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41.
42.
碳十八键合锆胶固定相的制备与色谱性能评价 总被引:5,自引:0,他引:5
用诱导聚合胶体凝聚法(PICA)制得的二氧化锆微球与碳十八三乙氧基硅烷反应制备了碳十八键合锆胶固定相(ODZ),评价了该柱填料的色谱性能,并用此固定相分离了中性和碱性化合物。 相似文献
43.
O. de la Iglesia M. Pedernera R. Mallada Z. Lin J. Rocha J. Coronas J. Santamaría 《Journal of membrane science》2006,280(1-2):867-875
MCM-48 membranes have been prepared on alumina supports of different pore sizes. A battery of characterization techniques has been used to study the physical properties and the quality of the membranes prepared. The highest quality membranes were prepared on supports with pore size of up to 60 nm. The MCM-48 membranes were tested in the separation of gas phase mixtures and a cyclohexane/O2 selectivity higher than 270 was obtained. The selective separation of organic compounds from inert components is a result of the cooperative effects of capillary condensation in MCM-48 pores and of the specific interactions of the permeating compounds and the membrane material. 相似文献
44.
Pinto FG Andrada D Magalhães CG Nunes BR de Amorim FR Franco MB Saint'pierre TD da Silva JB Curtius AJ 《Analytical and bioanalytical chemistry》2005,383(5):825-832
Different chemical modifiers for use with electrothermal atomic absorption spectrometry (ET AAS) were investigated in relation
to determining the selenium in human urine samples. The samples were diluted in a solution containing 1% v/v HNO3 and 0.02% m/v cetyltrimethylammonium chloride (CTAC). Studying the modifiers showed that the use of either Ru or Ir as the
permanent modifier gave low sensitivity to Se and the peak shape was very noisy, while Zr or Rh gave no peak at all. The same
occurred when Zr was used in solution. For mixtures of permanent modifiers, Ir plus Rh or Zr plus Rh gave very low sensitivity,
Zr plus Rh with co-injection of Ir in solution was also not efficient, Zr plus Rh in solution gave good sensitivity, but the
best results were obtained with a mixture of Zr and Rh as the permanent modifier and co-injection of Rh in solution. Using
this last modifier, the following dilutions with the HNO3 and CTAC were studied: 1:1, 1:2, 1:3 and 1:4. The best dilution was 1:1, which promoted good sensitivity and a more defined
peak shape and made it possible to correct for the background using a deuterium arc lamp. Under these conditions, a characteristic
mass of 26±0.2 pg was obtained for Se in aqueous solution. Six certified urine samples were analyzed using matrix matching
calibration and the measured concentrations were in agreement with the certified values, according to a t-test at the 95%
confidence level. Recovery tests were carried out and the recoveries were in the range 100–103%, with relative standard deviation
better than 9%. The limit of detection (LOD, 3 sd, n=10) was 3.0 μg L−1 in the sample. The treated graphite tube could be used for at least 600 atomization cycles without significant alteration
of the analytical signal. 相似文献
45.
M. Jochum R. Bakry I. Wartusch C. W. Huck H. Engelhardt G. K. Bonn 《Chromatographia》2002,56(5-6):263-268
Summary This paper reports on the use of a polymer-based, strong anion-exchange stationary phase for rapid, selective and sensitive
analysis of physiological important mono-, di- and oligosaccharides by high-performance anion-exchange chromatography (HPAEC)
with pulsed amperometric detection (PAD) under alkaline conditions. The adsorbent was obtained by direct nitration of 3 and
5 μm, spherical non-porous highly cross-linked, styrene-divinylbenzene copolymer (PS-DVB) beads, followed by reduction of
superficially introduced nitro groups with nascent hydrogen and quaternization of the resultant amino groups with iodomethane.
Extended exposure to high pressure and strong alkaline conditions did not have any untoward effect on mechanical stability
and chromatographic performance. A comparison of the 3 and 5 μm beads showed, that the synthesized 3 μm highly cross-linked
PS-DVB particles are the preferred phases for the separation of monosaccharides and the 5 μm particles are preferable for
the separation of oligosaccharides. To demonstrate the suitability for the analysis of complex samples, the optimized and
validated system was used for the determination of glucose, fructose and sucrose in apple juice and other soft drinks such
as Coca Cola. Finally, analysis within a few minutes without sample pretreatment down to a lower limit of detection of 0.174–0.504
μg mL−1 at a linearity with R2>0.994 and a repooducibility higher than 98% further confirmed the efficiency of these polymeric sorbents. 相似文献
46.
