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151.
Laura Rubio María Leticia Oca Luis Sarabia Inmaculada García María Cruz Ortiz 《Journal of Chemometrics》2016,30(2):58-69
Internal standards can be added at different stages of an analytical procedure. When they are added at the beginning of a multiresidue method and their behavior is not exactly the same as that of the analytes, the intended correction for small variations within the analytical process could not be achieved. Because of this, in the present work, the use of d ‐optimal designs together with desirability functions is proposed to state the experimental response under study. The overall desirability function used relates two analytical criteria: to assess a similar chemical behavior of each analyte in relation to its internal standard and to avoid a significant reduction of the absolute peak area of the internal standards. This strategy has been applied to the analysis of the effect of four factors related to the extraction and purification steps of six tranquillizers and a β‐blocker from pig muscle analyzed by liquid chromatography–tandem mass spectrometry. The effect of those factors has been evaluated by means of an ad hoc d ‐optimal design consisting of only 11 experiments. The resulting levels of the four factors that enable to achieve the greatest overall desirability have also been compared with those obtained when either the standardized or absolute peak area has been considered as response. Differences in both the significant factors and their optimum levels have been observed. It is noticeable that the experimental effort necessary to study the effect of the factors has been reduced by more than 50% thanks to the d ‐optimal design. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
152.
The determination of rosiglitazone in dietary supplements by direct analysis in real-time mass spectrometry normally provides low repeatability. The [M+H]+ signal sharply decreased in the presence of strong-base and weak-acid ionic compounds because rosiglitazone decomposition occurred due to the hydrolysis of strong-base and weak-acid anions. The repeatability was improved and the influence of ionic compounds was minimized by the use of pioglitazone as an internal standard. Orbitrap mass spectrometry was used to provide high resolution in which isotopic interferences from M?+?1 of pioglitazone upon M of rosiglitazone were eliminated. This approach was used to determine rosiglitazone in tablet and dietary supplements in 1?min per sample. 相似文献
153.
Marcin Wieczorek Anna Tobiasz Danuta Dudek-Adamska Stanisław Walas Paweł Kościelniak 《Analytical letters》2017,50(14):2279-2291
Selenium was determined in serum, hair, and tobacco by inductively coupled plasma-mass spectrometry using 77Se, 78Se, and 82Se. The set of standards method (SSM) and the standard addition method (SAM) were applied to calibration with and without the use of internal standards (72Ge and 103Rh). In addition, the usefulness of the dynamic reaction cell (DRC) with methane as the reaction gas was characterized. The results obtained in different conditions were evaluated in terms of precision and accuracy. It was demonstrated theoretically and experimentally that an internal standard is a potential source of systematic errors as it can be influenced multiplicatively and additively by its own interferents (independently of selenium). Furthermore, it was shown that—against common opinion—an internal standard can fail in elimination of chemical interference effects influencing selenium and in increasing of precision of selenium determinations. The DRC was shown to be effective in the elimination of additive effects, although the results obtained by both SSM and SAM with DRC were systematically positively erroneous. Finally, selenium was determined accurately in each examined sample when SAM was applied to calibration, and signals were measured either for 82Se without the use of the DRC, or for 77Se or 78Se with the use of the DRC. In addition, it has also been shown that samples should be diluted prior to analysis to the greatest acceptable extent. 相似文献
154.
155.
In this paper, a theoretical investigation of nonlinear vibrations of a 2 degrees of freedom system when subjected to saturation
is studied. The method has been especially applied to a system that consists of a DC motor with a nonlinear controller and
a harmonic forcing voltage. Approximate solutions are sought using the method of multiple scales. It is shown that the closed-loop
system exhibits different response regimes. The nature and stability of these regimes are studied and the stability boundaries
are obtained. The effects of the initial conditions on the response of the system have also been investigated. Furthermore,
the second-order solution is presented and the corresponding results are compared with those of the first-order solution.
It is shown that by increasing the amplitude of the excitation voltage, the higher-order term in the solution becomes significant
and causes a drift in the response. In order to verify the obtained theoretical results, they are compared with the corresponding
numerical results. Good agreement between the two sets of results is observed. 相似文献
156.
