108 resultados para Scanning reference electrode technique

em Repositório Institucional UNESP - Universidade Estadual Paulista "Julio de Mesquita Filho"


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A highly sensitive amperometric biosensor for determination of carbamate pesticides directly in water, fruit and vegetable samples has been evaluated, electrochemically characterized and optimized. The biosensor strip was fabricated in screen printed technique on a ceramic support using silver-based paste for reference electrode, and platinum-based paste for working and auxiliary electrodes. The working electrode was modified by a layer of carbon paste mixed with cobalt(II) phthalocyanine and acetylcellulose. Cholinesterase (ChE) enzymes with low enzymatic charge were immobilized on this layer. The operational simplicity of the biosensor consists in that a small drop (similar to 50 mu l) of substrate or sample is deposited on a horizontally positioned biosensor strip representing the microelectrochemical cell. The working potential of the biosensor was 370 mV versus Ag/AgI on a ship reference electrode preventing the interference of electroactive species which are oxidable at more positive potentials. The biosensor was applied to investigate the degradation of two reference ChE inhibitors in freeze dried water under different storage conditions and for direct determination of some N-methylcarbamates (NMCs) in fruit and vegetable samples at ppb concentration levels without any sample pretreatment. A comparison of the obtained results for the total carbamate concentration was done against those obtained using HPLC measurements. (C) 1999 Elsevier B.V. B.V. All rights reserved.

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Biopsy by fine needle aspiration together with microbiological examination and scanning electron microscopy were evaluated in diagnosis of clinical bovine mastitis in a Prototheca zopfii outbreak. Fine needle aspiration was performed in 21 mammary quarters from ten Holstein cows presenting clinical mastitis caused by P. zopfii. The algae were previously identified in the microbiological examination of milk collected from these cows. Material aspirated from these 21 mammary glands was submitted to cytological staining (Gram, Giemsa and/or Shor staining). Fine needle aspiration enabled cytological identification of the algae in these 21 mammary glands, from which P. zopfii was isolated in the milk. Simultaneously, five mammary fragments collected by fine needle aspiration from these 21 mammary glands presenting clinical mastitis were also submitted to microbiological examination. P. zopfii was also isolated from these five fragments. Scanning electron microscopy technique also identified three of these five P. zopfii strains isolated from mammary fragments collected by cytological aspiration. These results suggest that fine needle aspiration may be an alternative method for the diagnosis of clinical mastitis.

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The presence of trace neutral organonitrogen compounds as carbazole and indole in derivative petroleum fuels plays an important role in the car's engine maintenance. In addition, these substances contribute to the environmental contamination and their control is necessary because most of them are potentially carcinogenic and mutagenic. For those reasons, a reliable and sensitive method was proposed for the determination of neutral nitrogen compounds in fuel samples, such as gasoline and diesel using preconcentration with modified silica gel (Merck 70-230 mesh ASTM) followed by differential pulse voltammetry (DPV) technique on a glassy carbon electrode. The electrochemical behavior of carbazole and indole studied by cyclic voltammetry (CV) suggests that their reduction occurs via a reversible electron transfer followed by an irreversible chemical reaction. Very well resolved diffusion controlled voltammetric peaks were obtained in dimethylformamide (DMF) with tetrabutylammonium tetrafluoroborate (TBAF(4) 0.1 mol L-1) for indole (-2.27 V) and carbazole (-2.67 V) versus Ag vertical bar AgCl vertical bar KClsat reference electrode. The proposed DPV method showed a good linear response range from 0.10 to 300 mg L-1 and a limit of detection (L.O.D) of 7.48 and 2.66 mu g L-1 for indole and carbazole, respectively. The results showed that simultaneous determination of indole and carbazole presents in spiked gasoline samples were 15.8 +/- 0.3 and 64.6 +/- 0.9 mg L-1 and in spiked diesel samples were 9.29 +/- 1 and 142 +/- 1 mg L-1, respectively. The recovery was evaluated and the results shown the values of 88.9 +/- 0.4 and 90.2 +/- 0.8% for carbazole and indole in fuel determinations. The proposed method was also compared with UV-vis spectrophotometric measures and the results obtained for the two methods were in good agreement according to the F and t Student's tests. (C) 2007 Elsevier B.V. All rights reserved.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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The musculature that sustains the stinging organ was studied in three species of social wasps using scanning electron microscopy technique. It were observed some differences among species in which sting autotomy occurs and in which it does not. These differences were related to the diameter,length and position of insertion of these muscles.

