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141.
Mariana Cristea Daniela Gheorghiu Ionita Maria Bruma B. C. Simionescu 《Journal of Thermal Analysis and Calorimetry》2008,93(1):63-68
Two aromatic polyimides and the corresponding poly(amic acid)s, with oxadiazole and para/meta phenoxyphenylene rings in the backbone, were synthesized and the structure — thermal properties correlation was followed
by dynamic mechanical analysis. Concerning the poly(amic acid)s, the glass transition domain was emphasized only for the compound
with meta-oriented rings because the process of imidization takes place with increasing temperature. A multiplex experiment was performed
to calculate the activation energy of the transition localized under 200°C. Consecutive heating-cooling-heating cycles were
accomplished. All phenomena are discussed by cross-examination of the storage modulus (E′), loss modulus (E″) and loss factor tanδ variation with temperature. 相似文献
142.
Andrei Medvedovici Florin Albu Iuliana Daniela Sora Stefan Udrescu Toma Galaon Victor David 《Biomedical chromatography : BMC》2009,23(10):1092-1100
A sensitive method for determination of free captopril as monobromobimane derivative in plasma samples is discussed. The internal standard (IS) was 5‐methoxy‐1H‐benzimidazole‐2‐thiol. Derivatization with monobromobimane immediately after blood collection and plasma preparation prevents oxidation of captopril to the corresponding disulfide compound and enhances the ionization yield. Consequently, derivatization enhances sample stability and detection sensitivity. Addition of the internal standard was made immediately after plasma preparation. The internal standard was also derivatized by monobromobimane, as it contains a thiol functional group. Preparation of plasma samples containing captopril and IS derivatives was based upon protein precipitation through addition of acetonitrile, in a volumetric ratio 1:2. The reversed‐phase liquid chromatographic separation was achieved on a rapid resolution cartridge Zorbax SB‐C18, monitored through positive electrospray ionization and tandem MS detection using the multiple‐reaction monitoring mode. Transitions were 408–362 amu for the captopril derivative and 371–260 amu for the internal standard derivative. The kinetics of captopril oxidation to the corresponding disulfide compound in plasma matrix was also studied using the proposed method. A linear log–log calibration was obtained over the concentration interval 2.5–750 ng/mL. A low limit of quantitation in the 2.5 ng/mL range was obtained. The analytical method was fully validated and successfully applied in a three‐way, three‐period, single‐dose (50 mg), block‐randomized bioequivalence study for two pharmaceutical formulations (captopril LPH 25 and 50 mg) against the comparator Capoten 50 mg. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
143.
Tongjit Kidchob Luca Malfatti Daniela Marongiu Stefano Enzo Plinio Innocenzi 《Journal of Sol-Gel Science and Technology》2009,52(3):356-361
The process of formation of cerium titanate films as a function of annealing temperature and composition has been studied
by combining X-ray diffraction analysis and far infrared spectroscopy. The films have been prepared by a sol–gel synthesis
using metal chlorides as precursors; the synthesis allows obtaining cerium titanate films upon annealing in air. A brannerite
type, CeTi2O6, phase has been identified by X-ray diffraction and Rietveld analysis on thin films. CeTi2O6 is formed upon annealing at 700 °C and in a limited range of ceria-titania mixed compositions. The far infrared spectra are
useful to observe the formation of crystalline phases at the beginning of the crystallization process at lower firing temperatures,
when the XRD analysis is not enough sensitive. 相似文献
144.
Iolinda Aiello Mauro Ghedini Annarita Grisolia Daniela Pucci Oriano Francescangeli 《Liquid crystals》2005,32(6):763-769
New Ni(II) and UO2(II) metallomesogens obtained from mesomorphic N,N'-salicyliden(3,3'-diamine-N-methyldipropylamine) ligands containing a pentadentate N3O2 chelating cavity and bearing two or four lateral substituents, are isolated and fully characterized. Some of the synthesized nickel and dioxouranium complexes show a SmC mesophase. To the best of our knowledge, these species are the first pentacoordinated Ni(II) and heptacoordinated UO2(II) metallomesogens to be reported. 相似文献
145.
