Determination of sulfur compounds in gasoline using mercury film electrode by square wave voltammetry

A sensitive method based on square wave voltammetry is described for the quantitative determination of elemental sulfur, disulfide and mercaptan in gasoline using a mercury film electrode. These sulfur compounds can be quantified by direct dissolution of gasoline in a supporting electrolyte followed by subsequent voltammetric measurement. The supporting electrolyte is 1.4 mol L-1 sodium acetate and No acetic acid in methanol. Chemical and optimum operational conditions for the formation of the mercury film were analyzed in this study. The values obtained were a 4.3 mu m thickness for the mercury film, a 1000 rpm rotation frequency, -0.9 V applied potential and 600 s depositing time. Voltammetric measurements were obtained using square wave voltammetry with detection limits of the 3.0 x 10(-9), 1.6 x 10(-7) and 4.9 x 10(-7) mol L-1 for elemental sulfur, disulfide and mercaptan, respectively. (C) 2007 Elsevier Ltd. All rights reserved.

Qualitative and quantitative tear film abnormalities in dogs

Anormalidades do filme lacrimal de cães podem ser classificadas quanto ao seu aspecto quantitativo, qualitativo ou ambos, sendo comumente observada na prática cotidiana. Intercorrências na produção de um ou mais componentes do filme lacrimal ensejam distúrbios oculares em graus variados, denominados ceratoconjuntivite seca. Diversas são as causas da ceratoconjuntivite seca em cães, mas a maioria dos casos é de caráter idiopático, estando associada à participação de linfócitos T. O diagnóstico em medicina veterinária é firmado com base nos valores obtidos pelo teste da lacrimal de Schirmer. O presente artigo objetiva revisar os aspectos relacionados à etiopatogenia e ao diagnóstico da ceratoconjuntivite seca em cães, assim como discutir novas modalidades terapêuticas para a doença.

Filmes finos de SrBi2Ta2O9 processados em forno microondas

Filmes finos de SrBi2Ta2O9 foram depositados em substratos de Pt/Ti/SiO2/Si e, pela primeira vez, sinterizados em forno microondas doméstico. Os padrões de difração de raios X mostraram que os filmes são policristalinos. O processamento por microondas permite utilizar baixa temperatura na síntese e obter filmes com boas propriedades elétricas. Ensaios de microscopia eletrônica de varredura (MEV) e de Força Atômica (MFA) revelam boa aderência entre filme e substrato, com microestrutura de superfície apresentando grãos finos e esféricos e rugosidade de 4,7 nm. A constante dielétrica e o fator de dissipação, para freqüência de 100 KHz, à temperatura ambiente, foram de 77 e 0,04, respectivamente. A polarização remanescente (2Pr) e o campo coercitivo (Ec) foram 1,04 miC/cm² e 33 kV/cm. O comportamento da densidade de corrente de fuga revela três mecanismos de condução: linear, ôhmico e outro mecanismo que pode ser atribuído à corrente de Schottky. Dos padrões de DRX, análises das imagens por MEV e topografia de superfície por MFA observa-se que 10 min de tratamento térmico a 550 ºC, em forno microondas, é tempo suficiente para se obter a cristalização do filme.

Electronic ceramics based on polycrystalline SnO2, TiO2 and (Sn xTi1-x)O2 solid solution

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

Grain size effect on the electrical response of SnO2 thin and thick film gas sensors

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

Study of the dielectric and ferroelectric properties of chemically processed BaxSr1-xTiO3 thin films

Polycrystalline BaxSr1-xTiO3 (x = 0.4 and 0.8) thin films with a perovskite structure were prepared by the polymeric precursor method on a platinum-coated silicon substrate. High-quality thin films with uniform composition and thickness were successfully produced by dip-coating and spin-coating techniques. The resulting thin films prepared by dip and spin-coating showed a well-developed dense polycrystalline structure with uniform grain size distribution. The metal-BST-metal structure of the thin films displays good dielectric and ferroelectric properties. The ferroelectric nature to BaxSr1-xTiO3 (x = 0.8) thin film, indicated by butterfly-shaped C-V curves and confirmed by the hysteresis curve, showed 2P(r) = 5.0 muC/cm(2) and E-c = 20 kV/cm. The capacitance-frequency curve reveals that the dielectric constant may reach a value of up to 794 at 1 kHz. on the other hand, the BaxSr1-xTiO3 (x = 0.4) thin films had paraelectric nature and dielectric constant and the dissipation factor at a frequency of 100 kHz were 680 and 0.01, respectively, for film annealed at 700 degreesC. In addition, an examination of the film's I-V curve at room temperature revealed the presence of two conduction regions in the BaxSr1-xTiO3 (x = 0.4 and 0.8) thin films, showing ohmic-like behavior at low voltage and a Schottky-emission or Poole-Frenkel mechanism at high voltage. (C) 2001 Elsevier B.V. B.V. All rights reserved.