Summary The effect of silica gel pretreatment and of different bonding techniques, on the chromatographic properties of octadecyl
bonded phases is described. The experiments show that a monomeric octadecyl bonded phase, prepared from silica gel that has
not been treated before bonding, has a poor selectivity towards polycyclic aromatic hydrocarbons (PAHs) and shows high adsorption
of basic components. Silica gel treatment before the bonding of the monofunctional silane does not give a substantial improvement.
Polymeric phases on the other hand show a much better PAH selectivity and a lower adsorptivity towards basic components. Further
improvement can be achieved with the polymeric modification if silica gel treatment is carried out before bonding. 相似文献
47.
Takatsugu Masuda Cara L. Nygren Kunimitsu Uchinokura 《Journal of solid state chemistry》2003,176(1):175-179
The structure of Cu2Fe2Ge4O13, previously thought to be CuFeGe2O6, has been determined from single-crystal X-ray diffraction data to be monoclinic, P21/m, a=12.1050(6), b=8.5073(4), c=4.8736(2) Å, β=96.145(1)°, Z=2, with R1=0.0231 and wR2=0.0605. The unique structure has an oligomer of four germanate tetrahedra, cross-linked laterally by square-planar copper ions, joined end-to-end by a zigzag chain of edge-sharing iron oxide octahedra. Running along the a-direction the metal oxide chain consists of alternating Cu-Cu and Fe-Fe dimers. A hypothetical series of homologous structures (Cun−2Fe2GenO3n+1 with n=3,4,…,∞) with different length germanate oligomers is proposed, where as n increases, the infinite chain of the CuGeO3 is approached. In this context, Cu2Fe2Ge4O13 is viewed as being built from blocks of CuGeO3 and the Fe oxide chains. This material has significance to the study of low-dimensional mixed-spin systems. 相似文献
48.
W. Wasiak 《Chromatographia》1987,23(6):423-426
Summary A column packing containing thiol groups chemically bonded to the silica surface was synthesized. The thiol functional groups were used as ligands capable of forming stable complexes with Cu(II). The prepared material was characterized by gas chromatography using unsaturated linear and branched hydrocarbons as well as cyclic and aromatic hydrocarbons. The occurrence of specific metal—olefin interactions resulting from the formation of -complexes during the chromatographic process was observed.Part IV of a series on transition metal complexes in GC. Part III see ref. [1]. 相似文献
49.
Summary Two reversed-phase LC systems were investigated by frontal analysis for the determination of linear chromatographic conditions,
as defined according to the isotherm concept. The Partisil ODS-3 bonded silica and the PRP-1 polystyrene-divinylbenzene resin
were used as stationary phases together withtrans-2-hexen-al as test solute and methanol-water mixtures as mobile phases. Particular attention was paid to the respective influence
of the two main parameters which may cause sorbent overloading, that is, the capacity factor (k′) and the solute concentration
in the mobile phase (Cm). Provided that k′Cm≤10−2 M, linear chromatographic behaviour was observed for both sorbents, the maximum capacities of which were found greater than
1mmolg−1. 相似文献
50.
In this paper interfacial edge crack problems are considered by the application of the finite element method. The stress intensity factors are accurately determined from the ratio of crack-tip-stress value between the target given unknown and reference problems. The reference problem is chosen to produce the singular stress fields proportional to those of the given unknown problem. Here the original proportional method is improved through utilizing very refined meshes and post-processing technique of linear extrapolation. The results for a double-edge interface crack in a bonded strip are newly obtained and compared with those of a single-edge interface crack for different forms of combination of material. It is found that the stress intensity factors should be compared in the three different zones of relative crack lengths. Different from the case of a cracked homogeneous strip, the results for the double edge interface cracks are found to possibly be bigger than those for a single edge interface crack under the same relative crack length. 相似文献