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1.
Valdemar I. Esteves Susana S.F. Lima Diana L.D. Lima Armando C. Duarte 《Analytica chimica acta》2004,513(1):163-167
The simultaneous separation and determination of organic acids in several samples of white and red Port wines was performed by capillary zone electrophoresis using indirect UV detection with 2,6-pyridinedicarboxylic acid as a background electrolyte buffer. Operational parameters like migration time, temperature, voltage and capillary length were optimized. Sixteen samples of red wine and four samples of white wine were used to analyze for tartaric, malic, lactic, succinic and acetic acids using glyoxylic acid as the internal standard. The method is rapid, sensitive and quantitative, and time-consuming sample preparation, such as solid-phase extraction or liquid-liquid extraction procedure, is not required. 相似文献
2.
Rodolfo G. Fiorot João F. Allochio Filho Thieres M.C. Pereira Valdemar Lacerda Jr. Reginaldo B. dos Santos Wanderson Romão Sandro J. Greco 《Tetrahedron letters》2014
A clean, efficient and facile one-pot protocol was developed for the synthesis of a series of new aminonaphthoquinones derived from 2-hydroxy-1,4-naphthoquinone (lawsone) by three-component Mannich reaction using catalytic amount of p-TsOH in CH3CN, at room temperature. At the present work, we improved the yield and significantly reduced the reaction time for several Mannich reactions with different amine and aromatic aldehydes using a non-expensive, mild catalyst and suitable solvent. 相似文献
3.
Renzo C. Silva Giovanna F. Carneiro Lúcio L. Barbosa Valdemar Lacerda Jr. Jair C. C. Freitas Eustáquio V. R. de Castro 《Magnetic resonance in chemistry : MRC》2012,50(2):85-88
Low‐field 1H NMR was used in this work for the analysis of mixtures involving crude oils and water. CPMG experiments were performed to determine the transverse relaxation time (T2) distribution curves, which were computed by the inverse Laplace transform of the echo decay data. The instrument's ability of quantifying water and petroleum in biphasic mixtures following different methodologies was tested. For mixtures between deionized water and petroleum, one achieved excellent results, with root mean squared error of cross‐validation (RMSECV) of 0.8% for a regression between the water content (wt %) and the relative area of the water peak in the T2 distribution curve, or a standard deviation of 0.9% for the relationship between the water content and the relative water peak area, corrected by the relative hydrogen index of the crude. In the case of biphasic mixtures of Mn2+‐doped water and crude oils, the best result of RMSECV = 1.6% was achieved by using the raw magnetization decay data for a partial least squares regression. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
4.
Mauricio Gomes Constantino Valdemar Lacerda Júnior Gil Valdo Jos Da Silva 《Journal of heterocyclic chemistry》2003,40(2):369-371
A new and efficient 2‐step synthesis of 3‐hydroxychromone is described. Commercially available chromone is converted to the corresponding epoxide which is rearranged with niobium pentachloride to 3‐hydroxychromone in 61% overall yield. 相似文献
5.
Bain AD Baron M Burger SK Kowalewski VJ Rodríguez MB 《The journal of physical chemistry. A》2011,115(33):9207-9216
Cyclohexane is an extremely flexible molecule that oscillates, at room temperature, between two clearly distinct and extreme conformations that cannot be distinguished at room temperature; so much so that the NMR spectrum is a single line that includes all 12 protons be they axial or equatorial. This raises the interesting question as to what happens when there are equal substituents at the 1 and 4 carbon atoms of the ring. Therefore substitution in the 1,4-positions in the cyclohexane ring has been the subject of considerable interest because some form of interconversion between extreme conformations could lead to the existence of a rather unusual behavior. To study this problem, the interconversion in (di- or tetra-1,4)-substituted six-membered cyclohexane-type rings, trans-1,4-dibromo-1,4-dicyanocyclohexane, was found to be a particularly suitable candidate. Although X-ray diffraction studies on the crystalline solid found the molecule to be centrosymmetric, it still shows a significant dipole moment μ in solution, as determined with a procedure that leads to the vapor phase values of μ. Furthermore, the low magnetic field proton NMR spectrum at ambient temperature appears as a single line, a situation that changes with increasing field intensity and different solvents. Both these effects are attributed to dynamics, because small distortions can easily disrupt the exact cancellation of the individual dipoles (which are quite strong) associated with each end of the molecule. The molecule can exist in two forms, with both the bromines in an axial geometry or both in an equatorial position. Interconversion between these forms is observed, as in the parent cyclohexane. The single NMR line observed at low magnetic fields is due to fast exchange and requires that the two forms have roughly equal populations. Spectra obtained at low temperature confirm this, and variable-temperature studies allow measurement of the rates, leading to an enthalpy of activation of 62 kJ mol(-1). More details of the interconversion are provided by some new calculation methods. Even for a relatively small molecule like this, calculation of a full potential energy surface is prohibitive. However, methods are now available to follow the molecule along the reaction coordinate in quite an efficient way. The results of these calculations lead to an extremely detailed picture of chair-chair interconversion in a di- and tetrasubstituted six-membered ring of the cyclohexane family. 相似文献
6.