Influence of strains and defects on ferroelectric and dielectric properties of thin-film barium-strontium titanates

Pristine, W and Mn 1% doped Ba(0.6)Sr(0.4)TiO(3) epitaxial thin films grown on the LaAlO(3) substrate were deposited by pulsed laser deposition (PLD). Dielectric and ferroelectric properties were determined by the capacitance measurements and X-ray diffraction was used to determine both residual elastic strains and defect-related inhomogeneous strains-by analyzing diffraction line shifts and line broadening, respectively. We found that both elastic and inhomogeneous strains are affected by doping. This strain correlates with the change in Curie-Weiss temperature and can qualitatively explain changes in dielectric loss. To explain the experimental findings, we model the dielectric and ferroelectric properties of interest in the framework of the Landau-Ginzburg-Devonshire thermodynamic theory. As expected, an, elastic-strain contribution due to the epilayer-substrate misfit has an important influence on the free-energy. However, additional terms that correspond to the defect-related inhomogeneous strain had to be introduced to fully explain the measurements.

SrBi2Nb2O9 thin films crystallized using a low power microwave oven

SrBi2Nb2O9 thin films were produced by the polymeric precursor method using an aqueous solution. The crystallization of the films was carried out using a domestic microwave oven by means of a SiC susceptor in order to absorb the microwave energy and rapidly transfer the heat to the film. Low microwave power and short time have been used. The films obtained are well-adhered, homogeneous and with good specularity, even when treated at 600 degreesC for 10 min. The microstructure and the structure of the films can be tuned by adjusting the crystallization conditions. Depending on the direction of the heat flux it is possible to obtain preferential oriented or polycrystalline films in the microwave oven for 10 min. The microstructure presented a polycrystalline nature with spheroid small mean grain size when the susceptor is placed above the substrate. When the susceptor is placed below the substrate, the films presented platelet grains with mean grain size around 250 nm and a 001 orientation. For comparison, films were also prepared by the conventional method at 700 degreesC for 2 h. (C) 2003 Elsevier Ltd. All rights reserved.

Analytical procedure for total mercury determination in fishes and shrimps by chronopotentiometric stripping analysis at gold film electrodes after microwave digestion

A method for the total mercury determination in fish and shrimps employing chronopotentiometric stripping analysis on gold film electrodes is described. Fish and shrimp tissues were digested using a microwave oven equipped with closed vessels. We developed a microwave heating program which decomposed all the samples employing diluted nitric acid and hydrogen peroxide. The proposed method was validated by analyzing a certified reference material and then applied for different fish species from fresh water and seawater acquired in local markets of São Paulo city, Brazil. The Brazilian legislation establishes 0.5 and 1 mg per kilogram of fish as upper limit of mercury for omnivorous and predator species, respectively. Except for blue shark tissues, the mercury content was situated below 0.5 mu g g(-1) for all the analyzed samples. The detection limit of the proposed method was calculated as 5 ng g(-1) of sample utilizing 5 minutes of electrodeposition (+300 mV vs. Ag/AgCl) on the gold electrode. (c) 2006 Elsevier Ltd. All rights reserved.

Dielectric spectroscopy analysis of CaCu3Ti4O12 polycrystalline systems

Dielectric spectroscopy was used in this study to examine CaCu3Ti4O12 polycrystalline samples. The analysis involved systems presenting low non-Ohmic properties, and the grain's internal domain was evaluated separately from the contribution of barrier-layer capacitances associated with Schottky-type barriers in this type of material. The effect of oxygen-rich atmosphere and high cooling rate was evaluated, revealing a strong increase in the dielectric properties of the CaCu3Ti4O12 system under these conditions. This effect was attributed to a chemical change in the grain's internal domain, which may be considered an internal barrier-layer capacitance of the polycrystalline material. (c) 2006 American Institute of Physics.