Alex Virgilio Renata Stabile Amais Daniela Schiavo José Anchieta Gomes Neto Joaquim de Araújo Nóbrega 《Analytical letters》2017,50(5):842-852
A procedure for the determination of As, Cd, Cr, Ni, Pb, and V in phytotherapy medicines by inductively coupled plasma–tandem mass spectrometry is reported. The use of tandem mass spectrometry with oxygen into an octopole reaction system at various gas flow rates and the combination of on-mass and mass-shift modes was evaluated. Cadmium, Cr, Ni, and Pb were determined as free atomic ions while As and V were determined as the oxides AsO+ and VO+ in the same run. Samples were prepared by microwave-assisted digestion with dilute nitric acid and hydrogen peroxide. Two plant-certified reference materials (apple leaves and tomato leaves) were used to check the accuracy. For tandem mass spectrometry with 0.5?mL min?1 O2, recoveries in the 85–113% were typically obtained and no statistical differences were observed at the 95% confidence level (t-test) in comparison with the certified values. Using these conditions, the limits of detection for the method were 0.01, 0.0002, 0.008, 0.008, 0.003, and 0.002?µg g?1 for As, Cd, Cr, Ni, Pb, and V, respectively. The procedure was used for the analysis of four phytotherapic drugs and the determined concentrations were up to 0.168?µg g?1 As, 0.03?µg g?1 Cd, 0.82?µg g?1 Cr, 1.18?µg g?1 Ni, 0.52?µg g?1 Pb, and 2.4?µg g?1 V with average precision values of 8% as the relative standard deviation. The found concentrations were compared with limits proposed in official guidelines and, in most cases, the values were below the maximum limits allowed. 相似文献
146.
147.
Carolina G. Dos Santos Daniela T. Marquez Charles-Oneil L. Crites Jose Carlos Netto-Ferreira Juan C. Scaiano 《Tetrahedron letters》2017,58(5):427-431
Two different hybrid materials composed of gold nanoparticles (AuNPs) supported on either commercial niobium oxide HY 340 or mesoporous niobium oxide catalyzed the Friedel-Crafts alkylation of anisole by benzyl chloride. Excitation of the surface plasmon of the supported AuNPs allowed the reaction to occur at lower temperatures by acting as an alternative heat source. The localized heating produced via plasmon excitation permitted the acid catalyzed reaction to occur - at the Lewis acid sites on the Nb2O5 support - at 80 °C while thermal-dark reactions using a conventional heat source, required temperatures of 120 °C or higher. The catalytic activity of the tested hybrid materials decreased with storage time. However, the deactivation showed to be reversible upon lyophilisation indicating that the nature of the deactivation could be due to water adsorption. 相似文献
148.
In this study, the synthesis, structural characterisation and mesomorphic and optical properties of seven new bent-shaped and polycatenar bent-shaped compounds derived from chalcone and cyanopyridine are reported. The mesomorphic behaviour was investigated by differential scanning calorimetry (DSC), polarised optical microscopy (POM) and X-ray diffraction (XRD) and correlated with the molecular structure. Two bent-core hexacatenars molecules (Ic and IIc) presented liquid crystalline properties, showing a hexagonal columnar (Colh) phases at room temperature, being each disc constituted by two mesogens. Optical studies were also performed for the final molecules, being conducted by ultraviolet-visible and fluorescence spectrometry. The cyanopyridine derivatives show moderate luminescence quantum yields, ranging between 18% and 27%, with emission maxima around 371 nm. It is also shown that while the chalcone central unit favours a calamitic liquid crystalline behaviour in molecules with lower number of aliphatic chains, a polycatenar structure with cyanopyridine as the central unit favours a Colh arrangement, also providing luminescence properties to the molecule. 相似文献
149.
Daniela Belli Dell’Amico Luca Labella Fabio Marchetti Simona Samaritani 《Coordination chemistry reviews》2010,254(5-6):635-645
In this review we summarize some recent literature data concerning synthetic procedures, properties, structure, reactivity and applications of halo-carbonyl complexes of palladium, platinum and gold, taking into consideration that the organometallic chemistry of these metals, with a particular attention to the halo-carbonyls, has been reviewed 20 years ago [F. Calderazzo, J. Organomet. Chem. 400 (1990) 303]. A brief overview of the early studies is provided. 相似文献
150.
Oana Carp Luminita Patron Daniela C. Culita Petru Budrugeac Marcel Feder Lucian Diamandescu 《Journal of Thermal Analysis and Calorimetry》2010,101(1):181-187
The thermal stability of two kinds of dextran-coated magnetite (dextran with molecular weight of 40,000 (Dex40) and 70,000
(Dex70)), obtained by dextran adsorption onto the magnetite surface is investigated in comparison with free dextran in air
and argon atmosphere. The thermal behavior of the two free dextran types and corresponding coated magnetites is similar, but
atmosphere dependent. The magnetite catalyzes the thermal decomposition of dextran, the adsorbed dextran displaying lower
initial decomposition temperatures comparative with the free one in both working atmospheres. The dextran adsorbed onto the
magnetite surface decomposes in air through a strong sharp exothermic process up to ~450 °C while in argon atmosphere two
endothermic stages are identified, one in the temperature range 160–450 °C and the other at 530–800 °C. 相似文献