956 resultados para limit of quantitation


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An amperometric oxygen sensor based on a polymeric nickel-salen (salen = N,N '-ethylenebis(salicydeneiminato)) film coated platinum electrode was developed. The sensor was constructed by electropolymerization of nickel-salen complex at a platinum electrode in acetonitrile/tetrabuthylamonium perchlorate by cyclic voltammetry. The voltammetric behavior of the modified electrode was investigated in 0.5 mol L-1 KCl solution in the absence and presende of molecular oxygen. A significant increased of cathodic peak current (at -0.20 vs. SCE) of the modified electrode with addition of oxygen to the solution was observed. This result shows that the nickel-salen film on the surface of the electrode promotes the reduction of oxygen. The reaction can be brought about electrochemically where in the nickel(II) complex is first reduced to a nickel(I) complex at the electrode surface. The nickel(I) complex then undergoes a catalytic oxidation by the oxygen molecular in solution back to the nickel(II) complex, which can then be electrochemically re-reduced to produce an enhancement of the cathodic current. The plot of the cathodic current versus the dissolved oxygen concentration for chronoamperometry (potential fixed = -0.20 V) at the sensor was linear in the concentration range of 3.95 to 9.20 mg L-1 with concentration limit of 0.17 mg L-1 O-2. The modified electrode proposed is useful for the quality control and routine analysis of dissolved oxygen in commercial water and environmental water samples. The results obtained for the levels of dissolved oxygen are in agreement with the results obtained with an O-2 commercial sensor. (C) 2011 Published by Elsevier Ltd.

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The reproducibility of the 6-min walking test (6MWT) needs to be more solidly studied. This study aimed to investigate the reproducibility of two 6MWTs performed on subsequent days in a large and representative sample of patients with chronic obstructive pulmonary disease (COPD), and to quantify the learning effect between the two tests, as well as its determinants.In a retrospective observational study, 1,514 patients with COPD performed two 6MWTs on subsequent days. Other measurements included body composition (dual X-ray absorptiometry), dyspnoea (Medical Research Council scale) and comorbidity (Charlson index).Although the 6MWT was reproducible (intraclass correlation coefficient=0.93), patients walked farther in the second test (391 m, 95% CI 155-585 m versus 418 m, 95% CI 185-605 m; p < 0.0001). on average, the second 6MWT increased by 27 m (or 7%), and 82% of patients improved in the second test. Determinants of improvement >= 42 m in the second test (upper limit of the clinically important change) were as follows: first 6MWT < 350 m, Charlson index < 2 and body mass index < 30 kg.m(-2) (OR 2.49, 0.76 and 0.60, respectively).The 6MWT was statistically reproducible in a representative sample of patients with COPD. However, the vast majority of patients improved significantly in the second test by an average learning effect of 27 m.

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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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A tungsten carbide coating on the integrated platform of a transversely heated graphite atomizer was used as a modifier for the direct determination of Se in soil extracts by graphite furnace atomic absorption spectrometry. Diethylenetriaminepentaacetic acid (0.0050 mol L-1) plus ammonium hydrogencarbonate (1.0 mol L-1) extracted predominantly available inorganic selenate from soil. The formation of a large amount of carbonaceous residue inside the atomizer was avoided with a first pyrolysis step at 600 degreesC assisted by air during 30 s. For 20 muL of soil extracts delivered to the atomizer and calibration by matrix matching, an analytical curve (10.0-100 mug of L-1) with good linear correlation (r = 0.999) between integrated absorbance and analyte concentration was established. The characteristic mass was similar to63 pg of Se, and the lifetime of the tube was similar to750 firings. The limit of detection was 1.6 mug L-1, and the relative standard deviations (n = 12) were typically <4% for a soil extract containing 50 mug of L-1. The accuracy of the determination of Se was checked for soil samples by means of addition/recovery tests. Recovery data of Se added to four enriched soil samples varied from 80 to 90% and indicated an accurate method.

