909 resultados para flow-based


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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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PLZT thin films were prepared by a dip coating process using Pechini's method, also known as polymeric precursor method. The PLZT solution was obtained from a mixture of the individual cation solutions and the process to prepare each solution is based on metallic citrate polymerization. The viscosity of the PLZT solution was adjusted at 40 cP while the ionic concentration was adjusted at 0.1 M. PLZT solutions were deposited on silicon (100) and platinum coated silicon (100) substrates with withdrawal speed at 5 mm/min. The coated substrates were thermally treated with a heating rate of 1 degreesC/min up to 300 degreesC and 5 degreesC/min up to 650 degreesC in order to obtain homogeneous and cracks free films. The influence of oxygen flow on crystallization and morphology of PLZT (9/65/35) thin film is discussed. (C) 2002 Elsevier B.V. Ltd and Techna S.r.l. All rights reserved.

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A flow-injection (FI) spectrophotometric procedure exploiting merging zones is proposed for the determination of azithromycin in pharmaceutical formulations. The method is based on the reaction of azithromycin with tetrachloro-phenzoquinone (p-chloranil) accelerated by hydrogen peroxide and conducted in a methanol medium, producing a purple-red color compound (lambda(max) = 540 nm). The FI system and the experimental conditions were optimized using a multivariate method. Beer's law is obeyed in a concentration range of 50 - 1600 mu g mL(-1) with an excellent correlation coefficient (r = 0.9998). The detection limit and the quantification limit were 6.6 and 22.1 mu g mL(-1), respectively. No interference was observed from the common excipients, and the recoveries were within 98.6 to 100.4%. The procedure was applied to the determination of azithromycin in pharmaceuticals with a high sampling rate (65 samples h(-1)). The results obtained by the proposed method were in good agreement with those obtained by the comparative method at 95% confidence level.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Droplets formed at the tip of a tube under the same conditions possess extreme uniformity of form, volume and weight. These properties of liquid drop formation have been known for a long time and consequently many applications for the drop have been found in instrumentation and chemical analysis methods. In the present paper, we report on the analytical use of a dynamic LED-based flow-through optical absorption detector with optical path length controlled by continuous dropping of a solution. This arrangement consists of a flow cell built within a high-intensity red LED (lambda (max)=630 nm). The feasibility of the detector is demonstrated by colorimetric determination of methylene blue, and ammonium by Berthelot's reaction, in a flow-injection system. For ammonium, the reaction forms a blue dye (indophenol) with a maximum absorption at 630-650 nm. The detection limit, considered as 3 times the signal of the blank, is better than 125 mu g l(-1). The small flow cell represents a good combination of optical path length, low volume and fast washout. This detector can be used advantageously in automated methods and can represent a solution to problems of optical detection involving gas bubbles and precipitation of particles in turbidimetric applications.

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A flow-injection spectrophotometric procedure is proposed for methyldopa determination in pharmaceutical preparations. The determination is based on formation of a yellow product (measured at 410 nm) after complexation of methyldopa with molybdate. Under optimal conditions, Beer's law is obeyed in a concentration range of 50-200 mg l(-1) methyldopa. Typical correlation between absorbance and analyte concentration was 0.9999. Usual excipients used as additives in pharmaceuticals do not interfere with the proposed method. The analytical frequency was 210 h(-1) and the relative standard deviation (R.S.D.) was <= 2% for sample solution containing 150 mg l(-1) methyldopa (n = 11). The analytical results obtained in commercial formulations by applying the proposed FIA method were in good agreement with labeled values and those obtained by the Brazilian Pharmacopoeia procedure at 95% confidence level. (C) 2005 Elsevier B.V. All rights reserved.

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Rhizoctonia solani AG-1 IA causes leaf blight on soybean and rice. Despite the fact that R. solani AG-1 IA is a major pathogen affecting soybean and rice in Brazil and elsewhere in the world, little information is available on its genetic diversity and evolution. This study was an attempt to reveal the origin, and the patterns of movement and amplification of epidemiologically significant genotypes of R. solani AG-1 IA from soybean and rice in Brazil. For inferring intraspecific evolution of R. solani AG-1 IA sampled from soybean and rice, networks of ITS-5.8S rDNA sequencing haplotypes were built using the statistical parsimony algorithm from Clement et al. (2000) Molecular Ecology 9: 1657-1660. Higher haplotype diversity (Nei M 1987, Molecular Evolutionary Genetics Columbia University Press, New york: 512p.) was observed for the Brazilian soybean sample of R. solani AG-1 IA (0.827) in comparison with the rest of the world sample (0.431). Within the south-central American clade (3-2), four haplotypes of R. solani AG-1 IA from Mato Grosso, one from Tocantins, one from Maranhao, and one from Cuba occupied the tips of the network, indicating recent origin. The putative ancestral haplotypes had probably originated either from Mato Grosso or Maranhao States. While 16 distinct haplotypes were found in a sample of 32 soybean isolates of the pathogen, the entire rice sample (n=20) was represented by a single haplotype (haplotype 5), with a worldwide distribution. The results from nested-cladistic analysis indicated restricted gene flow with isolation by distance (or restricted dispersal by distance in nonsexual species) for the south-central American clade (3-2), mainly composed by soybean haplotypes.

