Otimização da preparação de eletrodo de pasta de carbono contendo riboflavina imobilizada em suporte inorgânico

The aim of this work was to optimize the preparation of electrodes with riboflavin (RF) immobilized on a silica surface modified with niobium oxide and carbon paste. Electrode preparation was optimized employing a factorial design consisting of two levels and three factors. The electrochemical properties of immobilized RF were investigated by cyclic voltammetry. The factorial analysis was carried out analysing the current intensity (Ipa). It was possible to optimize the electrode to get the best reversibility in the redox process, i. e. the lowest separation between anodic and cathodic peak potentials and a current ratio close to unity. The concentration of supporting electrolyte has a small effect. The proportion has the highest effect and the interaction factor between proportion and mixture has also a significant effect on the current intensity.

Voltametria de onda quadrada. Segunda parte: aplicações

The aim of this work is to discuss some selected applications of square wave voltammetry published in the last five years. The applications focused here cover several electroanalytical fields such as: determination of pesticides; molecules with biological activity; metals and other environmental pollutants. Special attention is given to the work developed in the Grupo de Materiais Eletroquímicos e Métodos Eletroanalíticos - IQSC - USP concerning the utilization of square wave voltammetry, with different kinds of electrodes, for the determination of pesticides in natural waters and active principles in pharmaceutical formulations. The new methodology is simple, fast and sensitive when compared with the traditional ones such as chromatography and spectrophotometry. The satisfactory results obtained provide alternative procedures for the quality control of drugs and the monitoring of pesticides in natural environments.

Estudo de efeito dos sais precursores sobre as propriedades eletrocatalíticas de eletrodos de Ti-SnO2/Sb preparados por decomposição térmica

The physical and electrochemical properties of Ti-SnO2/Sb electrodes obtained by the thermal decomposition of solutions of the precursor salts SnCl2×2H2O/SbCl3 and SnSO4/Sb2(SO4)3 were investigated. The reversibility of the cyclic voltammetric response of the Fe(CN)6(4-)/Fe(CN)6(3-) redox couple was assessed using the obtained electrodes. Their catalytic activity for the oxygen-evolving reaction and maximum capacity for electronic transfer were also evaluated by potential and current linear scans in 0.5 mol L-1 H2SO4. Additionally, scanning electron microscopy analyses allowed the visualization of the morphology of the oxide films obtained. The best results were presented by the electrodes obtained from the chloride salt precursors.

Eletrodos de pasta de carbono modificados com ácidos húmicos: estudo e determinação de metais em meio aquoso

Since 1992, the carbon paste electrodes modified with humic acids have been used for studying the behavior of metals in aqueous solutions. Many parameters influence the performance of the electrodes, such as the humic acid ratio, the nature of the humic acid, the accumulation time, the pH, the scan rate, and the preparation of the electrodes itself. There are various methos of preparing the electrodes. The goal of this paper is to review some of them. The advantages of using electrodes modified with humic acids as electrochemical sensors for evaluating metals in aqueous solution are stressed.

Filmes de diamante CVD dopado com boro. Parte I . Histórico, produção e caracterização

This review presents a brief account concerning the production, characterization and evolution of the knowledge in the area of diamond and boron-doped diamond films. The most important methods used for the growth of these films, such as chemical vapor deposition and high pressure/high temperature systems, as well as the several kinds of reactors which can be employed are reviewed. However, larger emphasis is given to the CVD method. Morphological, structural and electric properties of these films, as well as their role in the performance of voltammetric electrodes for electrochemistry and electroanalytical chemistry are also discussed.

Preparação de eletrodos opticamente transparentes

A simple experiment for the preparation of transparent conducting glass electrodes by deposition of pure and fluorine doped SnO2 films is described. This procedure was tested in the undergraduate inorganic course at IQ-UNICAMP. The success in achieving a conducting layer was easily checked using the standard probes of a volt-ohm meter. The optical transmittance and thickness were studied by UV-vis spectrophotometry. To discuss the experimental results we place significant emphasis on molecular orbital and energy band model theories. The undergraduate students can also discuss the concepts related to the electronic properties of solids and to interesting new materials, such as transparent conducting films, which are the subject of significant current research and technological applications.

Eletrocatálise das reações de oxidação de hidrogênio e de redução de oxigênio

This work discusses the electrocatalytic processes taking place in the polymer electrolyte fuel cell electrodes, specifically the hydrogen oxidation reaction (HOR) and the oxygen reduction reaction (ORR), because these are clear examples of electrochemical reactions favored by the use of electrocatalysts. Since the gaseous reactants are very little soluble in the electrolyte, the use of special electrodes, named gas diffusion electrodes, is required to promote easy and continuous access of reactant gases to the electrocatalytic sites. Besides this, other important aspects such as the use of spectroscopic techniques and of theoretical models to improve the knowledge of the electrocatalytic systems are shortly discussed.

