Determination of nickel in fuel ethanol using a carbon paste modified electrode containing dimethylglyoxime

A mercury-free electrode chemically modified with carbon paste containing dimethylglyoxime was used for determination of nickel in fuel ethanol. The instrumental parameters and composition of the modified paste were optimized. The analytical curve for nickel determination from 5.0 x 10(-9) to 5.0 x10(-7) mol(-1) was obtained using 25 min of accumulation time. The detection limit and amperometric sensitivity obtained for this method were 2.7 x 10 mol(-1) and 5.2 x 10(8) mu A mol(-1) L, respectively. The values for nickel concentration in four commercial samples of fuel ethanol were obtained in the range of 1.1 x 10(-8) to 6.9 x 10(-8) mol(-1). A comparison to graphite furnace atomic absorption spectrometry (GFAAS) was performed for nickel determination in commercial samples of ethanol.

Adsorption of chromium(VI) by titanium(IV) oxide coated on a silica gel surface

Titanium(IV) oxide, coated on the surface of silica gel (surface area, 308 m2 g-1; amount of Ti(IV) per gram of modified silica gel, 1.8 x 10(-3) mol), was used to adsorb CrO4(2-) ions from acidic solutions. The exchange capacity increased at lower pH values and was affected to some extent by the acid used. The material was used to preconcentrate Cr(VI) from 0.5 ppm solutions of chromate very efficiently and virtually 100% recovery was achieved in every instance.

Surface protection of fluoroindate glasses by sol-gel dip-coated SnO2 thin layers

SnO2 coatings were deposited by a sol-gel dip-coating process to shield fluoroindate glasses (40In-F-3:16BaF(2):20SrF(2):20ZnF(2):2NaF:2GaF(3)) against corrosion in aqueous environments. The effect of the number of coating applications and of the withdrawal speed on the thickness, density and roughness of tin oxide films was investigated by X-ray reflectivity. Film thickness increases both with the number of coating applications and the withdrawal speed. The aqueous leaching of uncoated and SnO2-coated fluoroindate glasses was studied by scanning electron microscopy (SEM) and infrared spectroscopy (FTIR), showing that the glass surface was protected against hydrolytic attack. (C) 1999 Elsevier B.V. B.V. All rights reserved.

Studies of the voltammetric behavior and determination of diazo reactive dyes at mercury electrode

The electrochemical reduction of two reactive dyes: Procion Red HE-3B 9 (RR120) and Procion Green HE-4BD (RG19) was investigated using cyclic voltammetry, differential pulse and DC, polarography, chronoamperometry and controlled potential electrolysis at mercury electrodes. The bis-azo groups of the RR120 dye are reduced together in one single step of four electrons, the bis-azo groups of the RG19 dye are reduced in two steps owing to the difference in the electron densities promoted by the different substituents in the benzene rings adjacent to the azo groups. The bis-monochlorotriazine reactive groups in both dyes are reduced only in acidic medium in their protonated form, leading to the reduction of the triazine groups. The reduction mechanism of both reactive dyes is discussed. Both dyes can be quantified in aqueous medium by differential pulse polarography in the concentration range of 1 x 10(-7) mol L-1 to 1 x 10(-5) mol L-1 by monitoring the reduction of the chromophore group or the reactive group.

An electrode of the second kind for benzoate determination in medicinal syrups

This paper describes the construction of an electrode of the second kind, Pt\Hg\Hg-2(Bzt)(2)\graphite, sensitive to benzoate ion (Bzt). The electrode provides a near-Nernstian response (-58.19 mV/decade at 25 degrees C) to benzoate ion in the concentration range 1.11 x 10(-1) to 5.00 x 10(-4) M at pH 7.0 and ionic strength 0.500-3.00M, adjusted with NaClO4. The electrode is easily constructed, shows a fast response time, is low in cost, has excellent response stability, and has a lifetime greater than 24 months. which is much longer than those earlier reported for other systems. A further salient feature of the electrode is that perchlorate does not interfere in its response, which may be advantageous in the analysis of perchloric acid-treated samples. It was applied to the determination of sodium benzoate in some commercial expectorating medicinal syrups using the standard additions method. The results obtained by the proposed procedure compare very favorably with those obtained through the reference method recommended by the United States Pharmacopeia. (C) 1998 Academic Press.

