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141.
This work presents the carrying out of boiling-point distributions by simulated distillation with direct-column heating rather than oven-column heating. Column-heating rates of 300 degrees C/min are obtained yielding retention times of 73 s for n-tetratetracontane. The calibration curves of the retention time versus the boiling point, in the range of n-pentane to n-tetratetracontane, are identical to those obtained by slower oven-heating rates. The boiling-point distribution of the reference gas oil is compared with that obtained with column oven heating at rates of 15 to 40 degrees C/min. The results show boiling-point distribution values nearly the same (1-2 degrees F) as those obtained with oven column heating from the initial boiling point to 80% distilled off. Slightly higher differences are obtained (3-4 degrees F) for the 80% distillation to final boiling-point interval. Nonetheless, allowed consensus differences are never exceeded. Precision of the boiling-point distributions (expressed as standard deviations) are 0.1-0.3% for the data obtained in the direct column-heating mode. 相似文献
142.
Sabbioni C Mandrioli R Ferranti A Bugamelli F Saracino MA Forti GC Fanali S Raggi MA 《Journal of chromatography. A》2005,1081(1):65-71
Glycyrrhizin is the main active compound of Glycyrrhiza glabra root extracts; according to recent studies, glycyrrhizin and its aglycon, glycyrrhetic acid, have interesting therapeutic properties. A new capillary electrophoretic method has been developed for the separation and quantification of glycyrrhizin, beta-glycyrrhetic acid and its isomer a-glycyrrhetic acid. Separation of the analytes was achieved in less than 3 min on a fused silica capillary, by injecting the samples at the short end of the capillary (effective length: 8.5 cm). The background electrolyte was composed of pH 10.0 carbonate buffer, methanol and ethylene glycol (80/10/10) and contained 0.4% beta-cyclodextrin; indomethacin was used as the internal standard. Diode array detection was used, with quantitative assays carried out at 254 nm. Linearity was found over the 5-200 and 2.5-100 microg mL(-1) concentration ranges for glycyrrhizin and glycyrrhetic acid, respectively. This method has been applied to the determination of the analytes in different matrices (liquorice roots and commercial confectionery products), and to the purity control of beta-glycyrrhetic acid obtained from the hydrolysis of glycyrrhizin. When analysing beta-glycyrrhetic acid and its epimer in roots, the samples were purified by means of a suitable solid-phase extraction (SPE) procedure with Oasis HLB cartridges, which granted good selectivity, eliminating matrix interference. 相似文献
143.
Boundary feedback stabilizability of parabolic equations 总被引:1,自引:0,他引:1
Roberto Triggiani 《Applied Mathematics and Optimization》1980,6(1):201-220
A parabolic equation defined on a bounded domain is considered, with input acting on theboundary expressed as a specifiedfeedback of the solution. Both Dirichlet and mixed (in particular, Neumann) boundary conditions are treated. Algebraic conditions based on the finitely many unstable eigenvalues are given, ensuring the existence ofboundary vectors, for which all the solutions to theboundary feedback parabolic equation decay exponentially to zero ast+ in (essentially) the strongest possible space norm. A semigroup approach is employed.Research partially supported by Air Force Office of Scientific Research under Grant AFOSR-77-3338.A preliminary version of this paper has appeared in the Proceedings of the International Symposium on the Mathematical Theory of Networks and Systems, held at Delft University, The Netherlands, July 3–6, 1979; pp. 428–433. 相似文献
144.
145.
Guidoboni E de los Rios I Ienco A Marvelli L Mealli C Romerosa A Rossi R Peruzzini M 《Inorganic chemistry》2002,41(4):659-668
Reaction of [(triphos)Re(CO)(2)(OTf)] (1) [triphos = MeC(CH(2)PPh(2))(3); OTf = OSO(2)CF(3)] with P(4)S(3) and P(4)Se(3) yields pairs of coordination isomers, namely, [(triphos)Re(CO)(2)[eta(1)-P(apical)-P(4)X(3)]](+) (X = S, 2; Se, 5) and [(triphos)Re(CO)(2)[eta(1)-P(basal)-P(4)X(3)]](+) (X = S, 3; Se, 6). The latter represent the first examples of the eta(1)-P(basal) coordination achieved by the P(4)X(3) molecular cage. Further reaction of 2/3 and 5/6 mixtures with 1 affords the dinuclear species [[(triphos)Re(CO)(2)](2)[mu,eta(1:1)-P(apical,)P(basal)-P(4)X(3)]](2+) (X = S, 4; Se, 7) in which the unprecedented M-eta(1)-P(basal)/eta(1)-P(apical)-M' bridging coordination of the P(4)X(3) molecule is accomplished. A theoretical analysis of the bonding properties of the two coordination isomers is also presented. The directionality of apical vs basal phosphorus lone pairs is also discussed in terms of MO arguments. 相似文献
146.
