Cost-effective composite electrode for the fast voltammetric screening and determination of riboflavin (B2) and pyridoxine (B6) in pharmaceuticals

Different solid composites made by mechanical dispersions of graphite particles into heated paraffin (from 65 to 80% graphite, in mass) were prepared and assessed in order to optimize their use in electrochemical and electroanalytical procedures for bioanalysis. Besides these, composites were also evaluated by thermoanalytical techniques aiming to study their conservation and long-term stability (over eight months without special care), among others. Best results were found at 80% m/m graphite in paraffin. Such electrode combines low-cost, stability, sensitivity, ease of maintenance and clearance, besides the possibilities of manufacture in many different forms and shapes (with or without modifications) and applicability in a wide range of pH. Electrochemical studies by different voltammetric techniques involving vitamins from complex B (riboflavin and pyridoxine) leaded to a better understanding about their electrooxidative processes onto carbon-composite electrodes, specially regarding reversibility and pH-dependence. Data were also acquired and optimized with analytical purposes, being square-wave voltammetry in pH 4.2 chosen by its many advantages. Good linearity between peak responses as function of concentration were reached from 5 to 43 μmol L-1 for riboflavin (peak at -0.257 V) and up to 8.5 × 10-4 mol L -1 for pyridoxine (peak at +1.04 V), best studied conditions; limits of detection (at an S/N of 3) for both analites showed to be circa 1.0 mol L-1. Different commercial samples were analyzed for riboflavin (EMS® complex B syrup) and pyridoxine (Citoneurin 5000 Merck® ampoules) providing 96.6% and 98.7% recoveries, respectively.

Preparation and characterization of LiNi0.8Co0.2O2/PANI microcomposite electrode materials under assisted ultrasonic irradiation

A preparation method for a new electrode material based on the LiNi0.8Co0.2O2/polyaniline (PANI) composite is reported. This material is prepared by in situ polymerization of aniline in the presence of LiNi0.8Co0.2O2 assisted by ultrasonic irradiation. The materials are characterized by XRD, TG-DTA, FTIR, XPS, SEM-EDX, AFM, nitrogen adsorption (BET surface area) and electrical conductivity measurements. PANI in the emeraldine salt form interacts with metal-oxide particles to assure good connectivity. The dc electrical conductivity measurements at room temperature indicate that conductivity values are one order of magnitude higher in the composite than in the oxide alone. This behavior determines better reversibility for Li-insertion in charge-discharge cycles compared to the pristine mixed oxide when used as electrode of lithium batteries. (c) 2005 Elsevier B.V. All rights reserved.

Preparation and study as positive electrode of Li0.33La0.56TiO3-PANI nanocomposite

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

Structural and electrochemical properties of LiCoO2 prepared by combustion synthesis

LiCoO2 powders were prepared by combustion synthesis, using metallic nitrates as the oxidant and metal sources and urea as fuel. A small amount of the LiCoO2 phase was obtained directly from the combustion reaction, however, a heat treatment was necessary for the phase crystallization. The heat treatment was performed at the temperature range from 400 up to 700 degreesC for 12 h. The powders were characterized by X-ray diffraction (XRD), X ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and specific surface area values were obtained by BET isotherms. Composite electrodes were prepared using a mixture of LiCoO2, carbon black and poly(vinylidene fluoride) (PVDF) in the 85:10:5% w/w ratio. The electrochemical behavior of these composites was evaluated in ethylene carbonate/dimethylcarbonate solution, using lithium perchlorate as supporting electrolyte. Cyclic voltammograms showed one reversible redox process at 4.0/3.85 V and one irreversible redox process at 3.3 V for the LiCoO2 obtained after a post-heat treatment at 400 and 500 degreesC.Raman spectroscopy showed the possible presence of LiCoO2 with cubic structure for the material obtained at 400 and 500 degreesC. This result is in agreement with X-ray data with structural refinement for the LiCoO2 powders obtained at different temperatures using the Rietveld method. Data from this method showed the coexistence of cubic LiCoO2 (spinel) and rhombohedral (layered) structures when LiCoO2 was obtained at lower temperatures (400 and 500 degreesC). The single rhombohedral structure for LiCoO2 was obtained after post-heat treatment at 600 degreesC. The maximum energy capacity in the first discharge was 136 mA g(-1) for the composite electrode based on LiCoO2 obtained after heat treatment at 700 degreesC. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Composite resin color stability: influence of light sources and immersion media

Objective: This study evaluated the influence of light sources and immersion media on the color stability of a nanofilled composite resin. Material and Methods: Conventional halogen, high-power-density halogen and high-power-density light-emitting diode (LED) units were used. There were 4 immersion media: coffee, tea, Coke (R) and artificial saliva. A total of 180 specimens (10 mm x 2 mm) were prepared, immersed in artificial saliva for 24 h at 37 +/- 1 degrees C, and had their initial color measured with a spectrophotometer according to the CIELab system. Then, the specimens were immersed in the 4 media during 60 days. Data from the color change and luminosity were collected and subjected to statistical analysis by the Kruskall-Wallis test (p<0.05). For immersion time, the data were subjected to two-way ANOVA test and Fisher's test (p<0.05). Results: High-power-density LED (Delta E=1.91) promoted similar color stability of the composite resin to that of the tested halogen curing units (Jet Lite 4000 plus - Delta E=2.05; XL 3000 - Delta E=2.28). Coffee (Delta E=8.40; Delta L=-5.21) showed the highest influence on color stability of the studied composite resin. Conclusion: There was no significant difference in color stability regardless of the light sources, and coffee was the immersion medium that promoted the highest color changes on the tested composite resin.