Investigation of phase transition in ferroelectric Pb0.70Sr0.30TiO3 thin films

We have carried out dielectric and Raman spectroscopy studies at the 298-623 K temperature range in polycrystalline Pb0.70Sr0.30TiO3 thin films grown by a soft chemical method. The diffuse phase-transition behavior of the thin films was observed by means of the dielectric constant versus temperature curves, which show a broad peak. Such behavior was confirmed later by Raman spectroscopy measurements up to 823 K, indicating that a diffuselike phase transition takes place at around 548-573 K. The damping factor of the E(1TO) soft mode was calculated using the damped simple harmonic oscillator model. on the other hand, Raman modes persist above the tetragonal to cubic phase transition temperature although all optical modes should be Raman inactive. The origin of these modes was interpreted in terms of a breakdown of the microscopic local cubic symmetry by chemical disorder. The lack of a well-defined transition temperature and the presence of broad bands at some temperature interval above the ferroelectric-paraelectric phase-transition temperature suggested a diffuse nature of the phase transition. This result corroborates the dielectric constant versus temperature data, which showed a broad ferroelectric phase transition in this thin film. (C) 2004 American Institute of Physics.

Simultaneous determination of zinc, copper, lead, and cadmium in fuel ethanol by anodic stripping voltammetry using a glassy carbon-mercury-film electrode

A new, versatile, and simple method for quantitative analysis of zinc, copper, lead, and cadmium in fuel ethanol by anodic stripping voltammetry is described. These metals can be quantified by direct dissolution of fuel ethanol in water and subsequent voltammetric measurement after the accumulation step. A maximum limit of 20% (v/v) ethanol in water solution was obtained for voltammetric measurements without loss of sensitivity for metal species. Chemical and operational optimum conditions were analyzed in this study; the values obtained were pH 2.9, a 4.7-mum thickness mercury film, a 1,000-rpm rotation frequency of the working electrode, and a 600-s pre-concentration time. Voltammetric measurements were obtained using linear scan (LSV), differential pulse (DPV), and square wave (SWV) modes and detection limits were in the range 10(-9)-10(-8) mol L-1 for these metal species. The proposed method was compared with a traditional analytical technique, flame atomic absorption spectrometry (FAAS), for quantification of these metal species in commercial fuel ethanol samples.

Prediction of cassava starch edible film properties by chemometric analysis of infrared spectra

Cassava starch has been shown to make transparent and colorless flexible films without any previous chemical treatment. The functional properties of edible films are influenced by starch properties, including chain conformation, molecular bonding, crystallinity, and water content. Fourier-transform infrared (FTIR) spectroscopy in combination with attenuated total reflectance (ATR) has been applied for the elucidation of the structure and conformation of carbohydrates. This technique associated with chemometric data processing could indicate the relationship between the structural parameters and the functional properties of cassava starch-based edible films. Successful prediction of the functional properties values of the starch-based films was achieved by partial least squares regression data. The results showed that presence of the hydroxyl group on carbon 6 of the cyclic part of glucose is directly correlated with the functional properties of cassava starch films.

Microstructure and dielectric properties of (Ba,Sr)TiO3 thin film produced by the polymeric precursor method

BaxSr1-xTiO3 (x = 0.6) (BST) thin films were successfully prepared on a Pt(111)/TiO2/SiO2/Si(100) substrate by spin coating, using the polymeric precursor method. BST films with a perovskite single phase were obtained after heat treatment at 700 degrees C. The multilayer BST thin films had a granular structure will a grain size of approximately 60 nm. A 480-nm-thick film was obtained by carrying out five cycles of the spin-coating/heating process. Scanning electron microscopy and atomic force microscopy analyses showed that the thin films had a smooth, dense, crack-free surface with low surface roughness (3.6 nm). At room temperature and at a frequency of 100 kHz, the dielectric constant and the dissipation factor were, respectively, 748 and 0.042. The high dielectric constant value was due to the high microstructural quality and chemical homogeneity of the thin films obtained by the polymeric precursor method.

Preparation and properties of ferroelectric Pb1-xCaxTiO3 thin films produced by the polymeric precursor method

Pb1- xCaxTiO3 thin films with x = 0.24 composition were prepared by the polymeric precursor method on Pt/Ti/SiO2/Si substrates. The surface morphology and crystal structure, and the ferroelectric and dielectric properties of the films were investigated. X-ray diffraction patterns of the films revealed their polycrystalline nature. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) analyses showed the surface of these thin films to be smooth, dense and crack-free with low surface roughness. The multilayer Pb1-xCaxTO3 thin films were granular in structure with a grain size of approximately 60-70 nm. The dielectric constant and dissipation factor were, respectively, 174 and 0.04 at a 1 kHz frequency. The 600-nm thick film showed a current density leakage in the order of 10(-7) A/cm(2) in an electric field of about 51 kV/cm. The C-V characteristics of perovskite thin films showed normal ferroelectric behavior. The remanent polarization and coercive field for the deposited films were 15 muC/cm(2) and 150 kV/cm, respectively. (C) 2001 Kluwer Academic Publishers.