We consider a linear steady-state eddy-current problem for a magnetic field in a bounded domain. The boundary consists of two parts: reachable with prescribed Cauchy data and unreachable with no data on it. We design an iterative (Landweber type) algorithm for solution of this problem. At each iteration step two auxiliary mixed well-posed boundary value problems are solved. The analysis of temporary problems is performed in suitable function spaces. This creates the basis for the convergence argument. The theoretical results are supported with numerical experiments. 相似文献
7.
Roberta C. Salles Valdemar Lacerda Jr Adilson Beatriz Felicia M. Ito Reginaldo B. dos Santos Sandro J. Greco Eustáquio V. R. de Castro Dênis P. de Lima 《Magnetic resonance in chemistry : MRC》2010,48(5):409-415
Bioactive cage‐like polycyclic compounds have attracted the attention of several research groups because of their unique appearance and their biological activities. Their structures were established on the basis of 1H NMR and 13C NMR spectroscopic data. The 1H and 13C signal assignments and most homonuclear hydrogen coupling constants were assigned by use of techniques such as 1D 1H and 13C NMR and 2D gCOSY, non‐edited gHSQC and gHMBC. The gNOESY experiments proved the endo‐stereochemistry. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
8.
Bodnar Taras Okhrin Yarema Vitlinskyy Valdemar Zabolotskyy Taras 《Computational Management Science》2018,15(2):297-317
Computational Management Science - In the paper we consider two types of utility functions often used in portfolio allocation problems, i.e. the exponential utility and the quadratic utility. We... 相似文献
9.
Mauricio Gomes Constantino Valdemar Lacerda Júnior Paulo Roberto Invernize Luiz Carlos da Silva Filho Gil Valdo José da Silva 《合成通讯》2013,43(20):3529-3539
Abstract The behavior of several epoxides when treated with NbCl5 was studied. In general, the studied epoxides reacted rapidly with NbCl5, giving, in most cases, more than one product (chlorohydrins, products containing solvent residues, as well as rearrangement products). A detailed study was performed to verify the effects of the temperature (rt, 0°C, or ?78°C) and of the NbCl5 molar concentration on the composition of the products, yield, and time required for the reactions. 相似文献
10.
When using capillary electrophoresis with a diode array detector, the wavelength at maximum absorbance is often chosen to quantify a given analyte. However, the background noise for every wavelength should be taken into account as it is by maximising the signal to noise ratio that the lowest limit of detection will be obtained. Here, we proposed an algorithm allowing to correct an electropherogram from its background absorption and to estimate the background noise. Applying it to all the electropherograms obtained in each wavelength channel allows obtaining the background noise as a function of the wavelength, which can be used to calculate the signal to noise ratio. This not only allows selecting the best wavelength to maximise the limit of detection of a given analyte, but also to generate a noise normalised base peak electropherogram (nn-BPE). It is shown that the noise normalised base peak electropherograms substantially improve the peaks visualisation. The algorithm is part of a graphic user interface that runs under MatLab environment; it does not require any programming knowledge and is freely available. 相似文献