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81.
M. Piñeiro-Iglesias M. Miñones-Vázquez E. Vázquez-Blanco S. Muniategui-Lorenzo P. López-Mahía D. Prada-Rodríguez 《Chromatographia》2002,56(7-8):483-488
Summary The aim of this work is to establish the best conditions for concentration and purification steps in the trace analysis of
aliphatic and polycyclic aromatic hydrocarbons (PAH) from atmospheric particulate matter by gas chromatography-flame ionisation
detection (GC-FID) and high performance liquid chromatography with ultraviolet and fluorescence detection (HPLC-UV-FL). The
best results for the more volatile compound were obtained with a combination of rotary evaporation and a stream of nitrogen
(near to 100% for aliphatic hydrocarbons and from 70 to 105% for PAH). Two types of solid phase extraction (SPE)cartridges
(Supelclean
tm
LC-Silica SPE tubes and Sep-Pak? Plus silica cartridges) and glass column were examined for the purification and fractionation step. Blank chromatograms of
both types of cartridges analysed by GC-FID made this study difficult, because a PSS (programmed split-splitless) injector
was employed thereby increasing the sensitivity. This problem was not observed in the HPLC-UV-FL blank chromatograms of these
cartridges. Glass columns filled with silica and alumina were chosen because no interference was found in the GC-FID blank
chromatograms and the best recoveries in the fractionation of both aliphatic hydrocarbons and PAH were achieved. This is especially
important when aliphatic hydrocarbons concentrations are lower than 1 μg mL−1. Finally, the selected conditions were applied to the analysis of hydrocarbons in real atmospheric particulate samples. 相似文献
82.
Two vanadyl salen complexes having peripheral styryl substituents have been reacted with 1-methyl-3-(3-mercaptopropyl)-imidazolium chloride using azoisobutyronitrile as radical initiator. The resulting compounds contain at the same time a vanadyl salen complex and one imidazolium cation. In agreement with the expectations in view of their structure, these compounds were insoluble in conventional organic solvents, but completely miscible in imidazolium ionic liquids. These vanadyl salen complexes bonded to an imidazolium cation are highly active and reusable catalysts for the cyanosilylation of aldehydes. Moderate enantiomeric excesses were obtained using the chiral version of this complex. 相似文献
83.
Fibers and 3D mesh scaffolds from biodegradable starch-based blends: production and characterization
The aim of this work is the production of fibers from biodegradable polymers to obtain 3D scaffolds for tissue engineering of hard tissues. The scaffolds required for this highly demanding application need to have, as well as the biological and mechanical characteristics, a high degree of porosity with suitable dimensions for cell seeding and proliferation. Furthermore, the open cell porosity should have adequate interconnectivity for a continuous flow of nutrients and outflow of cell metabolic residues as well as to allow cell growth into confluent layers. Blends of corn starch, a natural biodegradable polymer, with other synthetic polymers (poly(ethylene vinyl alcohol), poly(epsilon-caprolactone), poly(lactic acid)) were selected for this work because of their good balance of properties, namely biocompatibility, processability and mechanical properties. Melt spinning was used to produce fibers from all the blends and 3D meshes from one of the starch-poly(lactic acid) blends. The experimental characterization included the evaluation of the tensile mechanical properties and thermal properties of the fibers and the compression stiffness, porosity and degradation behavior of the 3D meshes. Light microscopy picture of 3D meshes. 相似文献
84.
CuAl2O4, NiAl2O4, and three ternary spinels CuxNi1?xAl2O3 have been prepared, in polycrystalline form, by solid-state reaction of mixtures of CuO, NiO, and Al2O3 at 1223 K. X-Ray powder diffractometry, coupled with adequate computational methods, allowed determination of the unit-cell length, oxygen positional parameter, and cation distribution for each compound. Interdependence of these structural parameters is closely analyzed on the ternary oxide spinels. The one-electron difference between the Cu2+ and Ni2+ ions was found to be enough to render them distinguishable by X-ray powder diffraction. 相似文献
85.
86.
J. J. LaBrecque Z. A. De Benzo E. Marcano C. A. Peña 《Journal of Radioanalytical and Nuclear Chemistry》1984,84(2):407-413
The comparison of an ambient temperature mercuric iodide spectrometer (HgI2) with a conventional cooled Si(Li) spectrometer is presented for the determination of niobium in Venezuelan laterites in the laboratory. The energy resolution of the HgI2 spectrometer was only about 590 eV (FWHM) at 5.9 keV compared to about 150 eV for the conventional Si(Li) spectrometer. The efficiency was about 5 times lower in the region of the NbK
peak as compared to the Si(Li) detector. Even though its energy resolution and efficiency is much poorer than the conventional Si(Li), the results it produced for the determination of niobium were acceptable for use in the exploration and exploitation of a niobium-rich deposit such as Cerro Impacto, Estado Bolívar, Venezuela. 相似文献
87.
88.
JPC – Journal of Planar Chromatography – Modern TLC - A new simple, rapid, and selective high-performance thin-layer chromatographic (HPTLC) method with metronidazole as the internal... 相似文献
89.
Kučinskaitė Agnė Pobłocka-Olech Loretta Krauze-Baranowska Mirosława Briedis Vitalis Savickas Aruñas Sznitowska Małgorzata 《平面色谱法杂志一现代薄层色谱法》2007,20(2):121-125
SPE and TLC have been used for qualitative and quantitative analysis of salidroside, rosavin, rosarin, and rosin in commercially available dry extracts from Rhodiola rosea roots. The best separation of all the compounds was achieved on silica gel TLC plates with ethyl acetate—methanol—water, 77 + 13 + 10 (v/v), as mobile phase. UV detection was performed at λ = 215 nm for salidroside and at λ= 245 nm for the rosavins (rosavin, rosarin, and rosin). Detection limits for salidroside and the rosavins were 90 ng and 60 ng per spot, respectively. Results from quantitative analysis confirmed the manufacturer’s declaration of the amounts of salidroside and the rosavins in the extracts.
相似文献90.
A. González Arias C. Torres C. de
Francisco J. M. Muñoz P. Hernández
Gómez O. Alejos O. Montero J. I. Iñiguez 《Journal of Thermal Analysis and Calorimetry》2006,86(1):195-198
The article discusses theory and experiment about the measurement of
defect concentration in Ti-substituted yttrium iron garnet by means of thermogravimetry
techniques. The two possible cases arising from oxygen interchange with atmosphere,
oxygen vacancies and interstitial cations, may be analyzed quantitatively
from the derived expressions. The possibility of another type of defects being
present in the samples, not associated to oxygen evolution, is not excluded.
Measurements were carried out in air and CO2 for different
Ti contents. The substitution tends to increase slightly the defect parameter
θ in YIG, while a CO2 reducing atmosphere is
much more effective than the Ti substitution for increasing θ. Calculations
for a given single-phased sample sintered in air show two possibilities: a
deficit of one oxygen atom for every 2.5 unit cells of 96 atoms, or one excess
cation for every 3.5 cells. Other samples show very similar results. The accuracy
involved in the measurements is about 2–3%. 相似文献