Badorrey R Cativiela C Díaz-de-Villegas MD Díez R Galbiati F Gálvez JA 《The Journal of organic chemistry》2005,70(24):10102-10105
[reaction: see text] Addition of trimethylsilyl cyanide to ketimines derived from (R)-2,2-dimethyl-1,3-dioxolan-4-yl methyl ketone to generate a quaternary stereocenter has been achieved with high yields and excellent diastereoselectivity. The stereoselectivity was found to be temperature and solvent dependent. The beta-hydroxy-alpha-amino nitrile of syn configuration was the major compound in kinetically controlled reactions, whereas the anti stereoisomer was obtained in excess in thermodynamically controlled reactions. Double stereodifferentiation under kinetic control conditions was successful, and the cyanation reaction occurred with complete syn diastereoselectivity using the matched pair. The versatility of the resulting amino nitrile as a synthetic intermediate was tested by performing the synthesis of orthogonally protected (R)-(2-aminomethyl)alanine. 相似文献
147.
Heinz-Peter Klein Ulf Thewalt Karl Döppert Roberto Sanchez-Delgado 《Journal of organometallic chemistry》1982,236(2):189-195
The trinuclear titanium(IV) complex (π-C5H5)2TiClOTi(π-C5H5)ClOTiCl(π-C5H5)2 · CHCl3 is formed by hydrolysis of (π-C5H5)2TiCl2 at pH > 3.5 and can be isolated in the crystalline state from the reaction of (π-C5H5)2TiCl2 with Ag2O and water in chloroform. Its structure is determined by X-ray analysis. 相似文献
148.
A series of cyano-bridged binuclear mixed valence complexes of the general formula M-Ru(III)(NH(3))(4)pyCOOH [pyCOOH = isonicotinic acid; M = cis-Ru(bpy)(2)(CN)(2), 1 (bpy = 2,2' bipyridine); trans-Ru(py)(4)(CN)(2), 2 (py = pyridine); [Ru(CN)(6)](4)(-), 3; [Fe(CN)(6)](4)(-), 4] have been prepared and anchored through the carboxylic function to nanocrystalline TiO(2) or SnO(2) electrodes. The complexes display a reversible electrochromic behavior in the range of applied potential from -0.5 to +0.5 V, versus SCE. Tuning of the electronic transitions in the visible and near-infrared spectral regions is achieved through changes of the solvent and of the cyano-bridged metal moiety M. 相似文献
149.
Hortencia Silva-Jiménez Roberto Zazueta-Sandoval 《Applied biochemistry and biotechnology》2005,121(1-3):205-217
In previous work, purification procedures and zymogram analysis conducted with supernatants of crude extracts from aerobic
mycelium of the YR-1 strain of Mucor circinelloides isolated from petroleum-contaminated soils indicated the existence of only one soluble alcohol oxidase (sAO) activity. In
the present work enzymatic activity of alcohol oxidase (AO) was also detected in the mixed membrane fraction (MMF) of a high-speed
centrifugation procedure after drastic ballistic cellular homogenization to break the mycelium from strain YR-1. When mycelial
cells were gently broken by freezing the mycelium with liquid nitrogen, smashing in a mortar, and submitting the samples to
an isopycnic sucrose gradients (10–60% sucrose), AO activity was detected in particular and discrete fractions of the gradient,
showing specific density values quite different from the density of peroxisomes. The results suggest that there could be a
different intracellular pattern of distribution of the microsomal fraction in aerobically grown mycelium depending on the
carbon source used in the culture media, including alcohols and hydrocarbons, but not in glucose. In working with particulate
fractions, we found two AO activities: a new membrane alcohol oxidase (mAO) activity and the sAO. Both activities appear to
be located in the inner of the cells in specific compartments different from the peroxisomes, so mAO could be in the membrane
of these compartments and sAO in the lumen of the vesicles. We also assayed other enzymatic activities involved in hydrocarbon
biodegradation to establish its intracellular location and other enzymatic activities such as peroxidase to use them as intracellular
markers of different organelles. In the case of monooxygenase, the first enzymatic step in the hydrocarbon biodegradation
pathway, its location was in the same fractions where AOs were located, suggesting the existance of a specific organelle that
contains the enzymatic activities involved in hydrocarbon biodegradation. 相似文献
150.
Roberto Fernández de la Pradilla 《Tetrahedron》2006,62(11):2684-2692
(E,E) and (Z,E) γ-alkoxy dienyl sulfones undergo nucleophilic epoxidation with remarkable regio- and stereoselectivity to render syn oxiranes in a process mainly controlled by the alkoxy stereocenter. Upon epoxidation γ-hydroxy dienyl sulfoxides provide sulfinyl and sulfonyl oxiranes along with bis-epoxides formed through a Payne rearrangement that can be prevented by silylation of the OH group. Interestingly, the presence of a γ-silyloxy group can invert the stereochemical trend of the molecule affording mainly an anti epoxidation process. 相似文献