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31.
Summary The advantages and disadvantages of high performance precipitation liquid chromatography have been demonstrated for polystyrene
homopolymers. Depending on the mobile phase composition at the dissolution point of the polymeric sample and surface properties
of the stationary phase, elution is governed either by a solution process or by adsorption. A contribution by adsorption was
noticed on silica as well as on reversed phases based on silica with a normal phase gradient of increasing polarity (heptane
to dichloromethane). Elution was solely governed by solubility of the polymers on both types of stationary phase for polystyrenes
with a molecular weight above 35 000 and reversed phase gradient of decreasing polarity (methanol to dichloromethane). Under
these conditions an identical dependence of elution solvent composition on sample size was found as for turbidity titrations.
Due to differences in the velocity of the eluent front and the polymeric sample with porous stationary phases the polymers
can be eluted as colloidal solutions Non-porous stationary phases are superior in this respect because the velocities of eluent
and solutes are identical. 相似文献
32.
V. G. Berezkin V. R. Alishoyev E. N. Victorova V. S. Gavrichev V. M. Fateeva 《Chromatographia》1982,16(1):126-131
Summary The use of crystallohydrates, crystallohydrate solutions and melts as stationary phases in gas chromatography has been proposed. Crystallohydrates have been shown to display high selectivity in the separation of polar organic compounds when use is made of water vapours as the mobile phase. Some aspects of gas-liquid chromatography in water vapours and with the stationary phase comprising crystallohydrates have been studied, and the preliminary results obtained point to the desirability of further progress in this field.Presented at the 14th International Symposium on Chromatography London, September, 1982 相似文献
33.
Six isotypic R6ZTe2 phases have been synthesized in Ta at elevated temperatures and characterized by single crystal X-ray refinements for R=Y, Z=Rh, Pd, Ag, Y and for R=Lu, Z=Cu, Ag. All crystallize in the Sc6PdTe2-type structure, Pnma, Z=4, a∼21.5 Å, b∼4.1 Å, c∼11.4 Å. The results can be viewed as the replacement of Te3 atoms in the parent isotypic Sc2Te (or in the hypothetical Y2Te or Lu2Te analogues) by the above the Z, the Y example giving the new binary phase Y7Te2. The shorter (and stronger) metal-metal bonds concentrate in the region of metal (Z, Y) substitution, as revealed by larger integrated crystal orbital Hamilton population (ICOHP) values derived from linear muffin-tin-orbital (LMTO) calculations. Partial densities-of-states data for Y7Te2 reflect a similar behavior. Individual R-R bond distances are seen to deviate appreciably from the more fundamental overlap population measures for each. 相似文献
34.
Françoise Maugé Jean-Paul Gallas Jean-Claude Lavalley Guido Busca Gianguido Ramis Vincenzo Lorenzelli 《Mikrochimica acta》1988,95(1-6):57-61
In the far IR region at low molybdenum loadings, Mo-SiO2 catalysts present a pseudomolybdate or a polymolybdate species, while bulk-like MoO3 appears at loadings close to the geometrical monolayer coverage. W-SiO2 and V-SiO2 spectra show bands close to those observed on the corresponding bulk oxides.In the case of TiO2, Al2O3, ZrO2 supported catalysts, a band is observed near 1000 cm–1 which is assigned to the Mo=O stretching vibration of coordinatively unsaturated Mo
n+ ions showing a stronger interaction with the support than one observed on silica. 相似文献
35.
A chemically bonded cellulose tris(3,5-dimethylphenylcarbamate) chiral stationary phase (CSP) was prepared by a radical polymerization reaction. The prepared CSP was packed into fused-silica capillaries with inner diameter of 75 microm to perform enantiomer separations in CEC. The electrochromatographic behavior of the CSP was investigated. On the prepared CSP, high EOF could be generated under acidic mobile phases, which represented an advantage for the separation of acidic enantiomers. Several neutral, acidic, and basic enantiomers were resolved on the prepared CSP under aqueous mobile phases. The column efficiencies were between 20,000 and 100,000 plates/m, which were much higher than those of HPLC. In addition, it was observed that the separation of some enantiomers benefited from the adoption of THF as mobile phase modifier. 相似文献
36.
Since the introduction of micelles by Terabe et al. (1984), many different species have been employed as carriers for electrokinetic chromatography. As it is not possible to separate uncharged solutes or ions with equal mobility in capillary electrophoresis, these phases are added to introduce or improve selectivity.
This review surveys the application of particles as pseudo-stationary phases. Up to now only very few applications exist based either on polymer particles for the separation of catechols and primary amines or silica-based material. With these particles separations are shown for phenols, polycyclic aromatic hydrocarbons and naphthalene derivatives. The characteristic properties of particles as pseudo-stationary phases and their benefits as well as their limitations are discussed. 相似文献
37.
38.
A series of commercial monomeric and polymeric C(18), C(27), and C(30) stationary phases were compared with immobilized poly(ethylene-co-acrylic acid) stationary phases synthesized in-house. The columns were characterized on the basis of methylene selectivity, silanol activity, metal activity, pore size, shape selectivity, and the ability to separate tocopherol isomers and carotenoid isomers. Monomeric and polymeric C(30) phases were shown to yield excellent separations of the tocopherol isomers while the polymeric C(30) and polyethylene phases were more appropriate to the separation of carotenoids. 相似文献
39.
Improved quantification limits in chiral capillary electrochromatography by peak compression effects
The peak compression effect has been applied to improve quantification limits in chiral capillary electrochromatography (CEC). A stationary phase based on the chiral selector vancomycin (Chirobiotic V) was used for separations of the enantiomers of mianserin. By adding solvents with a low dielectric constant, e.g. 2-propanol or tetrahydrofuran, to the sample solution, peak compression could be induced. The plate numbers for the minor enantiomer increased from approximately 100,000 to 1.4-1.6 million plates/m, when the composition of the mobile phase was adjusted so that the analyte eluted within either one of two system zones originating from the sample solution. A 10-fold improvement in the quantification limit for the minor enantiomer was obtained compared to elution under non-focused conditions. 相似文献
40.
The main thermodynamic characteristics of the adsorption of haloadamantanes on graphitized thermal carbon black were determined by experimental measurements and by calculations in terms of molecular-statistic theory of adsorption. Using experimental data, the Kovac retention indices were calculated and the optimum conditions for gas-chromatographic separation of haloadamantanes on stationary phases with different polarity were elucidated. The influence of the cage effect in the adamantane unit on the chromatographic properties of haloadamantanes was established. 相似文献