Preparation and Characterization of Graphite-Epoxy Composite Modified with Zinc Hexacyanoferrate and Their Electrochemical Behaviour in Presence of Substituted Anilines

The growth of zinc hexacyanoferrate (ZnHCF) hybrid film on the surface of graphite-epoxy composite (GEC) electrodes was demonstrated by cyclic voltammetry. Surface morphology of the hybrid film was investigated by using scanning electron microscopy. The effect of the type of monovalent cations on the redox behaviour of hybrid film was also studied. This effect indicated that the radius of the hydrated cation mainly determines the ion permeability of the film.The electrochemical behavior of the substituted anilines (procaine and sulfamerazine) in 1 M KCl of the modified GEC electrode showed a decrease of the cathodic currents while increasing the concentration of these analytes. The developed sensor also showed excellent stability for long time usage, higher sensitivity and cost-effective fabrication.

Electrode surface modifications improve cathode hydrogen production and anode capacity in Ni-MH batteries

This paper reports results from electrochemical evaluations of electrodes used as cathodes for a hydrogen evolution reaction and anodes in Ni-MH batteries that had been surface-modified by micro-encapsulation, co-deposition and sol-gel methods. The surface modifications produced actual improvements in the corresponding electrochemical reactions by enhancing the performance and/or the mechanical stability of the electrode material. (c) 2005 International Association for Hydrogen Energy. Published by Elsevier Ltd. All rights reserved.

Enhanced photoabsorption properties of composites of Ti/TiO2 nanotubes decorated by Sb2S3 and improvement of degradation of hair dye

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

Volumetric microleakage assessment of glass-ionomer-resin composite hybrid materials

Objective: This study was intended to quantify the marginal leakage of three glass-ionomer-resin composite hybrid materials and compare it with the leakage exhibited by a glass-ionomer cement and a bonded resin composite system. Method and materials: Standardized Class V cavities were prepared on root surfaces of 105 extracted human teeth, randomly assigned to five groups of 21 each, and restored with either Ketac-Fil Aplicap, Z100/Scotchbond Multi-Purpose Plus, Vitremer, Photac-Fil Aplicap, or Dyract. The teeth were thermally stressed for 500 cycles and stained with methylene blue. The microleakage was quantified spectrophotometrically, and the data were statistically analyzed with Friedman's test. Results: There were no significant differences in microleakage among the five groups. Restorations of all tested materials showed some marginal leakage in Class V cavities. Conclusion: The microleakage performance of glass-ionomer-resin composite hybrid materials was similar to those of a conventional glass-ionomer and a bonded resin composite system.

Photoelectrochemical properties of FTO/p-NiO electrode induced by UV light irradiation

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Avaliação da limpeza de CDtrodo construídos a partir de CD de ouro gravável/fita adesiva de galvanoplastia

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

Poole-Frenkel effect in amorphous poly(p-phenylene sulfide)

The conductivity of poly(p-phenylene sulfide) (PPS) amorphous samples sandwiched between metallic electrodes has been studied as a function of applied voltage, temperature, and electrode material. The voltage (U) dependence of the currents for electric fields within the range 10(3)-10(6) V/cm exhibits exp beta U-1/2 behavior with beta = beta(Schottky) below the glass transition temperature (T-g congruent to 90 degrees C), and beta = beta(Poole-Frenkel) above T-g. Coordinated temperature measurements of de currents with different metallic contacts and thermally stimulated currents (TSC) indicate, however, that the conductivity at T < T-g is consistent with the so-called ''anomalous'' Poole-Frenkel effect rather than the Schottky effect. Consequently, the p-type conductivity in amorphous PPS is proposed to be a bulk-limited process due to ionization of two different types of acceptor centers in the presence of neutral hole traps. (C) 1996 John Wiley & Sons, Inc.

Electrical properties of screen printed BaTiO3 thick films

The deposition of thick film pastes by screen-printing is a relatively simple and convenient method to produce thicker layers with thickness up to 100 mum. In the present work, the barium titanate thick films were prepared from mechanically activated powders based on BaC03 and TiO2. After mixing, the powders were calcined at low temperature by slow heating and cooling rates. The thick films were deposited on to Al2O3 substrates through hybrid technology. The obtained films were fired at 850 degreesC together with electrode material (silver/palladium). The electrical properties of thick films: dielectric permittivity, dielectric losses, Curie temperature, hysteresis loop were reported. The obtained BT thick films can be applied in as multilayer capacitors or in gas sensor application. (C) 2003 Elsevier Ltd. All rights reserved.

A surface modification for hydrogen storage intermetallic particles by sol-gel method

A new process for the surface modification of hydrogen storage intermetallic particles used as anode material in secondary batteries is proposed in this article. The copper oxide particles coverage obtained by the sol-gel method is proposed to produce, under operational conditions of a Ni-MH battery, a metallic framework that tolerates the volume changes in charge/discharge cycles and does not inhibit the hydrogen absorption. Furthermore it was noticed an enhancement on the discharge capacity of the electrode material that can be related to a new hydrogen storage phase or to an inhibition of the surface oxidation promoted by the film coverage.

Síntese, caracterização e avaliação eletroquímica de nanopartículas intermetálicas ordenadas PtSb e PtSn

Pós-graduação em Ciência e Tecnologia de Materiais - FC