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61.
A simple spray pyrolysis setup is used to grow multi-walled carbon nanotubes (MWCNTs), from a ferrocene solution in benzene
as precursor. The effects of process variables such as growth temperature, position of the aerosol generator and position
in the reactor where the sample was formed were investigated. These variables have a strong influence on the graphitization
degree, homogeneity, diameter and alignment of the nanotubes, as observed by TEM, SEM, XRD and Raman spectroscopy. Vertically
aligned MWCNT arrays with high density were obtained in large areas (10 × 10 mm2), with high yield (2.1 mg cm−2) and at a growth rate at 1.43 μm min−1, by a suitable choice of the experimental conditions. 相似文献
62.
Bertini I Jiménez B Piccioli M 《Journal of magnetic resonance (San Diego, Calif. : 1997)》2005,174(1):125-132
To optimize 13C direct detected experiments for the observation of signals close to a paramagnetic center, we have assessed the sensitivity of different sequences based on CO-Cali coherence transfer. Features of CACO experiments were tested for Calbindin D9k, in which one of the two native Ca2+ ions is replaced by the paramagnetic Ce3+ ion. We have studied the comparison of single vs multiple quantum coherence transfer evolution as well as the influence of in-phase vs anti-phase detection of 13CO signals and finally the comparison of a coherence transfer step based on a CyO in plane with respect to a Cy ali in plane. The acquisition of the anti-phase component of the signal, accomplished by the removal of the last refocusing steps, allowed the identification of some signals unobserved with other pathways. The structural dependency of paramagnetism-induced nuclear relaxation is such that the identification of the most suitable coherence transfer pathway is not known "a priori" but it is driven by the relative proximity of Cali and CO to the paramagnetic center. 相似文献
63.
Intermodal dispersion between the supermodes of a directional coupler may induce undesirable pulse breakup in a sufficiently large device. When this happens the device will no longer exchange power between its arms, and the extinction ratio is completely canceled. It is shown that, by carefully designing the coupling area of the directional coupler, one may compensate for intermodal dispersion. The compensating device should accomplish three basic requirements: inverse intermodal dispersion, balanced coupling of each supermode, and maximum power transfer while preserving the sign of the slope of the coupling coefficient with frequency for multiplexing-demultiplexing applications. This structure is designed and optimized with a genetic algorithm. 相似文献
64.
Versatile chelating behavior of benzil bis(thiosemicarbazone) in zinc, cadmium, and nickel complexes
Reactions of benzil bis(thiosemicarbazone), LH(6), with M(NO(3))(2).nH(2)O (M = Zn, Cd, and Ni), in the presence of LiOH.H(2)O, show the versatile behavior of this molecule. The structure of the ligand, with the thiosemicarbazone moieties on opposite sides of the carbon backbone, changes to form complexes by acting as a chelating molecule. Complexes of these metal ions with empirical formula [MLH(4)] were obtained, although they show different molecular structures depending on their coordinating preferences. The zinc complex is the first example of a crystalline coordination polymer in which a bis(thiosemicarbazone) acts as bridging ligand, through a nitrogen atom, giving a 1D polymeric structure. The coordination sphere is formed by the imine nitrogen and sulfur atoms, and the remaining position, in a square-based pyramid, is occupied by an amine group of another ligand. The cadmium derivative shows the same geometry around the metal ion but consists of a dinuclear structure with sulfur atoms acting as a bridge between the metal ions. However, in the nickel complex LH(6) acts as a N(2)S(2) ligand yielding a planar structure for the nickel atom. The ligand and its complexes have been characterized by X-ray crystallography, microanalysis, mass spectrometry, IR, (1)H, and (13)C NMR spectroscopies and for the cadmium complex by (113)Cd NMR in solution and in the solid state. 相似文献
65.
We introduce and study matrix Christoffel functions for a matrix
weight W.
We find an explicit expression of the matrix Christoffel functions
in terms of any sequence of orthonormal matrix polynomials with
respect to W. An extremal property related to the matrix moment
problem defined by W is established for the matrix Christoffel
functions. We finally find the relative asymptotic behavior of
the matrix Christoffel functions associated to matrix weights in
the matrix Nevai class. 相似文献
66.
Kleij AW Souto B Pastor CJ Prados P de Mendoza J 《The Journal of organic chemistry》2003,68(22):8711-8714
The selective preparation and complete structural characterization of a small series of 1,2-anti-heterodisubstituted calix[4]arenes has been accomplished. These compounds were obtained in two steps from unsubstituted p-tert-butylcalix[4]arene by tribenzoylation and a subsequent one-pot, two-step sequence involving alkylation with simultaneous partial deacylation, resulting in heterodisubstituted calixarenes carrying an alkyl and an aroyl group. The monoalkyl-tribenzoyl intermediate, prior to in situ deprotection, could also be isolated. 相似文献
67.
68.
69.
Rosa Mª. González-Rodríguez Beatriz Cancho-GrandeJesús Simal-Gándara 《Journal of chromatography. A》2009,1216(32):6033-6042
A gas chromatographic ion trap mass spectrometry (GC-ITMS) method was developed for the determination of 11 new generation fungicides (benalaxyl, benalaxyl-M, boscalid, cyazofamid, famoxadone, fenamidone, fluquinconazole, iprovalicarb, pyraclostrobin, trifloxystrobin and zoxamide) in grapes and wines. Samples were extracted with ethyl acetate:hexane (1:1, v/v) and cleaned-up with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. The addition of analyte protectants (3-ethoxy-1,2-propanediol, d-sorbitol and l-gulonic acid γ-lactone) in the final extracts allowed to avoid the matrix-induced response enhancement effect on quantitation process with absolute recoveries ca. 100%. Precision (expressed as relative standard deviation) was lower than 16% for all fungicides. Limits of detection and quantitation were lower than 0.01 mg/kg or mg/L, except for cyazofamid, much smaller in all cases than maximum residue levels (MRLs) established by European Union for grapes and by Switzerland and Italy for wines. The proposed method was applied to determine fungicide residues in three different white grapes for vinification produced in Ribeiro area in Galicia (NW Spain), as well as in their corresponding final wines. 相似文献
70.
Tatiana Visnevschi-Necrasov Sara C. Cunha Eugénia Nunes M. Beatriz P.P. Oliveira 《Journal of chromatography. A》2009,1216(18):3720-3724
A method based on matrix solid-phase dispersion (MSPD) has been developed for the determination of 12 isoflavones in Trifolium pratense L. Dried leaf samples were blended with C18, placed in small columns and isoflavones extracted with dichloromethane–methanol. Analyses were performed by high performance liquid chromatography with diode array detection (HPLC-DAD) with 2-methoxyflavone as internal standard. Several dispersants, eluents and clean-up steps were tested during the optimization of the process in order to obtain the best selectivity and yields. Mean recoveries ranged from 70% to 119%, with relative standard deviations <18%. The limits of detection were between 0.006 mg/l for biochanin A and 0.108 mg/l for daidzin. The performance of the optimized method in real samples was compared with a conventional method based in solid–liquid extraction (SLE). 相似文献