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981.
Stenger Fernanda Cristina Cechinel-Filho Valdir Meyre-Silva Christiane Bresolin Tania Mari Belle Rodrigues Clvis Antonio 《Chromatographia》2009,69(2):183-187
Chitosan was modified with lauroyl chloride to prepare a solid support for the application of matrix solid-phase dispersion (MSPD) for the extraction of flavonoids from the medicinal plant Aleurites moluccana. The laurylchitosan prepared by the homogenous and heterogeneous method, was characterized using analytical methods such as potentiometric titration and infrared spectroscopy. The hydrophobic properties were studied by naphthalene incorporation. The MSPD performance was evaluated by extraction of swertisin and 2″-O-rhamnosylswertisin from the leaves of A. moluccana. 相似文献
982.
Maria Paula Campello Marina Balbina Isabel Santos Přemysl Lubal Radek Ševčík Romana Ševčíková 《Helvetica chimica acta》2009,92(11):2398-2413
The protonation constants of 2‐[4,7,10‐tris(phosphonomethyl)‐1,4,7,10‐tetraazacyclododecan‐1‐yl]acetic acid (H7DOA3P) and of the complexes [Ln(DOA3P)]4? (Ln=Ce, Pr, Sm, Eu, and Yb) have been determined by multinuclear NMR spectroscopy in the range pD 2–13.8, without control of ionic strength. Seven out of eleven protonation steps were detected (pK =13.66, 12.11, 7.19, 6.15, 5.77, 2.99, and 1.99), and the values found compare well with the ones recently determined by potentiometry for H7DOA3P, and for other related ligands. The overall basicity of H7DOA3P is higher than that of H4DOTA and trans‐H6DO2A2P but lower than that of H8DOTP. Based on multinuclear‐NMR spectroscopy, the protonation sequence for H7DOA3P was also tentatively assigned. Three protonation constants (pKMHL, pKMH2L, and pKMH3L) were determined for the lanthanide complexes, and the values found are relatively high, although lower than the protonation constants of the related ligand (pK , pK , and pK ), indicating that the coordinated phosphonate groups in these complexes are protonated. The acid‐assisted dissociation of [Ln(DOA3P)]4? (Ln=Ce, Eu), in the region cH+=0.05–3.00 mol dm?3 and at different temperatures (25–60°), indicated that they have slightly the same kinetic inertness, being the [Eu(H2O)9]3+ aqua ion the final product for europium. The rates of complex formation for [Ln(DOA3P)]4? (Ln=Ce, Eu) were studied by UV/VIS spectroscopy in the pH range 5.6–6.8. The reaction intermediate [Eu(DOA3P)]* as ‘out‐of‐cage’ complex contains four H2O molecules, while the final product, [Eu(DOA3P)]4?, does not contain any H2O molecule, as proved by steady‐state/time‐resolved luminescence spectroscopy. 相似文献
983.
Manuel A.V. Ribeiro da Silva Ana I.M.C. Lobo Ferreira Joana I.T.A. Cabral Ana Filipa L.O.M. Santos Ana Rita G. Moreno Tiago L.P. Galvão Inês M. Rocha Paula M.V. Fernandes Sílvia Q. Salgueiro Vanessa A.F. de Moura Isabel M.S.C. Oliveira Paula C. Cotelo Mariana R.A. Ribeiro 《The Journal of chemical thermodynamics》2009,41(9):984-991
984.
Freitas LS Von Mühlen C Bortoluzzi JH Zini CA Fortuny M Dariva C Coutinho RC Santos AF Caramão EB 《Journal of chromatography. A》2009,1216(14):2860-2865
In this work the higher peak capacity and resolution of comprehensive two-dimensional gas chromatography (GCxGC) has been successfully applied, for the first time, to tentatively identify several polar organic compounds of organic extracts of aqueous phases resulting from microwave demulsification process of water-in-crude oil emulsions. Results have shown that higher temperatures and longer exposure time to microwave irradiation produced water phases with a wider variety of polar organic compounds. The microwave process showed to be suitable for the extraction of several polar compounds classes of petroleum. The proposed microwave extraction method and GCxGC identification of polar compounds of petroleum samples are of practical interest for the petrochemical industry due to corrosion and related problems associated with these polar compounds in refinery equipments. The GCxGC/time-of-flight MS technique shows to be very important in the total separation of different classes of compounds and allows the identification of many compounds in these classes. 相似文献
985.