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A rapid and simple method for procaine determination was developed by flow injection analysis (FIA) using a screen-printed carbon electrode (SPCE) as amperometric detector. The present method is based on the amine/hydroxylamine oxidation from procaine monitored at 0.80 V on SPCE in sodium acetate solution pH 6.0. Using the best experimental conditions assigned as: pH 6.0, flow rate of 3.8 mL min(-1), sample volume of 100 mu L and analytical path of 30 cm it is possible to construct a linear calibration curve from 9.0 x 10(-6) to 1.0 x 10(-4) mol L-1. The relative standard deviation for 5.0 x 10(-5) mol L-1 procaine (15 repetitions using the same electrode) is 3.2% and detection limit calculated is 6.0 x 10(-6) mol L-1. Recoveries obtained for procaine gave a mean values from 94.8 to 102.3% and an analytical frequency of 36 injections per hour was achieved. The method was successfully applied for the determination of procaine in pharmaceutical formulation without any pre-treatment, which are in good accordance with the declared values of manufacturer and an official method based on spectrophotometric analysis. (c) 2006 Elsevier B.V. All rights reserved.

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An analytical approach based on the generalized integral transform technique is presented, for the solution of laminar forced convection within the thermal entry region of ducts with arbitrarily shaped cross-sections. The analysis is illustrated through consideration of a right triangular duct subjected to constant wall temperature boundary condition. Critical comparisons are made with results available in the literature, from direct numerical approaches. Numerical results for dimensionless average temperature and Nusselt numbers are presented for different apex angles.

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An automatic Procedure with a high current-density anodic electrodissolution unit (HDAE) is proposed for the determination of aluminium, copper and zinc in non-ferroalloys by flame atonic absorption spectrometry, based on the direct solid analysis. It consists of solenoid valve-based commutation in a flow-injection system for on-line sample electro-dissolution and calibration with one multi-element standard, an electrolytic cell equipped with two electrodes (a silver needle acts as cathode, and sample as anode), and an intelligent unit. The latter is assembled in a PC-compatible microcomputer for instrument control, and far data acquisition and processing. General management of the process is achieved by use of software written in Pascal. Electrolyte compositions, flow rates, commutation times, applied current and electrolysis time mere investigated. A 0.5 mol l(-1) HNO3 solution was elected as electrolyte and 300 A/cm(2) as the continuous current pulse. The performance of the proposed system was evaluated by analysing aluminium in Al-allay samples, and copper/zinc in brass and bronze samples, respectively. The system handles about 50 samples per hour. Results are precise (R.S.D < 2%) and in agreement with those obtained by ICP-AES and spectrophotometry at a 95% confidence level.

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A simple and attractive method for quantification of ascorbic acid (AA) in beers, soda, natural juices and commercial vitamin C tablets was achieved by combining Bow injection analysis and amperometric detection. An array of gold microelectrodes electrochemically modified by deposition of palladium was employed as working electrode which was almost unaffected by fouling effects. Ascorbic acid was quantified in beverages and vitamin tablets using amperometric differential measurements. This method is based on three steps involving the flow injection of: 1) the sample plus a standard addition of AA, 2) the pure sample, and 3) the enzymatically-treated sample. The enzymatic treatment was carried out with Cucumis sativus tissue, which is a rich source of ascorbate oxidase, at pH 7. The calibration plots for freshly prepared ascorbic acid standards were very linear in the concentration range of 0.18-1.8 mg L-1 with a relative standard deviation (RSD) < 1%, while for real samples the deviations were between 2.7% to 8.9%.

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A flow injection system with online sample preparation is proposed for the determination of phosphite in liquid fertilizers by spectrophotometry. After loop-based injection, phosphite is oxidized by an acidic permanganate solution (1.0 10(-2) mol L-1 KMnO4 + 1.0 mol L-1 H2SO4) in a heated reactor (50 degreesC). The phosphate generated is then determined by the molybdenum blue method. Influence of flow rates, temperature, and concentration and order of addition of reagents, sample volume, and reactor configuration for the blue complex formation on recorded signals were investigated. The pow system was applied to phosphite determination in commercial samples of liquid fertilizers. The proposed system handles about 80 samples per hour [0.05-0.40% (w/v) H3PO3; R = 0,9998], consuming about 80 muL sample, 1 mg KMnO4, 25 mg (NH)(6)Mo7O24, and Ia mg ascorbic acid per determination. Results are precise [relative standard deviation less than or equal to 3.5% for 0.1% (w/v) H3PO3, n = 12] and in agreement with those obtained by gravimetry at 95% confidence level. (C) 2000 John Wiley & Sons, Inc.

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The application process of fluid fertilizers through variable rates implemented by classical techniques with feedback and conventional equipments can be inefficient or unstable. This paper proposes an open-loop control system based on artificial neural network of the type multilayer perceptron for the identification and control of the fertilizer flow rate. The network training is made by the algorithm of Levenberg-Marquardt with training data obtained from measurements. Preliminary results indicate a fast, stable and low cost control system for precision fanning. Copyright (C) 2000 IFAC.