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Trypanosoma cruzi proteins from epimastigote membranes, herein referred as antigens, have been used for the construction of an amperometric immunosensor for serological diagnosis of Chagas' disease. The proteins used had a molecular mass ranging from 30 to 100 kDa. The gold electrode was treated with cysteamine and glutaraldehyde prior to antigen immobilization. Antibodies present in the serum of patients with Chagas' disease were captured by the immobilized antigens and the affinity interaction was monitored by chronoamperometry at a potential of -400 mV (versus Ag pseudo-reference electrode) using peroxidase-labeled IgG conjugate and hydrogen peroxide, iodide substrate. The incubation time to allow maximum antigen-antibody and antibody-peroxidase-labeled IgG interactions was 20 min with a reactivity threshold at -0.104 mu A. (c) 2004 Elsevier B.V. All rights reserved.

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In this work, a simple route to prepare carbon supported Pt/C, Pt:Ru/C, Pt:Mo/C and Pt:Ru:Mo/C catalysts is reported. The electrochemical properties of the several carbon materials used as substrates in the absence and in the presence of supported platinum and platinum alloys catalysts were investigated using cyclic voltammetry and employing the thin porous coating electrode technique. The activity of the dispersed catalysts composed of Pt/C with respect to the oxygen reduction and of alloy/C with respect to methanol oxidation was investigated using steady state polarization measurements. The performance with respect to the oxygen reduction reaction of the Pt/C catalyst prepared on heat-treated Vulcan carbon substrate is equivalent to that reported in the literature for the state-of-the-art electrocatysts. Pt:Ru:Mo/C samples prepared in this work presented the higher catalytic effect for methanol electro-oxidation.

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

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Fatigue, corrosion and wear resistance are important parameters in aircraft components development as landing gear. High strength/weight ratio and effective corrosion resistance make of titanium alloys an alternative choice to replace steel and aluminum alloys. However, titanium alloys have poor tribological properties, which reduce devices performance under friction. PVD coatings tribological systems has been increased due to their attractive mechanical properties as low environmental impact, low friction coefficient, low wear rate and hardness up to 2000 HV.In this study the influence of TiN deposited by PVD on the fatigue strength of Ti-6Al-4V alloy was evaluated. Comparison of fatigue strength of coated specimens and base material shows also a decrease when parts are coated. It was observed that the influence is more significant in high cycle fatigue tests. Scanning electron microscopy technique (SEM) was used to observe crack origin sites and fracture features. (C) 2010 Published by Elsevier Ltd.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Purpose: The aim of this study was (1) to determine the fluoride content in the meals served to children aged up to 36 months in daycare centres of two municipalities with different levels of fluoride in the water supply, (2) to calculate the mean fluoride ingested daily by the children when consuming those meals and (3) to analyse the contribution of this consumption to the development of dental fluorosisMaterials and Methods: Samples of the meals served to the children were collected during a whole week. The fluoride content of the samples of solid foods and milk was analysed using an ion-specific electrode combined with reference electrode after diffusion facilitated by hexamethyldisiloxane Samples of beverages were buffered with an equal volume of total ionic strength adjustment buffer and analysed using a combined electrode. The results were compared using the Mann Whitney testResults: Mean fluoride contents of the meals were of 0.204 +/- 0 179 and 0.322 +/- 0.242 mu g F/mL (P < 0.05), respectively, in the municipalities with low and adequate fluoride content. Daily fluoride intake in the former was 0.013 +/- 0.003 mg/kg body weight/day and in the latter was 0.012 +/- 0 001 mg/kg body weight/day (P > 0 05)Conclusions: The children were not exposed to dental fluorosis in the daycare centres However, the risk cannot be ignored, considering the meals and the use of fluoridated dentifrices at home may also contribute to fluoride intake.

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Objective: This study evaluated the bioavailability of fluoride after topical application of a dual-fluoride varnish commercially available in Brazil, when compared to Duraphat T. Material and methods: The urinary fluoride output was evaluated in seven 5-year-old children after application of the fluoride varnishes, in two different phases. In the first phase (I), children received topical application of the fluoride varnish Duofluorid XII (2.92% fluorine, calcium fluoride + 2.71% fluorine, sodium fluoride, FGM (TM)). After 1-month interval (phase II), the same amount (0.2 mL) of the fluoride varnish Duraphat (2.26% fluorine, sodium fluoride, Colgate T) was applied. Before each application all the volunteers brushed their teeth with placebo dentifrice for 7 days. Urinary collections were carried out 24 h prior up to 48 h after the applications. Fluoride intake from the diet was also estimated. Fluoride concentration in diet samples and urine was analyzed with the fluoride ion-specific electrode and a miniature calomel reference electrode coupled to a potentiometer. Data were tested by ANOVA and Tukey's post hoc test (p < 0.05). Results: There were significant differences in the urinary fluoride output between phases I and II. The use of Duofluorid XII did not significantly increase the urinary fluoride output, when compared to baseline levels. The application of Duraphat caused a transitory increase in the urinary fluoride output, returning to baseline levels 48 h after its use. Conclusions: The tested varnish formulation, which has been shown to be effective in in vitro studies, also can be considered safe.