Flight tests of modern high-performance fighter aircraft reveal the presence of limit cycle oscillation (LCO) responses for aircraft with certain external store configurations. Conventional linear aeroelastic analysis predicts flutter for conditions well beyond the operational envelope, yet these store-induced LCO responses occur at flight conditions within the flight envelope. Several nonlinear sources may be present, including aerodynamic effects such as flow separation and shock-boundary layer interaction and structural effects such as stiffening, damping, and system kinematics. No complete theory has been forwarded to accurately explain the mechanisms responsible. This research examines a two degree-of-freedom aeroelastic system which possesses kinematic nonlinearities and a strong nonlinearity in pitch stiffness. Nonlinear analysis techniques are used to gain insight into the characteristics of the behavior of the system. Numerical simulation is used to verify and validate the analysis. It is found that when system damping is low, the system clearly exhibits nonlinear interaction between aeroelastic modes. It is also shown that although certain applied forcing conditions may appear negligible, these same forces produce large amplitude LCOs under specific realizable circumstances. 相似文献
157.
Kaori Kobayashi Takanori Matsui Shozo Tsunekawa 《Journal of Molecular Spectroscopy》2011,269(2):242-247
The trans-ethyl methyl ether molecule has three low-lying torsional modes, that is, two inequivalent methyl internal rotations and an asymmetric skeletal torsion. The internal rotations of the CCH3 and OCH3 methyl rotors and the skeletal torsion correspond to the vibrational modes, ν28, ν29 and ν30 respectively. In this study, the microwave absorption spectrum in the ν28 = 1 CCH3 torsional state was analyzed for the first time. Nine hundred fifty seven lines up to J = 48 and K = 4 were assigned, and the rotational, centrifugal distortion and internal rotational tunneling parameters were determined with the use of a tunneling matrix formalism. By combining the present results on the ν28 = 1 torsional state with those for the ν30 = 1 skeletal torsional state and the ν29 = 1 OCH3 torsional state, torsional couplings are estimated in order to understand quantitatively the inverted A/E sequence patterns observed for those three excited torsional states. 相似文献
158.
The leakage current behaviours of polycrystalline BiFeO3 thin films are investigated by using both conductive atomic force microscopy and current-voltage characteristic measurements. The local charge transport pathways are found to be located mainly at the grain boundaries of the films. The leakage current density can be tuned by changing the post-annealing temperature, the annealing time, the bias voltage and the light illumination, which can be used to improve the performances of the ferroelectric devices based on the BiFeO3 films. A possible leakage mechanism is proposed to interpret the charge transports in the polycrystalline BiFeO3 films. 相似文献
159.
The catalytic activity of ortho‐palladated [Pd{C6H2(CH2CH2NH2)‐(OMe)2,3,4}(m‐Br)]2, a complex of homoveratrylamine in the copper‐free Sonogashira coupling reaction has been investigated. This complex is a catalyst that is efficient, stable and non‐sensitive to air and moisture in the Sonogashira reaction. In this homogeneous catalytic system, various aryl halides were efficiently coupled with phenylacetylene in mostly moderate to good yields in N‐methylpyrrolidone at 100 °C under copper‐free conditions. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
160.
In the paper, a cross‐flow fan in refrigerant operating condition is systematically simulated using user‐defined functions. Three‐dimensional simulations are acquired with Navier–Stokes equations coupled with k–ε turbulence model, and internal flow characteristics of an indoor split‐type air conditioner are obtained, which is mainly composed of cross‐flow fan and heat exchanger. It has systematically been simulated in the isothermal flow condition that the performance of cross‐flow fan may be reduced easily with dry or humid air, and in the refrigerant operating condition in which user‐defined functions are applied to the humid air, considered as a mixture of dry air and vapor. A density‐modulated function is adopted to deal with the condensation of the vapor at the heat‐transfer region approximately. The results show flow mechanism of the two gas‐phase flow, including phase‐vary process. The distribution of the parameters is not uniform at the inlet of the machine, the intensity and position of pressure and velocity vary along the axial direction of the fan, the distribution of vapor volume fraction and turbulent intensity in heat‐transfer region is obtained, and the external characteristic data of the indoor machine are obtained and analyzed. Compared with the experimental data, the calculated characteristic curves and designed parameters are on target. © British Crown Copyright 2010/MOD. Reproduced with permission. Published by John Wiley & Sons, Ltd. 相似文献