802 resultados para Electrochemical characterizations


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A sensor was fashioned to monitor the volume of nutrient in a solid substrate-based growth media by using electrochemical admittance spectroscopy. Several experimental parameters were investigated (i.e. The use of two- or three-electrode cells, the superficial area of the electrode, the amount of nutrient solution added to the growth media, and the influence of varying the dc and ac potential) to assess how these variables affect the admittance of the system. A linear correlation was observed between the maximum of the imaginary admittance and the volume of nutrient present. The response factor was 2.8 x 10(-5) S cm(-2) ml(-1) and the limit of detection (LOD) was 0.54 ml. The humidity of the growth media does not change the response of the nutrient toward the monitoring measurements. These results demonstrate that the volume of nutrient in this solid substrate-based growth media can be assessed using a ceramic sensor to measure the imaginary admittance. (C) 2002 Elsevier B.V. B.V. All rights reserved.

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Pt-modified RuO2 was prepared by a sol-gel procedure on titanium substrates in the form of thin films of similar to2-mum thickness. X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) analyses showed that these films actually consist of Pt nanoparticles dispersed in RuO2 and that neither metallic Ru nor Pt-Ru alloy are present on the surface. Electrodes with different Pt:Ru nominal compositions were prepared and their electrocatalytic activity for the oxidation of methanol was investigated by potential sweeps and chronoamperometry. The results obtained show an enhancement effect for methanol oxidation that can be interpreted as associated to the formation of hydrous oxides on the RuO2 surface.

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The oxidation of a reactive dye, Reactive Blue 4, RB4, (C.I. 61205), widely used in the textile industries to color natural fibers, was studied by electrochemical techniques. The oxidation on glassy carbon electrode and reticulated vitreous carbon electrode occurs in only one step at 2.0 < PH < 12 involving a two-electron transfer to the amine group leading to the imide derivative. Dye solution was not decolorized effectively in this electrolysis process. Nevertheless, the oxidation of this dye on Ti/SnO2/SbOx (3% mol)/RuO2 (1% mol) electrode showed 100% of decolorization and 60% of total organic carbon removal in Na2SO4 0.2 M at PH 2.2 and potential of +2.4 V. Experiments on degradation photoelectrocatalytic were also carried out for RB4 degradation in Na2SO4 0.1 K PH 12, using a Ti/TiO2 photoanode biased at +1.0 V and UV light. After 1 h of electrolysis the results indicated total color removal and 37% of mineralization. (c) 2004 Elsevier Ltd. All rights reserved.

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The oxidation of a reactive dye, Cibacron Blue F3GA, CB, (C.I. 61211), widely used in the textile industries to color natural fibers, was studied by electrochemical techniques. The oxidation on glassy carbon electrode occurs in two steps at 2.0 < pH < 10 involving one electron transfer each to the amine group leading to the imide derivative. Stable films of poly-L-lysine (PLL) in the presence of glutaraldehyde (GA) 97.5%:2.5% on glassy carbon electrode can be used to detect low levels of dye using its oxidation peak at +0.75V by voltammetry. Linear calibration graphs were obtained for the CB reactive dye, from 1.0 X 10(-6) to 1.0 X 10(-5) mol L-1 in B-R buffer, pH 2.0, using a pre-concentration off-line during 10 min. The detection limit (3 sigma/slope) was calculated to be 4.5 X 10(-8) mol L-1. Films of PLL can readily be applied for the determination of CB dye bearing aminoanthraquinone as chromophore and chlorotriazinyl as reactive group at concentrations at least 100 times lesser than using a glassy carbon electrode without modification. The method described was applied for the determination of CB dye in tap water and raw water collected from the municipal treatment plant with a recovery of 89.2% +/- 5.4 and 88.0% +/- 6.5, respectively. (c) 2005 Elsevier Ltd. All rights reserved.

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The electrochemical reduction of serine, glycine, and leucine protected by the 4-nitrobenzenesulfonyl, group in N,N-dimethylformamide at mercury cathode occurs at two steps. The first one at -0.8 V vs. SCE, after a one-electron transfer, leads the anion radical formation that dimerizes and adsorbs at electrode. In the second step at -1.4 V, an instable dianion forms which then cleaves. The mechanism is discussed.

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The microbiological leaching of chalcopyrite (CuFeS2) is of great interest because of its potential application to many CuFeS2-rich ore materials. However, the efficiency of the microbiological process is very limited because this mineral is one of the most refractory to bacterial attack. Knowledge of bacterial role during chalcopyrite oxidation is very important in order to improve the efficiency of bioleaching operation. The oxidative dissolution of a massive chalcopyrite electrode by Acidithiobacillus ferrooxidans was evaluated by electrochemical impedance spectroscopy (EIS) and atomic force microscopy (AFM). A massive chalcopyrite electrode was utilized in a Tait-type electrochemical cell in acid medium for different immersion times in the presence or absence of bacterium. The differences observed in the impedance diagrams were correlated with the adhesion process of bacteria on the mineral surface. (C) 2004 Elsevier B.V. All rights reserved.