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

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The study of superconducting samples in mesoscopic scale presented a remarkable improvement during the last years. Certainly, such interest is based on the fact that when the size of the samples is close to the order of the temperature dependent coherence length xi(T), and/or the size of the penetration depth lambda(T), there are some significant modifications on the physical properties of the superconducting state. This contribution tests the square cross-section size limit for the occurrence (or not) of vortices in mesoscopic samples of area L-2, where L varies discretely from 1 xi(0) to 8 xi(0).The time dependent Ginzburg-Landau (TDGL) equations approach is used upon taking the order parameter and the local magnetic field invariant along the z-direction. The vortex configurations at the equilibrium can be obtained from the TDGL equations for superconductivity as the system relaxes to the stationary state.The obtained results show that the limit of vortex penetration is for the square sample of size 3 xi(0) x 3 xi(0) in which only a single vortex are allowed into the sample. For smaller specimens, no vortex can be formed and the field entrance into the sample is continuous and the total flux penetration occurs at higher values of H/H-c2(0), where H-c2(T) is the upper critical field. Otherwise, for larger samples different vortices patterns can be observed depending on the sample size. (c) 2007 Elsevier B.V. All rights reserved.

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The problem of a fermion subject to a general mixing of vector and scalar potentials in a two-dimensional world is mapped into a Sturm-Liouville problem. Isolated bounded solutions are also searched. For the specific case of an inversely linear potential, which gives rise to an effective Kratzer potential in the Sturm-Liouville problem, exact bounded solutions are found in closed form. The case of a pure scalar potential with their isolated zero-energy solutions, already analyzed in a previous work, is obtained as a particular case. The behavior of the upper and lower components of the Dirac spinor is discussed in detail and some unusual results are revealed. The nonrelativistic limit of our results adds a new support to the conclusion that even-parity solutions to the nonrelativistic one-dimensional hydrogen atom do not exist. (c) 2004 Elsevier B.V. All rights reserved.

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The problem of a fermion subject to a convenient mixing of vector and scalar potentials in a two-dimensional space-time is mapped into a Sturm-Liouville problem. For a specific case which gives rise to an exactly solvable effective modified Poschl-Teller potential in the Sturm-Liouville problem, bound-state solutions are found. The behaviour of the upper and lower components of the Dirac spinor is discussed in detail and some unusual results are revealed. The Dirac delta potential as a limit of the modified Poschl-Teller potential is also discussed. The problem is also shown to be mapped into that of massless fermions subject to classical topological scalar and pseudoscalar potentials. Copyright (C) EPLA, 2007.

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Exact bounded solutions for a fermion subject to exponential scalar potential in 1 + 1 dimensions are found in closed form. We discuss the existence of zero modes which are related to the ultrarelativistic limit of the Dirac equation and are responsible for the induction of a fractional fermion number on the vacuum.

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This paper investigates the feasibility of using an energy harvesting device tuned such that its natural frequency coincides with higher harmonics of the input to capture energy from walking or running human motion more efficiently. The paper starts by reviewing the concept of a linear resonant generator for a tonal frequency input and then derives an expression for the power harvested for an input with several harmonics. The amount of power harvested is estimated numerically using measured data from human subjects. Assuming that the input is periodic, the signal is reconstructed using a Fourier series before being used in the simulation. It is found that although the power output depends on the input frequency, the choice of tuning the natural frequency of the device to coincide with a particular higher harmonic is restricted by the amount of damping that is needed to maximize the amount of power harvested, as well as to comply with the size limit of the device. It is also found that it is not feasible to tune the device to match the first few harmonics when the size of the device is small, because a large amount of damping is required to limit the motion of the mass.

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

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This work presents a methodology for iron determination in fuel ethanol using a modified carbon paste electrode with 1.10 fenantroline/nafion. The electrochemical parameters were optimized for the proposed system and the voltammetric technique of square wave was employed for iron determination. An accumulation time of 5 minutes, such as a 100 mV of pulse magnitude (E(sw)) and frequency (f) of 25 Hz were used as optimized experimental conditions. The modified carbon paste electrode presented linear dependence of amperometric signal with iron concentration in a work range from 6.0x10(-6) until 2.0x10(-5) mol L(-1) of iron, exhibiting a linear correlation coefficient of 0.9884, a detection limit of 2.4 x10(-6) mol L(-1) (n = 3) and amperometric sensibility of 4.5x10(5) mu A/mol L(-1). Analytical curve method was used for iron determination at a commercial fuel sample. Flame atomic absorption spectroscopy was employed as comparative technique.

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