Determination of iodide and idoxuridine at a glutaraldehyde-cross-linked poly-L-lysine modified glassy carbon electrode

The detection limit (about 0.017 mu g mL(-1)) for voltammetric determination of iodide (peak at +0.87 V vs. Ag/AgCl at pH 2) at a glutaraldehyde-cross-linked poly-L-lysine modified glassy carbon electrode involving oxidation to iodine was found to be several orders of magnitude lower than that for the voltammetric determination on a bare glassy carbon electrode. This method was applied successfully to the determination of iodide in two medicinal formulations. Idoxuridine was determined indirectly at the same electrode by accumulating it first at -0.8 V vs. Ag/AgCl. At this potential the C-I bond in the adsorbed idoxuridine is reduced giving iodide, which is then determined at the modified electrode. The method was successfully applied to the determination of idoxuridine in a urine sample.

Microwave synthesis of calcium bismuth niobate thin films obtained by the polymeric precursor method

The crystal structure, surface morphology and electrical properties of layered perovskite calcium bismuth niobate thin films (CaBi2Nb2O9-CBN) deposited on platinum coated silicon substrates by the polymeric precursor method have been investigated. The films were crystallized in a domestic microwave and in a conventional furnace. X-ray diffraction and atomic force microscopy analysis confirms that the crystallinity and morphology of the films are affected by the different annealing routes. Ferroelectric properties of the films were determined with remanent polarization P-r and a drive voltage V-c of 4.2 mu C/cm(2) and 1.7 V for the film annealed in the conventional furnace and 1.0 mu C/cm(2) and 4.0 V for the film annealed in microwave furnace, respectively. A slight decay after 10(8) polarization cycles was observed for the films annealed in the microwave furnace indicating a reduction of the domain wall mobility after interaction of the microwave energy with the bottom electrode. (C) 2006 Elsevier Ltd. All rights reserved.

Improvement of the chemical resistance of zirconium fluoride glasses coated with a Tiron (R) modified tin oxide layer prepared by the sol-gel process

In order to improve the chemical resistance of zirconium fluoride glass a protective transparent SnO2 layer was deposited by the solgel dip-coating process in the presence of Tiron (R) as particle surface modifier agent. After water immersion for different periods of time, both coated and non-coated fluoride glasses were analyzed by scanning electron microscopy, mass loss evaluation, infrared spectroscopy and X-ray photoelectron spectroscopy. In contrast to the effects occurring for non-coated glass, where the surface undergoes a rapid selective dissolution of the most soluble species, the results for the SnO2-coated glass showed that the filling of the film nanopores by dissolved glass material results in a hermetic barrier protecting the glass surface. The selective glass dissolution was confirmed by liquid chromatography measurements of the etching solution after each exposure time. (c) 2006 Elsevier B.V. All rights reserved.

SOLIDS COATED WITH SODIUM TETRACHLOROPALLADATE - SORBENTS FOR REDUCED SULFUR-COMPOUNDS IN AIR

A study of the preconcentration of tioethers in air by means of the passage of gas flow on solid sorbents coated with sodium tetrachloropalladate was undertaken with the aim of achieving chemical fixation. This fixation presented high specificity and blocked the migration of the sorbed compound through the other active sites. The species obtained were selectively dissolved in organic solvents, resulting in the sulfur reduced compound concentration in the organic phase, which could be determined spectrophotometrically.

Alumina/zirconia composite coated by biomimetic method

In this study, a bioactive zirconia-toughened alumina (ZTA) composite was developed for orthopedic applications. This composite was obtained by slip casting of suspension powder mixtures.Biomimetic processes were used to grow a bone-like apatite layer on composite substrates using sodium silicate solution as a nucleating agent and simulated body fluids. The composites, with or without coating, were characterized by diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy and scanning electron microscopy (SEM) with energy dispersion spectroscopy (EDS), and their apparent density was determined by the Archimedes method. The composites obtained by this process possessed the expected stiffness and dimensions and their density values were similar to those of the composite's theoretical density (98.8%TD). The morphology of the hydroxyapatite formed on the composite surface was homogeneous and composed of small globules, characterizing a carbonated hydroxyapatite. The results of the tests indicated that the method employed to produce the composite and its coating was efficient under the conditions of this study. (c) 2006 Elsevier B.V. All rights reserved.

