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α-Acetoxy acid methyl esters are prepared in excellent yields by treating aliphatic α-acetoxy dimethyl acetals with trichloroisocyanuric acid in DMF. 相似文献
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Benincasa C Maiuolo L Mazzotti F Perri E Sindona G Urso E 《Journal of mass spectrometry : JMS》2004,39(1):61-65
A method is presented which allows the identification and assay of a nucleoside in the presence of other analogues and homologues. The method is based on the conventional multiple reaction monitoring approach performed on the [M + H]+ ions of wild-type and modified nucleosides produced by the turbo ionspray ionization method on a triple-quadrupole mass spectrometer. The accuracy of the quantitative determination relies on the evaluation of a response factor rho, which takes into account the kinetics of dissociation of the parent ions into the protonated [B + 2H]+ nucleobase ions. The evaluation of the absolute concentration of each analyte in the examined mixture does not require any previous chromatographic separation. 相似文献
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T. Benincasa 《Numerical Functional Analysis & Optimization》2013,34(3-4):199-213
The paper presents a proof of the convergence for an iterative scheme of fractional steps type associated to the phase-field transition system (a nonlinear parabolic system) with non-homogeneous Cauchy–Neumann boundary conditions. The advantage of such method consists in simplifying the numerical computation necessary to be done in order to approximate the solution of a nonlinear parabolic system. On the basis of this approach, a numerical algorithm in the two dimensional case is introduced and an industrial implementation is made. 相似文献
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A peak breakthrough technique is described and evaluated for measuring the void volume of field-flow fractionation (FFF) channels, particularly those used for flow FFF. This technique uses a high-molecular-mass macromolecular or particulate probe that can be displaced rapidly by flow through the FFF channel with minimal transverse diffusion. The particles that emerge first are those carried through the entire length near the channel centerline at the apex of the parabolic flow profile. These particles generate a sharp breakthrough profile. The measured breakthrough time is two thirds of the void time, thus making it possible to calculate both the void time and the associated void volume. This method, although applicable to all FFF channels (and capable of extension to open tubes), is particularly useful for flow FFF because conventional low-molecular-mass void probes can diffuse into the permeable walls and thus distort void measurements. The theoretical basis of the breakthrough technique and an explanation for the sharpness of the breakthrough front are given. A method for compensating for deviations from perfect sharpness is developed in which the breakthrough time is identified with the time needed to reach 85-88% of the breakthrough peak maximum. Preliminary experimental results are shown using various protein probes in four different FFF channel systems. 相似文献
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Menéndez FE Espina Aránzazu Trobajo Camino García José R. Rodríguez Julio 《Journal of inclusion phenomena and macrocyclic chemistry》1993,15(3):215-230
Journal of Inclusion Phenomena and Macrocyclic Chemistry - The intercalation reactions betweenn-alkylamines and α-titanium phosphate in aqueous media have been investigated. The compounds with... 相似文献
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Sapochak LS Benincasa FE Schofield RS Baker JL Riccio KK Fogarty D Kohlmann H Ferris KF Burrows PE 《Journal of the American Chemical Society》2002,124(21):6119-6125
We present direct evidence for stable oligomers in vacuum-deposited thin films of zinc(II) bis(8-hydroxyquinoline) (Znq(2)). The tetramer [(Znq(2))(4)] is the energetically favored configuration in both the single crystal and the vacuum-deposited thin film. Oligomerization leads to distinct, symmetry-driven differences between the electronic states in Znq(2) and those in the archetypal organic electroluminescent molecule tris(8-hydroxyquinoline) aluminum (Alq(3)). In the case of the Znq(2) tetramer, symmetry leads to an extended network of overlapping pyridyl and phenolato moieties in the solid film. Analysis of the electronic structure of (Znq(2))(4) calculated by ab initio Hartree-Fock (HF) methods reveals a localization and energy shift of high-lying occupied and low-lying unoccupied states on symmetry related ligands located on opposite sides of the supramolecular structure resulting in a dipole moment for (Znq(2))(4) tetramer close to zero. The optimal pi-overlap pathways, altered charge distributions, and extended electronic states of tetrameric Znq(2) may be expected to enable low operating voltage organic light-emitting devices (OLEDs) based on Znq(2). We present preliminary evidence that the operating voltage of (Znq(2))(4)-based OLEDs is indeed lower than that of identical devices made with Alq(3). Strategic substitution of 8-hydroxyquinoline ligands and control of the structural symmetry of the corresponding metal chelates may offer a route to high efficiency and low operating voltage small molecule OLEDs. 相似文献
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The anti‐self‐dual Yang‐Mills equations are known to have reductions to many integrable differential equations. A general Bäcklund transformation (BT) for the anti‐self‐dual Yang‐Mills (ASDYM) equations generated by a Darboux matrix with an affine dependence on the spectral parameter is obtained, together with its Bianchi permutability equation. We give examples in which we obtain BTs of symmetry reductions of the ASDYM equations by reducing this ASDYM BT. Some discrete integrable systems are obtained directly from reductions of the ASDYM Bianchi system. 相似文献
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The coupling of the flow field-flow fractionation (FlFFF) to differential refractive index (DRI) and multiangle laser light scattering (LS) detectors is a powerful tool for characterizing charged polysaccharides such as alginate. However, the correct interpretation of the experimental results and extrapolation of meaningful molecular parameters by using an analytical tool with such a level of complexity requires improvement of the knowledge of the alginate behavior in the channel and careful optimization of the operating conditions. Therefore, the influence of the critical operating parameters, such as crossflow rate, carrier composition and concentration, and sample load, on the alginate retention was carefully evaluated. Combined information obtained simultaneously by DRI and LS detectors over the wide range of the crossflow rate, carrier liquid concentration, and injected amount, allowed to set the appropriate combination of optimal parameters. It was found that the crossflow rate of 0.25 mL/min, carrier solution containing 5x10(-2 )mol/L ammonium or sodium chloride, and 50-100 microg of injected sample mass were necessary to achieve complete separation and determination of the meaningful molecular characteristics. The values of the weight-average hydrodynamic radius (R(Hw)), radius of gyration (R(G)), and molar mass (M), obtained under the optimal conditions were in good agreement to those found for alginates in the literature. 相似文献
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The effects of carrier ionic strength and electrolyte composition on the retention of poly(ethylene oxide) in aqueous flow field-flow fractionation have been investigated in this work. The study shows retention to be particularly sensitive to the presence of salts, as well as to the nature of the cation. Specifically, retention effects due to sample load are found to be very different in solutions containing potassium salts compared to those observed in solutions of the corresponding sodium salts. In a potassium-containing medium, the dependence of retention on sample mass is similar to that found previously for polyelectrolytes. This effect, which is particularly prominent for samples of low molecular mass, can be attributed to specific interactions between cation and polymer. 相似文献