912 resultados para analytical method


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The generalized temperature integral I(m, x) appears in non-isothermal kinetic analysis when the frequency factor depends on the temperature. A procedure based on Gaussian quadrature to obtain analytical approximations for the integral I(m, x) was proposed. The results showed good agreement between the obtained approximation values and those obtained by numerical integration. Unless other approximations found in literature, the methodology presented in this paper can be easily generalized in order to obtain approximations with the maximum of accurate.

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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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This paper analyzes through Multiple Scales Method a response of a simplified nonideal and nonlinear vibrating system. Here, one verifies the interactions between the dynamics of the DC motor (excitation) and the dynamics of the foundation (spring, damper, and mass). We remarked that we consider cubic nonlinearity (spring) and quadratic nonlinearity (DC motor) of the same order of magnitude according to experimental results. Both analytical and numerical results that we have obtained had good agreement.

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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.

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This work presents an electroanalytical method based on square-wave voltammetry (SWV) for the determination of quinizarine (QNZ) in a mixture of Britton-Robinson buffer 0.08 mol L-1 with 30% of acetonitrile. The QNZ was oxidized at glassy carbon electrode in and the well-defined peak at +0.45 V vs. Ag/AgCl can be used for its determination as colour marker in fuel samples. All parameters were optimized and analytical curves can be constructed for QNZ concentrations ranging from 2.0 x 10(-6) mol L-1 to 1.4 x 10(-5) mol L-1, using f = 60 Hz and E-sw = 25 mV. The method offers a limit detection of 4.12 x 10(-7) mol L-1 and a standard deviation of 4.5% when six measurements of 1.25 x 10(-5) mol L-1 are compared. The method was successfully applied for determining QNZ in gasoline and diesel oil and the obtained results showed good agreement with those reported previously. (c) 2006 Elsevier Ltd. All rights reserved.

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A high-performance liquid chromatography (HPLC) method for the determination of acetaldehyde in fuel ethanol was developed. Acetaldehyde was derivatized with 0.900 mL 2,4-dinitrophenylhydrazine (DNPHi) reagent and 50 mu L phosphoric acid 1 mol L-1 at a controlled room temperature of 15 degrees C for 20 min. The separation of acetaldehyde- DNPH (ADNPH) was carried out on a Shimadzu Shim-pack C-18 column, using methanol/LiCl(aq) 1.0 mM (80/20, v/v) as a mobile phase under isocratic elution and UV-Vis detection at 365 nm. The standard curve of ADNPH was linear in the range 3-300 amg L-1 per injection (20 mu L) and the limit of detection (LOD) for acetaldehyde was 2.03 mu g L-1, with a correlation coefficient greater than 0.999 and a precision (relative standard deviation, RSD) of 5.6% (n=5). Recovery studies were performed by fortifying fuel samples with acetaldehyde at various concentrations and the results were in the range 98.7-102%, with a coefficient of variation (CV) from 0.2% to 7.2%. Several fuel samples collected from various gas stations were analyzed and the method was successfully applied to the analysis of acetaldehyde in fuel ethanol samples.

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An analytical approach for the spin stabilized satellite attitude propagation is presented using the non-singular canonical variables to describe the rotational motion. Two sets of variables were introduced for Fukushima in 1994 by a canonical transformation and they are useful when the angle between z-satellite axis of a coordinate system fixed in artificial satellite and the rotational angular momentum vector is zero or when the angle between Z-equatorial axis and rotation angular momentum vector is zero. Analytical solutions for rotational motion equations and torque-free motion are discussed in terms of the elliptic functions and by the application of some simplification to get an approximated solution. These solutions are compared with a numerical solution and the results show a good agreement for many rotation periods. When the mean Hamiltonian associated with the gravity gradient torque is included, an analytical solution is obtained by the application of the successive approximations' method for the satellite in an elliptical orbit. These solutions show that the magnitude of the rotation angular moment is not affected by the gravity gradient torque but this torque causes linear and periodic variations in the angular variables, long and short periodic variations in Z-equatorial component of the rotation angular moment and short periodic variations in x-satellite component of the rotation angular moment. The goal of this analysis is to emphasize the geometrical and physical meaning of the non-singular variables and to validate the approximated analytical solution for the rotational motion without elliptic functions for a non-symmetrical satellite. The analysis can be applied for spin stabilized satellite and in this case the general solution and the approximated solution are coincidence. Then the results can be used in analysis of the space mission of the Brazilian Satellites. (C) 2007 COSPAR. Published by Elsevier Ltd. All rights reserved.

