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  • 1
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Low-molecular-weight hydrocarbons ; Extraterrestrial atmospheres ; Chemically bonded squalene(ane) phase ; 13C and29Si CP-MAS NMR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Chemically bonded squalene(ene) phases have been synthesized via a hydride modified silanization process using dimethylchlorosilane, triethoxysilane and trichlorosilane. The surface structure of the bonded phases were characterized with DRIFT and solid state NMR studies. The results of the latter indicate successful bonding of a non-terminal olefin to the silica surface and that bonding of individual squalene molecules appeared not to occur at the same site(s) presumably due to steric hindrance. Among the phases examined, the trichlorosilane-based material exhibits better chromatographic properties probably due to greater surface coverage and hence effective non-polar interaction between the solutes and the bonded ligands. Under isothermal conditions, the present packings produced fast and efficient separation of C1–C4 saturated hydrocarbons on shorter columns than similar columns containing alkyl- or bidentate alkyl-modified silica packings at low column head pressure and are thermally stable at temperatures up to 250°C or higher.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Oligomeric stationary phases ; Enthalpy-entropy compensation ; Methylene and phenyl selectivity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The effect of temperature and mobile phase composition (methanol-water) on the retention behaviour of an oligomeric series of n-octylsilyl bonded phases in reversed-phase liquid chromatography has been investigated. Plots of lnk against 1/T (van't Hoff plot) and the enthalpy of transfer (ΔHo) yields linear relationships under the conditions studied. The ΔHo values of the aromatic hydrocarbons and n-alkyl benzoates are higher than those of the polar compounds due to their higher level of interaction with the stationary phase. A linear plot of ΔHo vs. ΔSo suggest that the retention process, which is essentially controlled by non-specific (dispersive) interactions between the solutes and the bonded ligands, is identical for all cases evaluated. The existence of similar retention mechanisms is confirmed by the constant value of the enthalpy-entropy compensation temperature of the columns for a given class of componds. As expected, decreasing the methanol content (% v/v) of the mobile phase results in increased eluite retention times. The methylene and phenyl selectivities are found to be independent of the carbon content of the stationary phases and varied only with the eluent composition. In addition to their high stability under aggressive mobile phase conditions as previously reported, the results of this study generally showed that the solute retention process on oligomeric phases are similar to those exhibited by the conventional reversed phases.
    Type of Medium: Electronic Resource
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