Determination of organic and inorganic mercury species in water and sediment samples by HPLC on-line coupled with ICP-MS 总被引:2,自引:0,他引:2
José Soares dos Santos Miguel de la Guárdia Maria Lúcia Pires dos Santos 《Talanta》2009,80(1):207-3009
This paper describes a preconcentration method for Hg2+ and MeHg+ in water samples using sodium diethyldithiocarbamate immobilized in polyurethane foam (PU-NaDDC) and an extraction method for several mercury species in sediment samples, including MeHg+, EtHg+ and PhHg+, which is simple, rapid, and uses a single organic solvent. Separation and measurement were done by high-performance liquid chromatography on-line with inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Initially, the test of recovery was applied using procedures compatible with HPLC. Under the optimum extraction conditions, recoveries of 96.7, 96.3 and 97.3% were obtained for MeHg+, EtHg+, and PhHg+, respectively, from n = 4 spiked sediment samples. This study also demonstrates that the combination of solid-phase extraction on PU-NaDDC with HPLC separation and ICP-MS detection is an effective preconcentration procedure for simultaneous measurement of Hg2+ and MeHg+ at ultra-trace levels in water samples. The application of the proposed procedure to the determination of mercury species in drinking water sample was investigated. The proposed method clearly gave satisfactory average recoveries between 93.7 and 101.5%. 相似文献
986.
Phabyanno Rodrigues Lima Paulo Rogério Barbosa de Miranda Adriano Bof de Oliveira Marília Oliveira Fonseca Goulart Lauro Tatsuo Kubota 《Electroanalysis》2009,21(21):2311-2320
The present work explores, for the first time, the electrocatalytic oxidation of ascorbic acid (AscH2) and its determination in the presence of uric acid (UA) on the in situ activated 4‐nitrophthalonitrile modified carbon paste electrode. The kinetic constant κ for the catalytic reaction for the electrocatalytic oxidation of ascorbic acid, evaluated by cyclic voltammetry, chronoamperometry and RDE voltammetry provided values around 106 L mol?1 s?1. The sensor provided a linear response range for AscH2 and UA from 5.0 up to 120.0 μmol L?1 with detection limits of 1.6 μmol L?1and 1.3 μmol L?1, respectively. The sensor was applied for the simultaneous determination of AscH2 and UA in urine samples and the average recoveries for these samples were 99.8 (±3.1)% and 99.9 (±2.1)%, respectively . 相似文献
987.
M. A. V. Ribeiro da Silva Ana Filipa L. O. M. Santos 《Journal of Thermal Analysis and Calorimetry》2009,95(2):333-344
The present work is part of a broader research program on the energetics of formation of heterocycles, aiming the study of
the enthalpic effects of the introduction of different substituents into heterocycles. In this work we present the results
of the thermochemical research on sulphur heterocycles of the type substituted thiophenes with different kind of substituents,
mainly alkyl, ester, acetyl, carboxamide, acetamide, carbonitrile and carboxaldehyde.
The standard (p
o=0.1 MPa) molar enthalpies of formation, in the condensed phase, at T=298.15 K, of a large number of substituted thiophenes, were derived from their standard massic energies of combustion, measured
by rotating-bomb combustion calorimetry, while the standard molar enthalpies of vaporization or sublimation of those compounds
were obtained either by high temperature Calvet Microcalorimetry, or by the temperature dependence of their vapour pressures
determined by the Knudsen effusion technique. The standard molar enthalpies of formation, of the studied sulphur heterocycles
in the gaseous phase, were then derived. The results are interpreted in terms of structural contributions to the energetics
of the substituted thiophenes, the internal consistency of the results is discussed and, whenever appropriate and possible,
empirical correlations are suggested for the estimation of standard molar enthalpies of formation, at T=298.15 K, of substituted thiophenes. A Table of enthalpic increments for different group substituents in positions 2 or 3
of the thiophene ring has been established. 相似文献
988.
A. L. M. de Oliveira J. M. Ferreira Márcia R. S. Silva Soraia C. de Souza F. T. G. Vieira E. Longo A. G. Souza Iêda M. G. Santos 《Journal of Thermal Analysis and Calorimetry》2009,97(1):167-172
NiWO4 and ZnWO4 were synthesized by the polymeric precursor method at low temperatures with zinc or nickel carbonate as secondary phase.
The materials were characterized by thermal analysis (TG/DTA), infrared spectroscopy, UV–Vis spectroscopy and X-ray diffraction.
NiWO4 was crystalline after calcination at 350 °C/12 h while ZnWO4 only crystallized after calcination at 400 °C for 2 h. Thermal decomposition of the powder precursor of NiWO4 heat treated for 12 h had one exothermic transition, while the precursor heat treated for 24 h had one more step between
600 and 800 °C with a small mass gain. Powder precursor of ZnWO4 presented three exothermic transitions, with peak temperatures and mass losses higher than NiWO4 has indicating that nickel made carbon elimination easier. 相似文献
989.
990.