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A new approach is proposed in this work for the treatment of boundary value problems through the Adomian's decomposition method. Although frequently claimed as accurate and having fast convergence rates, the original formulation of Adomian's method does not allow the treatment of homogeneous boundary conditions along closed boundaries. The technique here presented overcomes this difficulty, and is applied to the analysis of magnetohydrodynamic duct flows. Results are in good agreement with finite element method calculations and analytical solutions for square ducts. Therefore, new possibilities appear for the application of Adomian's method in electromagnetics.

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Throughout the world, biomonitoring has become the standard for assessing exposure of individuals to toxic elements as well as for responding to serious environmental public health problems. However, extensive biomonitoring surveys require rapid and simple analytical methods. Thus, a simple and high-throughput method is proposed for the determination of arsenic (As), cadmium (Cd), copper (Cu), manganese (Mn), nickel (Ni), lead (Pb), and selenium (Se) in blood samples by using inductively coupled plasma-mass spectrometry (ICP-MS). Prior to analysis, 200 l of blood samples was mixed with 500 l of 10% v/v tetramethylammonium hydroxide (TMAH) solution, incubated for 10 min, and subsequently diluted to 10 ml with a solution containing 0.05% w/v ethylenediamine tetraacetic acid (EDTA) + 0.005% v/v Triton X-100. After that, samples were directly analyzed by ICP-MS (ELAN DRC II). Rhodium was selected as an internal standard with matrix-matching calibration. Method detection limits were 0.08, 0.04, 0.5, 0.09, 0.12, 0.04, and 0.1 g//L for As, Cd, Cu, Mn, Ni, Pb, and Se, respectively. Validation data are provided based on the analysis of blood samples from the trace elements inter-\comparison program operated by the Institut National de Sante Publique du Quebec, Canada. Additional validation was provided by the analysis of human blood samples by the proposed method and by using electrothermal atomic absorption spectrometry (ETAAS). The method was subsequently applied for the estimation of background metal blood values in the Brazilian population. In general, the mean concentrations of As, Cd, Cu, Mn, Ni, Pb, and Se in blood were 1.1, 0.4, 890, 9.6, 2.1, 65.4, and 89.3 g/L, respectively, and are in agreement with other global populations. Influences of age, gender, smoking habits, alcohol consumption, and geographical variation on the values were also considered. Smoking habits influenced the levels of Cd in blood. The levels of Cu, Mn, and Pb were significantly correlated with gender, whereas Cu and Pb were significantly correlated with age. There were also interesting differences in Mn and Se levels in the population living in the north of Brazil compared to the south.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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A small-scale method was developed for the simultaneous determination of γ-HCH, heptachlor, aldrin, dicofol, mirex, endosulfan I, endosulfan II and endosulfan sulphate in soil. The extraction and clean-up steps were combined into one step by transferring soil samples to chromatographic columns prepacked with neutral alumina. The pesticides elution was processed with n-hexane : dichloromethane (7:3) and the concentrated eluate was analysed using gas-liquid chromatography with electron capture detection. Analyses of the in vitro fortified samples with the selected pesticides were performed at three different levels. Mean recoveries for aldrin, γ-HCH and heptachlor, at levels of 2, 10 and 20 ng/g, ranged from 71 to 87%; for dicofol, at levels of 8, 40 and 80 ng/g, ranged from 97 to 103%; for endosulfan I and II, at levels of 5, 25 and 50 ng/g, ranged from 88 to 96%; for mirex, at levels of 6, 30 and 60 ng/g, ranged from 86 to 110%; and for endosulfan sulphate, at levels of 15, 75 and 150 ng/g, ranged from 93 to 104%. The method can be used for rapid determination of these pesticides in soil. © Springer-Verlag 1996.

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We present angular basis functions for the Schrödinger equation of two-electron systems in hyperspherical coordinates. By using the hyperspherical adiabatic approach, the wave functions of two-electron systems are expanded in analytical functions, which generalizes the Jacobi polynomials. We show that these functions, obtained by selecting the diagonal terms of the angular equation, allow efficient diagonalization of the Hamiltonian for all values of the hyperspherical radius. The method is applied to the determination of the 1S e energy levels of the Li + and we show that the precision can be improved in a systematic and controllable way. ©2000 The American Physical Society.

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We apply the Bogoliubov Averaging Method to the study of the vibrations of an elastic foundation, forced by a Non-ideal energy source. The considered model consists of a portal plane frame with quadratic nonlinearities, with internal resonance 1:2, supporting a direct current motor with limited power. The non-ideal excitation is in primary resonance in the order of one-half with the second mode frequency. The results of the averaging method, plotted in time evolution curve and phase diagrams are compared to those obtained by numerically integrating of the original differential equations. The presence of the saturation phenomenon is verified by analytical procedures.