968 resultados para constant pressure gradient elution


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The present study has attempted to investigate phase inversion and frictional pressure gradients during simultaneous vertical flow of oil and water two-phase through upward and downward pipes. The liquids selected were white oil (44 mPa s viscosity and 860 kg/m3 density) and water. The measurements were made for phase velocities varying from 0 to 1.24 m/s for water and from 0 to 1.87 m/s for oil, respectively. Experiments were carried either by keeping the mixture velocity constant and increasing the dispersed phase fraction or by keeping the continuous phase superficial velocity constant and increasing the dispersed phase superficial velocity. From the experimental results, it is shown that the frictional pressure gradient reaches to its lower value at the phase inversion point in this work. The points of phase inversion are always close to an input oil fraction of 0.8 for upward flow and of 0.75 for downward flow, respectively. A few models published in the literature are used to predict the phase inversion point and to compare the results with available experimental data. Suitable methods are suggested to predict the critical oil holdup at phase inversion based on the different viscosity ratio ranges. Furthermore, the frictional pressure gradient is analyzed with several suitable theoretical models according to the existing flow patterns. The analysis reveals that both the theoretical curves and the experimental data exhibit the same trend and the overall agreement of predicted values with experimental data is good, especially for a high oil fraction.

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A simple, sensitive, and mild method for the determination of amino compounds based on a condensation reaction with 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC-HCI) as the dehydrant with fluorescence detection has been developed. Amines were derivatized to their acidamides with labeling reagent 2-(2-phenyl-1H-phenanthro-[9,10-d]imidazole-1-yl)-acetic acid (PPIA). Studies on derivatization conditions indicated that the coupling reaction proceeded rapidly and smoothly in the presence of a base catalyst in acetonitrile to give the corresponding sensitively fluorescent derivatives with an excitation maximum at lambda(ex) 260nm and an emission maximum at lambda(em) 380nm. The labeled derivatives exhibited high stability and were enough to be efficiently analyzed by high-performance liquid chromatography. Identification of derivatives was carried out by online post-column mass spectrometry (LC/APCI-MS/MS) and showed an intense protonated molecular ion corresponding m/z [MH](+) under APCI in positive-ion mode. At the same time, the fluorescence properties of derivatives in various solvents or at different temperature were investigated. The method, in conjunction with a gradient elution, offered a baseline resolution of the common amine derivatives on a reversed-phase Eclipse XDB-C-8 column. LC separation for the derivatized amines showed good reproducibility with acetonitrile-water as mobile phase. Detection limits calculated from 0.78 pmol injection, at a signal-to-noise ratio of 3, were 3.1-18.2 fmol. The mean intra- and inter-assay precision for all amine levels were < 3.85% and 2.11%, respectively. Excellent linear responses were observed with coefficients of > 0.9996. The established method for the determination of aliphatic amines from real wastewater and biological samples was satisfactory. (c) 2006 Elsevier B.V. All rights reserved.

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A new approach based on microextraction by packed sorbent (MEPS) and reversed-phase high-throughput ultra high pressure liquid chromatography (UHPLC) method that uses a gradient elution and diode array detection to quantitate three biologically active flavonols in wines, myricetin, quercetin, and kaempferol, is described. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (selectivity, linearity, sensitivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters such as the type of sorbent material (C2, C8, C18, SIL, and C8/SCX), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, on the MEPS performance. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250 μL) in five extraction cycle and in a short time period (about 5 min for the entire sample preparation step). Under optimized conditions, excellent linearity View the MathML source(Rvalues2>0.9963), limits of detection of 0.006 μg mL−1 (quercetin) to 0.013 μg mL−1 (myricetin) and precision within 0.5–3.1% were observed for the target flavonols. The average recoveries of myricetin, quercetin and kaempferol for real samples were 83.0–97.7% with relative standard deviation (RSD, %) lower than 1.6%. The results obtained showed that the most abundant flavonol in the analyzed samples was myricetin (5.8 ± 3.7 μg mL−1). Quercetin (0.97 ± 0.41 μg mL−1) and kaempferol (0.66 ± 0.24 μg mL−1) were found in a lower concentration. The optimized MEPSC8 method was compared with a reverse-phase solid-phase extraction (SPE) procedure using as sorbent a macroporous copolymer made from a balanced ratio of two monomers, the lipophilic divinylbenzene and the hydrophilic N-vinylpyrrolidone (Oasis HLB) were used as reference. MEPSC8 approach offers an attractive alternative for analysis of flavonols in wines, providing a number of advantages including highest extraction efficiency (from 85.9 ± 0.9% to 92.1 ± 0.5%) in the shortest extraction time with low solvent consumption, fast sample throughput, more environmentally friendly and easy to perform.