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The electrochemical reduction of benzenesulfinic, p-toluenesulfinic, and p-nitrobenzenesulfinic acids was studied in dimethylsulfoxide solutions. From cyclic voltammetry experiments, a chemical reaction following the first electron transfer was detected during the reduction process. A cyclic voltammetry technique using ultramicroelectrodes has provided kinetic parameters for the electron-transfer steps, from which it was possible to observe the influence of the ring substituent on the electrochemical reduction. The mechanism of the electroreduction of aromatic sulfinic acids in dimethylsulfoxide depends upon the nucleophilic attack of the radical anion produced on the starting compound during the reduction processes.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Hydroxychloroquine (HCQ) is a halogenated aminoquinoline that presents wide biological activity, often being used as an antimalarial drug. The electrochemical reduction of HCQ was investigated by cyclic voltammetry and chronoamperometry using glassy carbon electrodes. By cyclic voltammetry, in acid medium, only the cathodic peak was observed. The electrochemical behavior of this peak is dependent on pH and the electrodic process occurs through an ErCi mechanism. The electron number (le) consumed in the reduction of HCQ was obtained by chronoamperometry. A method for the electrochemical determination of HCQ in pharmaceutical tablets was developed using differential pulse voltammetry. The detection limit reached was 11.2 mug ml(-1) of HCQ with a relative standard deviation of 0.46%. A spectrophotometric study of HCQ has been also carried out utilizing a band at 343 nm. The obtained detection limit and the relative standard deviation were 0.1 mug ml(-1) and 0.36%, respectively. The electrochemical methods are sufficiently accurate and precise to be applied for HCQ determination, in laboratorial routine, which can be used to determine the drug at low level. (C) 2003 Elsevier B.V. B.V. All rights reserved.

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The cathodic behaviour of oxides formed on titanium electrodes in physiological solutions at potentials between 3 and 5 V (vs. SCE) was studied by cyclic voltammetry. In case of anodic polarization at potentials higher than 3 V (vs. SCE), a cathodic peak at similar to 0.4 V (vs. SCE) appears in the cathodic scan, which could be due to the reduction of unstable peroxides. The results show that this peak depends on the anodic potential and the oxidation time. This behaviour supposedly is due to the formation of unstable titanium peroxides like TiO3 during anodization. Based on repetitive oxidation-reduction processes can be concluded that the created amount of TiO3 inside of the TiO2 surface layer seems to be constant. (c) 2006 Elsevier Ltd. All rights reserved.

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The effect of consecutive cyclic polarization in de-aerated 0.5 M NaOH solutions on the surface microstructure of mechanically polished Cu-Al-Ag alloys of different compositions and heat treatments has been studied using optical microscopy, SEM and EDS. The current peaks of the cyclic polarization curves do not depend on the alloy composition in the composition range studied. The repetitive potential scans between H2 and O2 evolution in alkaline media lead to preferential dissolution of aluminium, the roughness and phase composition of the surface of the alloys changing significantly. The quasistationary I-E curves of the different Cu-Al-Ag alloys studied consist in the superposition of the quasistationary I-E curves of high-purity Cu and Ag, the EDS microanalysis showing that aluminium is not present on the surface of the alloy in these conditions.

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The generation of active chlorine on Ti/Sn(1-x)Ir (x) O-2 anodes, with different compositions of Ir (x = 0.01, 0.05, 0.10 and 0.30 ), was investigated by controlled current density electrolysis. Using a low concentration of chloride ions (0.05 mol L-1) and a low current density (5 mA cm(-2)) it was possible to produce up to 60 mg L-1 of active chlorine on a Ti/Sn0.99Ir0.01O2 anode. The feasibility of the discoloration of a textile acid azo dye, acid red 29 dye (C.I. 16570), was also investigated with in situ electrogenerated active chlorine on Ti/Sn(1-x)Ir (x) O-2 anodes. The best conditions for 100% discoloration and maximum degradation (70% TOC reduction) were found to be: NaCl pH 4, 25 mA cm(-2) and 6 h of electrolysis. It is suggested that active chlorine generation and/or powerful oxidants such as chlorine radicals and hydroxyl radicals are responsible for promoting faster dye degradation. Rate constants calculated from color decay versus time reveal a zero order reaction at dye concentrations up to 1.0 x 10(-4) mol L-1. Effects of other electrolytes, dye concentration and applied density currents also have been investigated and are discussed.

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The design and characteristics of a novel electrochemical system, which uses a drop as a renewable electroanalytical sensor, are described. This article describes the performance of the electrochemical system, the coupling of the experimental arrangement with flow injection technique and a demonstration of its applicability for the measurement of sulfide. The method is based on renewable drops of ferricyanide ions, buffered by borate. The ferrocyanide ions, product of the reaction between ferricyanide and sulfide ions, are oxidized on a platinum microelectrode and the current measured is related to sulfide concentration. The measurements can be done in continuous or static flow mode. In continuous mode, the detection limit is 5.0 x 10(-5) mol L-1.

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A quantitative phase analysis was made of LiXCoO2 powders obtained by two distinct chemical methodologies at different temperatures (from 400 to 700degreesC). A phase analysis was made using Rietveld refinements based on X-ray diffraction data, considering the LiXCoO2 powders as a multiphase system that simultaneously contained two main phases with distinct, layered and spinel-type structures. The sults showed the coexistence of both structures in LiXCoO2 obtained at low temperature (400 and 500degreesC), although only the layered structure was detected at higher temperatures (600 and 700degreesC, regardless of the chemical powder process employed. The electrochemical performance, evaluated mainly by the cycling reversibility of LiXCoO2 in the form of cathode insertion electrodes, revealed that there is a close correlation between structural features and the electrochemical response, with one of the redox processes (3.3 v/3.9 v) associated only with the presence of the spinel-type structure. (C) 2003 Elsevier B.V. All rights reserved.