259 resultados para Flow rate variation


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Two high-performance liquid chromatographic methods for determination of residual monomer in dental acrylic resins are described. Monomers were detected by their UV absorbance at 230 nm, on a Nucleosil((R)) C-18 (5 mu m particle size, 100 angstrom pore size, 15 x 0.46 cm i.d.) column. The separation was performed using acetonitrile-water (55:45 v/v) containing 0.01% triethylamine (TEA) for methyl methacrylate and butyl methacrylate, and acetonitrile-water (60:40 v/v) containing 0.01% TEA for isobutyl methacrylate and 1,6-hexanediol dimethacrylate as mobile phases, at a flow rate of 0.8 mL/min. Good linear relationships were obtained in the concentration range 5.0-80.0 mu g/mL for methyl methacrylate, 10.0-160.0 mu g/mL for butyl methacrylate, 50.0-500.0 mu g/mL for isobutyl methacrylate and 2.5-180.0 mu g/mL for 1,6-hexanediol dimethacrylate. Adequate assay for intra- and inter-day precision and accuracy was observed during the validation process. An extraction procedure to remove residual monomer from the acrylic resins was also established. Residual monomer was obtained from broken specimens of acrylic disks using methanol as extraction solvent for 2 h in an ice-bath. The developed methods and the extraction procedure were applied to dental acrylic resins, tested with or without post-polymerization treatments, and proved to be accurate and precise for the determination of residual monomer content of the materials evaluated. Copyright (c) 2005 John Wiley & Sons, Ltd.

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Silica gel chemically modified with 2-aminotiazole groups (SiAT), was used for preconcentration of cupper, zinc, nickel and iron from gasoline, normally used as a engine fuel. Surface characteristics and surface area of the silica gel were obtained before and after chemical modification using FT-IR, Kjeldhal and surface area analysis (B.E.T.). The retention and recovery of the analyte elements were studied by applying batch and column techniques. The experimental parameters, such as shaking time in batch technique, flow rate and concentration of the eluent (HCl-0.25-2.00 mol 1(-1)) and the amount of silica, on retention and elution, have been investigated. Detection limits of the method for cupper, iron, nickel and zinc are 0.8, 3, 2 and 0.1 mug 1(-1), respectively. The sorption-desorption of the studied metal ions made possible the development of a preconcentration method for metal ions at trace level in gasoline using flame AAS for their quantification. (C) 2004 Published by Elsevier Ltd.

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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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This investigation was carried out within the Parana sedimentary basin and involved the sampling of 78 pumped tubular wells for evaluating the hydrochemistry and radioactivity due to the nuclides (238)U, (234)U, (222)Ra, (226)Ra, and (228)Ra in the Brazilian part of Guarani aquifer. Several significant correlations were found involving the geostatic pressure, for instance, specific flow rate, CO(3)(2-), SO(4)(2-) temperature, dissolved O(2), free CO(2), pH, redox potential Eh, conductivity, Na, HCO(3)-, CO(3)(2-) , SI(calcite), Cl(-), F(-), SO(4)(2-), and B. Carbonates precipitation was evidenced by inverse correlation between CO(3)(2-) and Ca, Mg, Sr, and Ba, whereas Na exhibited an opposite trend, dissolving rather than precipitating with increasing CO(3)(2-) concentration. An inverse correlation between 3 and K was found, possibly related to the increasing tendency of K to recombine with the thickness of the clayey layers. HCO(3)-played an important role on Na, Ca, Mg, and Sr dissolution. The dissolved U content and (234)U/(238)U activity ratio data were plotted on a two-dimensional diagram that was successfully utilized on identifying an unreported zone of U accumulation, though not necessarily of economic size and grade. The variability in chemical and radionuclides data indicated an important influence of the underlying Paleozoic sediments in the composition of waters from Guarani aquifer. The available data allowed estimate the groundwater residence time by two U-isotopes disequilibrium methods. Values of 45-61 ka were initially calculated, depending on the adopted porosity (15-20%), but a longer residence time (- 640 ka) was also estimated, which is more compatible with the hydraulic conductivity data in Guarani aquifer and groundwater flow velocity occurring at Milk River aquifer, Alberta, Canada. Such time range agrees with previously reported (14)C ages exceeding 30 ka BP at the more central parts of the Parana sedimentary basin. (c) 2005 Elsevier B.V. All rights reserved.

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The fast sequential multi-element determination of Ca, Mg, K, Cu, Fe, Mn and Zn in plant tissues by high-resolution continuum source flame atomic absorption spectrometry is proposed. For this, the main lines for Cu (324.754 nm), Fe (248.327 nm), Mn (279.482 nm) and Zn (213.857 nm) were selected, and the secondary lines for Ca (239.856 nm), Mg (202.582 nm) and K (404.414 nm) were evaluated. The side pixel registration approach was studied to reduce sensitivity and extend the linear working range for Mg by measuring at wings (202.576 nm; 202.577 nm; 202.578 nm; 202.580 nm: 202.585 nm; 202.586 nm: 202.587 nm; 202.588 nm) of the secondary line. The interference caused by NO bands on Zn at 213.857 nm was removed using the least-squares background correction. Using the main lines for Cu, Fe, Mn and Zn, secondary lines for Ca and K, and line wing at 202.588 nm for Mg, and 5 mL min(-1) sample flow-rate, calibration curves in the 0.1-0.5 mg L-1 Cu, 0.5-4.0 mg L-1 Fe, 0.5-4.0 mg L-1 Mn, 0.2-1.0 mg L-1 Zn, 10.0-100.0 mg L-1 Ca, 5.0-40.0 mg L-1 Mg and 50.0-250.0 mg L-1 K ranges were consistently obtained. Accuracy and precision were evaluated after analysis of five plant standard reference materials. Results were in agreement at a 95% confidence level (paired t-test) with certified values. The proposed method was applied to digests of sugar-cane leaves and results were close to those obtained by line-source flame atomic absorption spectrometry. Recoveries of Ca, Mg, K, Cu, Fe, Mn and Zn in the 89-103%, 84-107%, 87-103%, 85-105%, 92-106%, 91-114%, 96-114% intervals, respectively, were obtained. The limits of detection were 0.6 mg L-1 Ca, 0.4 mg L-1 Mg, 0.4 mg L-1 K, 7.7 mu g L-1 Cu, 7.7 mu g L-1 Fe, 1.5 mu g L-1 Mn and 5.9 mu g L-1 Zn. (C) 2009 Elsevier B.V. All rights reserved.

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