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A novel analytical approach, based on a miniaturized extraction technique, the microextraction by packed sorbent (MEPS), followed by ultrahigh pressure liquid chromatography (UHPLC) separation combined with a photodiode array (PDA) detection, has been developed and validated for the quantitative determination of sixteen biologically active phenolic constituents of wine. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (linearity, sensitivity, selectivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters on the MEPS performance such as the type of sorbent material (C2, C8, C18, SIL, and M1), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, were studied. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250 μL) in five extraction cycle and in a short time period (about 5 min for the entire sample preparation step). The wine bioactive phenolics were eluted by 250 μL of the mixture containing 95% methanol and 5% water, and the separation was carried out on a HSS T3 analytical column (100 mm × 2.1 mm, 1.8 μm particle size) using a binary mobile phase composed of aqueous 0.1% formic acid (eluent A) and methanol (eluent B) in the gradient elution mode (10 min of total analysis). The method gave satisfactory results in terms of linearity with r2-values > 0.9986 within the established concentration range. The LOD varied from 85 ng mL−1 (ferulic acid) to 0.32 μg mL−1 ((+)-catechin), whereas the LOQ values from 0.028 μg mL−1 (ferulic acid) to 1.08 μg mL−1 ((+)-catechin). Typical recoveries ranged between 81.1 and 99.6% for red wines and between 77.1 and 99.3% for white wines, with relative standard deviations (RSD) no larger than 10%. The extraction yields of the MEPSC8/UHPLC–PDA methodology were found between 78.1 (syringic acid) and 99.6% (o-coumaric acid) for red wines and between 76.2 and 99.1% for white wines. The inter-day precision, expressed as the relative standard deviation (RSD%), varied between 0.2% (p-coumaric and o-coumaric acids) and 7.5% (gentisic acid) while the intra-day precision between 0.2% (o-coumaric and cinnamic acids) and 4.7% (gallic acid and (−)-epicatechin). On the basis of analytical validation, it is shown that the MEPSC8/UHPLC–PDA methodology proves to be an improved, reliable, and ultra-fast approach for wine bioactive phenolics analysis, because of its capability for determining simultaneously in a single chromatographic run several bioactive metabolites with high sensitivity, selectivity and resolving power within only 10 min. Preliminary studies have been carried out on 34 real whole wine samples, in order to assess the performance of the described procedure. The new approach offers decreased sample preparation and analysis time, and moreover is cheaper, more environmentally friendly and easier to perform as compared to traditional methodologies.

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Our goal in this paper is to extend previous results obtained for Newtonian and secondgrade fluids to third-grade fluids in the case of an axisymmetric, straight, rigid and impermeable tube with constant cross-section using a one-dimensional hierarchical model based on the Cosserat theory related to fluid dynamics. In this way we can reduce the full threedimensional system of equations for the axisymmetric unsteady motion of a non-Newtonian incompressible third-grade fluid to a system of equations depending on time and on a single spatial variable. Some numerical simulations for the volume flow rate and the the wall shear stress are presented.

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An HPLC with SPE method has been developed for analysis of constituents in rat blood after oral administration of the extract of Acanthopanax senticosus (ASE). The plasma sample was prepared by SPE method equipped with Oasis HLB cartridge (3cc, 60 mg). The analysis was performed on a Dikma Diamonsil RP(18) column (4.6 mmx150 mm, 5 microm) with the gradient elution of solvent A (ACN) and solvent B (0.1% aqueous phosphoric acid, v/v) and the detection wavelength was set at 270 nm. The calibration curve was linear over the range of 0.156-15.625 microg/mL. The LOD was 60 ng/mL. The intraday precision was less than 5.80%, and the interday precision was less than 6.0%. The recovery was (87.30 +/- 1.73)%. As a result, 19 constituents were detected in rat plasma after oral administration of the ASE, including 11 original compounds in ASE and eight metabolites, and three of the metabolites originated from syringin in ASE. Six constituents were identified by comparing with the corresponding reference compounds.

