm thick films were deposited by dip-coating technique from the alkoxide solution and calcined at 560ºC in O2 atmosphere during 3 hours. The particles size of niobium oxide (V) powder (~20mm) was obtained from x-ray diffraction using the Scherrer equation. The coatings were characterized by cyclic voltammetry and cronoamperommetry techniques. The spectral variation of the optical transmittance were determined in situ as a function of the cyclical potencial and memory effect. The insertion process of lithium is reversible and change the film color from transparent (T=80%) to dark blue (T=20%).

Sistema automático para análise direta de ligas metálicas por eletrodissolução anódica e espectrometria de absorção atômica

An automatic system for the direct determination of lead and tin by atomic absorption spectrometry is described. The on-line treatment of the metallic samples was obtained by anodic electrodissolution in a flow injection system. Lead was determined by flame atomic absorption spectrometry (FAAS) and tin by graphite furnace atomic absorption spectrometry (GFAAS). A computer program managed the current source and the solenoid valves that direct the fluids. Good linear correlations between absorbance and current intensity for lead and tin were observed. Results were in agreement with the certified values. Precision was always better than 5%. The recommended procedure allows the direct determination of 60 or 30 elements/h using FAAS or GFAAS, respectively.

Estudo voltamétrico do complexo de cobre(II) com o ligante vermelho de alizarina S, adsorvido na superfície do eletrodo de grafite pirolítico

The alizarin red S (ARS) has been used as a spectrophotometric reagent of several metals for a long time. Now this alizarin has been used as modifier agent of electrodes, for voltammetric analyses. In this work cyclic voltammetry experiments was accomplished on closed circuit, with the objective of studying the voltammetric behavior of alizarin red S adsorbed and of its copper complex, on the surface of the pyrolytic graphite electrode. These studies showed that ARS strongly adsorbs on the surface of this electrode. This adsorption was used to immobilize ions copper(II) from the solution.

Desenvolvimento e aplicação de células eletroquímicas em camada delgada

Theoretical and practical aspects concerning construction and use of a thin layer electrochemical cell are presented. Construction was realized by a simple technic and geometry was optimized in order to minimize the problems of electrical resistance. A well known redox system was studied ((Fe(III)(CN)6(3-)/Fe(II)(CN) 6(4-)) using two experimental methods, cyclic voltammetry and pulse chronopotentiometry. A numerical integration based-program was developed to calculate the voltammetric current in case of nernstian and non-nernstian behaviours and a diffusional model was used to treat the chronopotentiometric data. Thermodynamic (potential, concentration) and kinetic parameters (diffusion coefficient) were successfully determined for the redox system studied in this work.

Adsorção de íons Cu2+ em latossolo vermelho-amarelo húmico

In environmental studies it is necessary to know the adsorption behavior of metals by soils, since the unfavorable effects of heavy metals and even the micronutrients at high concentrations in the environment are related to these adsorbents' ability to immobilize them. A sample of a humic yellow red oxisol from Araponga region in the State of Minas Gerais, Brazil, was used to verify the adsorption behavior of Cu2+ ions in this substrate. The mathematical model described by Langmuir's adsorption equation in its linearized form was applied and the values of the maximum capacity b and those of the constant related to the bonding energy a were obtained. Aliquots of copper nitrate solutions containing several concentrations of this metal were added to soil samples, the pH being predetermined for developing the adsorption experiments. The chemical and physical characterization of soil sample were performed by determining the organic carbon, nitrogen and phosphorus concentrations, cation exchange capacity (CEC), pH, concentration of metals (Al, Fe, K, Mg, Ca, Zn, Cu, Ni, Cr, Co, Pb, and Cd), granulometric analysis and X-ray diffraction. Langmuir isotherms presented two distinct adsorption regions at both pH 4 and pH 5, showing that the adsorptive phenomenon occurs in two distinct stages. The adsorption sites for the lower part presented greater bonding energy and low adsorption capacity compared with the adsorption sites of the part of the curve corresponding to higher Cu concentrations in the equilibrating solution.

Eletrodissolução anódica em sistema de injeção em fluxo: uma alternativa rápida e eficiente para dissolução de ligas metálicas

Anodic electrodissolution procedure in a flow injection system for determination of constituents in alloys is discussed. This approach implement sample preparation procedure by using a chamber and a DC power supply with constant direct current. Solid sample was attached to chamber as anode. In this review a general overview of these procedure is presented. The procedure presented a good performance characterized by a high sample throughput determinations, good accuracy and relative standard deviation.

Obtenção de um material adsorvente para íons de metais pesados, através da eletropolimerização de 2-mercaptobenzimidazol à superfície de carbono vítreo reticulado

Electrochemical methods applied to organic species transformation has been used as excellent synthesis tools. C-C bonds can be established, making possible polymer synthesis by both anodic and cathodic reactions of suitable monomer species at the working electrode surface. In this study, anodic procedure was used to electropolymerization of 2-mercaptobenzimidazole at reticulated glassy carbon (RGC) surface. 2-mercaptobenzimidazole presents ligand sites towards Hg2+, Ag+ and Cu2+ ions. The obtained material has been able to adsorb the above mentioned ions in aqueous solution.

Uso de espectrometria de massas em medidas eletroquímicas - a técnica de DEMS

The combination of cyclic voltammetry and on line mass spectrometry, called differential electrochemical mass spectrometry (DEMS), is already a well established method for on line identification and quantitative detection of the products and intermediates of electrochemical reactions. This article aims to show the principles of the method and how this technique have been used to study electrochemical problems such the electrocatalytic oxidation of organic molecules, as methanol and ethanol, at noble metal electrodes.

Dióxido de titânio sol-gel: propriedades e comportamento eletrocrômico

Titanium dioxide was prepared by hydrolysis and polycondensation of titanium tetraisopropoxide. TiO2 films were obtained by spin coating of the precursor solution on ITO substractes (glass covered with indium doped tin oxide). Films were prepared using different temperatures and hydrochloric acid contents. The effect of the drying temperature of the films (100 or 400ºC) was also investigated. TiO2 films were characterized by cyclic voltammetry, chronoamperometry, ultraviolete-visible spectroscopy, scanning electron microscopy and X-ray diffractrometry.