Adsorptive potentiometric stripping analysis of trace tamoxifen at a glassy carbon electrode

A highly sensitive adsorptive stripping procedure for trace measurement of the anticancer drug tamoxifen is described. The method is based on controlled adsorptive accumulation of the drug at an electrochemically treated glassy carbon electrode, followed by chronopotentiometric measurement of the surface species. The chronopotentiometric operation effectively addresses the large background contribution inherent to the glassy carbon electrode to yield a detection limit of 4 x 10(-10) M after 4 min preconcentration. The adsorptive stripping response is evaluated with respect to electrode type and conditioning, accumulation potential and lime, stripping current, pH, drug concentration, potential interferences, and other variables. Applicability to urine samples is illustrated. (C) 1997 Elsevier B.V. B.V.

Potentiometric determination of saccharin in commercial artificial sweeteners using a silver electrode

A simple, precise, rapid and low-cost potentiometric method for saccharin determination in commercial artificial sweeteners is proposed. Saccharin present in several samples of artificial sweeteners is potentiometrically titrated with silver nitrate solution using a silver wire as the indicator electrode, coupled to a titroprocessor. The best pH range was from 3.0 to 3.5 and the detection limit of sodium saccharin was 2.5 mg/ml. Substances normally found along with saccharin in several commercial artificial sweeteners such as maltodextrin, glucose, sucrose, fructose, aspartame, cyclamate, caffeine, sorbitol, lactose, nitrate, methyl- and n-propyl-p-hydroxybenzoate, benzoic, citric and ascorbic acids do not interfere even in significant amounts (e.g. 20 excess relative to saccharin). Chloride ion interferes when present in concentrations larger than 10 mg l(-1); this interference is eliminated with previous extraction of the sweetener from the aqueous medium with ethyl acetate. The results obtained by applying the proposed method compared very favorably with those given by the HPLC method recommended by the FDA. (C) 2003 Elsevier Ltd. All rights reserved.

Preparation, microstructural and electrical characterization of SrTiO3 thin films prepared by chemical route

Polycrystalline SrTiO3 thin films having a cubic perovskite structure were prepared at different temperatures by the polymeric precursor method on platinum-coated silicon substrate. Crystalline films with uniform composition and thickness were prepared by spin-coating and the post-deposition heat treatment was carried out at different temperatures. The film showed good structural, dielectric, and insulating properties, Scanning electron microscopy (SEM) micrographs showed no occurrence of interdiffusion between the bottom electrode (platinum) and the film during post-annealing, indicating a stable interface between the SrTiO3 and the bottom electrode. The dielectric constant and dissipation factor at a frequency of 100 kHz were 250 and 0.01, respectively, for a 360 nm thick film annealed at 600 degreesC. The capacitance versus applied voltage characteristics showed that the capacitance was almost independent of the applied voltage. The I-V characteristics were ohmic in low fields and a Schottky emission and/or Poole-Frenkel emission were postulated in high fields. Room temperature leakage current density was found to be in the order of 10(-7) A/cm(2) for a 360 nm thick film in an applied electric field of about 100 kV/cm. The charge storage density of 36 fC/mum(2) was obtained in an applied electric field of about 100 kV/cm. (C) 2001 Published by Elsevier B.V. Ltd. All rights reserved.

Dye-sensitized solar cell architecture based on indium-tin oxide nanowires coated with titanium dioxide

A new architecture for dye-sensitized solar cells is employed, based on a nanostructured transparent conducting oxide protruding from the substrate, covered with a separate active oxide layer. The objective is to decrease electron-hole recombination. The concept was tested by growing branched indium-tin oxide nanowires on glass using pulsed laser deposition followed by deposition of a sputtered titanium dioxide layer covering the wires. The separation of charge generation and charge transport functions opens many possibilities for dye-sensitized solar cell optimization. (c) 2007 Acta Materialia. Inc. Published by Elsevier Ltd. All rights reserved.

Test results of a superconducting fault current limiter using YBCO coated conductor

A single-phase superconducting fault current limiter (SFCL) using a 0.9 m length of YBCO coated conductor (CC) tape was tested in 220 V-60 Hz line for fault current up to 1 kA, operating in 77 K. In this work are presented the IN experimental curves measured under DC and AC currents for the electrical characterization of the CC tape in order to design a low voltage current limiter. The experimental setup is described and the test results are presented for a unit conducting a steady nominal AC current of 50 A and also during the fault time (I to 5 cycles.) the performance of the CC-based SFCL providing the limiting resistance developed in the whole tape length after few milliseconds of the beginning of the fault was analyzed.