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A systematic study was undertaken on the combustion and thermal decomposition of pelletized Ammonium Perchlorate (AP) to investigate the effects of pelletizing pressure and dwell time. At constant pressure, increasing the dwell time results in an increase in the burning rate up to a maximum and thereafter decreases it. The dwell time required for the pellets to have maximum burning rate is a function of pressure. The maximum burning rate is the same for all the pressures used and is also unaffected by increasing, to the range 90-250 μ, the particle size of AP used. In order to explain the occurrence of a maximum in burning rate, pellets were examined for their thermal sensitivities, physical nature and the changes occurring during pelletization with dwell time and pressure. The variations are argued in terms of increasing density, formation of defects such as dislocations leading to an increase in the number of reactive sites, followed by their partial annihilation at longer dwell times due to flow of material during pelletization.

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Experimental results are presented on the lateral growth of turbulent spots in a series of flows with favorable pressure gradients. It is shown that the wedge angle increases slowly with the Reynolds number and that a favorable pressure gradient inhibits the growth of turbulent spots and, in general, results in a nonlinear turbulent wedge. As soon as the pressure gradient decreases to the point where the flow becomes supercritical, however, spot growth increases rapidly and the associated turbulent wedge becomes linear.

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Investigations have been carried out of some aspects of the fine-scale structure of turbulence in grid flows, in boundary layers in a zero pressure gradient and in a boundary layer in a strong favourable pressure gradient leading to relaminarization. Using a narrow-band filter with suitable mid-band frequencies, the properties of the fine-scale structure (appearing as high frequency pulses in the filtered signal) were analysed using the variable discriminator level technique employed earlier by Rao, Narasimha & Badri Narayanan (1971). It was found that, irrespective of the type of flow, the characteristic pulse frequency (say Np) defined by Rao et al. was about 0·6 times the frequency of the zero crossings. It was also found that, over the small range of Reynolds numbers tested, the ratio of the width of the fine-scale regions to the Kolmogorov scale increased linearly with Reynolds number in grid turbulence as well as in flat-plate boundarylayer flow. Nearly lognormal distributions were exhibited by this ratio as well as by the interval between successive zero crossings. The values of Np and of the zero-crossing rate were found to be nearly constant across the boundary layer, except towards its outer edge and very near the wall. In the zero-pressure-gradient boundary-layer flow, very near the wall the high frequency pulses were found to occur mostly when the longitudinal velocity fluctuation u was positive (i.e. above the mean), whereas in the outer part of the boundary layer the pulses more often occurred when u was negative. During acceleration this correlation between the fine-scale motion and the sign of u was less marked.

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This is the first report on the study carried out on high-pressure free-radical initiated oxidated copolymerization of styrene (STY) with alpha-methylstyrene (AMS) at various temperatures (45-65degreesC) at constant pressure (100 psi) and then at various pressures (50-300 psi) keeping the temperature (50degreesC) constant. The compositions of the copolyperoxides obtained from the H-1 NMT spectra were utilized to determine the reactivity ratios of the monomers. The reactivity ratios indicate that STY forms an ideal copolyperoxide with AMS and the copolyperoxide is richer in AMS. The effect of temperature and oxygen pressure in the reactivity ratios of the monomers was studied. The rates of copolymerization (R-p) were used to determine the overall activation energies (E-a) and activation volume (DeltaV(#)) of copolymerization. The unusually higher values of the DeltaV(#) may be due to the pressurizing fluid oxygen which itself is a reactant in the copolymerization, the side reactions, and the chain-transfer reactions occuring during copolymerizations.

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We consider here the detailed application of a model Reynolds stress equation (Narasimha 1969) to plane turbulent wakes subjected to pressure gradients. The model, which is a transport equation for the stress exhibiting relaxation and diffusion, is found to be consistent with the observed response of a wake to a nearly impulsive pressure gradient (Narasimha & Prabhu 1971). It implies in particular that a wake can be in equilibrium only if the longitudinal strain rate is appreciably less than the wake shear. We then describe a further series of experiments, undertaken to investigate the range of validity of the model. It is found that, with an appropriate convergence correction when necessary, the model provides excellent predictions of wake development under favourable, adverse and mixed pressure gradients. Furthermore, the behaviour of constant-pressure distorted wakes, as reported by Keffer (1965, 1967), is also explained very well by the model when account is taken of the effective flow convergence produced by the distortion. In all these calculations, only a simple version of the model is used, involving two non-dimensional constants both of which have been estimated from a single relaxation experiment.