Utilização de técnicas eletroanalíticas na determinação de pesticidas em alimentos

The aim of this work is to discuss selected applications of electroanalytical techniques for the detection of pesticides in foods and beverages, published in the last ten years. The applications involved different working electrodes for the electroanalytical determination of pesticides, namely amperometric biosensors, cholinesterase-based biosensors, polymer-modified electrodes, ultramicroelectrodes and hanging mercury drop electrodes. They were used for several voltammetric and amperometric techniques in different analytical procedures for the detection and quantification of different classes of pesticides in different food matrices.

Filmes de nanodiamantes para aplicações em sistemas eletroquímicos e tecnologia aeroespacial

The goal of this work is to show the use of undoped nanodiamond films as a new material for electrochemical and aerospace applications. Correlation between the applications and physico-chemical features of nano and conventional CVD polycrystalline diamond films are presented. An important and innovative application of these nanodiamonds is organic electrosynthesis, including pharmaceutical and water disinfection products, as well as electroanalytical applications, for example, development of biosensors for detection of glucose, glutamate and dopamine. In aeronautics and space developments, these nanodiamonds could be used as electrodes in rechargable batteries and in tribological investigations.

Quimioluminiscencia electrogenerada del luminol usando electrodos de bajo costo

The purpose of the study was to observe eletrogenerated chemiluminescence (ECL) of luminol using different materials as electrodes such as wires, nails, coins, razor blades, etc. Based on the experimental observations and the mechanisms proposed in the literature, students should be capable of analyzing their results in order to understand the phenomena studied. Students could then elaborate a mechanism of action consistent with the experimental results which could rationalize the formation of intermediates in the reaction and the dependence of ECL on solution pH in addition to other points of interest

Evaluación de la reactividad de sulfuros de hierro y residuos mineros: una metodología basada en la aplicación de la voltamperometría cíclica

The mining industry around the world produces an important amount of wastes, which by their high toxic metal and iron sulfide content present a serious environmental problem. Iron sulfide oxidation under weathering conditions provokes the main environmental problem of the mining industry, the generation of Acid Rock Drainage (ARD). Up to now the prediction methodologies do not allow the study of important factors that influence the generation of ARD, producing in some cases erroneous or uncertain conclusions. This paper shows the utilization of cyclic voltammetry using carbon paste electrodes (CPE-Mineral) as an alternative tool in the study of the oxidation capacity of iron sulfides and mining wastes. This electrochemical technique constitutes a novel methodology to establish and understand the factors involved during generation of ARD. Results of several studies including selected sulfide samples and sulfide mining wastes have been described in order to show the capacity of this methodology as a complementary tool in the prediction of the generation of ARD.

Espectroscopia de impedância eletroquímica aplicada ao estudo das reações heterogêneas em ânodos dimensionalmente estáveis

This paper discusses different aspects related to the application of electrochemical impedance spectroscopy (EIS) in the study of heterogeneous electrochemical reactions occurring on Dimensionally Stable anodes (DSA®). The most relevant aspects of the semiconductor/electrolyte interface, the application of the EIS classical equivalent circuit approach and the ac porous model in DSA are presented. The paper shows that DSA type electrodes can be consistently investigated by using the ac porous model and an analysis is presented showing the advantage of applying this kind of approach to study heterogeneous reactions on DSA electrodes. Furthermore, some preliminary results on Ti/Ru0,3Ti(0,7-x)Sn x O2 based electrodes are presented to exemplify the use of the ac porous model analysis.

Princípio e utilização da técnica de efeito miragem de concentração

The aim of this work is to present the theoretical and experimental aspects of the mirage effect technique. We are especially interested in the concentration mirage effect, which is a powerful tool in the study of electrochemical reactions that produce ionic movements close to electrodes and to get some fundamental information on mass transport and charge transfer during electrochemical processes. Limitations of this technique are discussed as well as the recent attempts to overcome them.

Recentes avanços e novas perspectivas dos eletrodos íon-seletivos

This paper describes the recent progress in the development of polymeric membranes for ion-selective electrodes. The importance of knowing the mechanism of potential development in membranes for ion-selective electrodes to reach lower detection limits and improve selectivity are discussed. Recent advances and future trends of research on ion-selective electrodes are also reported.

Sensores eletroquímicos: considerações sobre mecanismos de funcionamento e aplicações no monitoramento de espécies químicas em ambientes microscópicos

Electrochemical sensors have attracted considerable attention in recent years because they provide data about the chemical state of our surroundings and the dynamics of the chemical transformations in the form a spatially resolved image. Particular interest has been directed to measurements in restricted-volume samples as new technologies enable the fabrication of miniaturized versions of sensors with reproducible characteristics. Taking these aspects into consideration, this review focuses on the use of electrodes of micrometer dimensions to acquire chemical information in microdomains in which concentrations may not be spatially homogeneous. This is possible because microelectrodes allow fast-response measurements with micrometer resolution to be performed. On the other hand, the use of microelectrodes as amperometric sensors presents an inherent drawback owing to the insufficient specificity toward the substrate of interest. Hence, some comments on strategies to enhance the selectivity of amperometric sensors are also made. Finally, recent applications of structurally microscopic electrodes as in vivo sensors are shown, as well as a prospect of the future trend in this field.