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We investigate the variation of the gas and the radiation pressure in accretion disks during the infall of matter to the black hole and its effect to the flow. While the flow far away from the black hole might be non-relativistic, in the vicinity of the black hole it is expected to be relativistic behaving more like radiation. Therefore, the ratio of gas pressure to total pressure (beta) and the underlying polytropic index (gamma) should not be constant throughout the flow. We obtain that accretion flows exhibit significant variation of beta and then gamma, which affects solutions described in the standard literature based on constant beta. Certain solutions for a particular set of initial parameters with a constant beta do not exist when the variation of beta is incorporated appropriately. We model the viscous sub-Keplerian accretion disk with a nonzero component of advection and pressure gradient around black holes by preserving the conservations of mass, momentum, energy, supplemented by the evolution of beta. By solving the set of five coupled differential equations, we obtain the thermo-hydrodynamical properties of the flow. We show that during infall, beta of the flow could vary up to similar to 300%, while gamma up to similar to 20%. This might have a significant impact to the disk solutions in explaining observed data, e.g. super-luminal jets from disks, luminosity, and then extracting fundamental properties from them. Hence any conclusion based on constant gamma and beta should be taken with caution and corrected. (C) 2011 Elsevier B.V. All rights reserved.

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Reliable bench mark experimental database in the separated hypersonic flow regime is necessary to validate high resolution CFD codes. In this paper we report the surface pressure and heat transfer measurements carried out on double cones (first cone semi-apex angle = 15, 25 deg.; second cone semi-apex angle= 35, 68 deg.) at hypersonic speeds that will be useful for CFD code validation studies. The surface pressure measurements are carried out at nominal Mach number of 8.35 in the IISc hypersonic wind tunnel. On the other hand the surface heat transfer measurements are carried out at a nominal Mach number of 5.75 in the IISc hypersonic shock tunnel. The flow separation point on the first cone, flow reattachment on the second cone and the wild fluctuation of the transmitted shock on the second cone surface (25/68 deg. double cone) in the presence of severe adverse pressure gradient are some of the flow features captured in the measurements. The results from the CFD studies indicate good agreement with experiments in the attached flow regime while considerable differences are noticeable in the separated flow regime.

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Laminar separation bubbles are thought to be highly non-parallel, and hence global stability studies start from this premise. However, experimentalists have always realized that the flow is more parallel than is commonly believed, for pressure-gradient-induced bubbles, and this is why linear parallel stability theory has been successful in describing their early stages of transition. The present experimental/numerical study re-examines this important issue and finds that the base flow in such a separation bubble becomes nearly parallel due to a strong-interaction process between the separated boundary layer and the outer potential flow. The so-called dead-air region or the region of constant pressure is a simple consequence of this strong interaction. We use triple-deck theory to qualitatively explain these features. Next, the implications of global analysis for the linear stability of separation bubbles are considered. In particular we show that in the initial portion of the bubble, where the flow is nearly parallel, local stability analysis is sufficient to capture the essential physics. It appears that the real utility of the global analysis is perhaps in the rear portion of the bubble, where the flow is highly non-parallel, and where the secondary/nonlinear instability stages are likely to dominate the dynamics.

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Scaling of pressure spectrum in zero-pressure-gradient turbulent boundary layers is discussed. Spatial DNS data of boundary layer at one time instant (Re-theta = 4500) are used for the analysis. It is observed that in the outer regions the pressure spectra tends towards the -7/3 law predicted by Kolmogorov's theory of small-scale turbulence. The slope in the pressure spectra varies from -1 close to the wall to a value close to -7/3 in the outer region. The streamwise velocity spectra also show a -5/3 trend in the outer region of the flow. The exercise carried out to study the amplitude modulation effect of the large scales on the smaller ones in the near-wall region reveals a strong modulation effect for the streamwise velocity, but not for the pressure fluctuations. The skewness of the pressure follows the same trend as the amplitude modulation coefficient, as is the case for the velocity. In the inner region, pressure spectra were seen to collapse better when normalized with the local Reynolds stress (-(u'v') over bar) than when scaled with the local turbulent kinetic energy (q(2) = (u'(2)) over bar + (v'(2)) over bar + (w'(2)) over bar)