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  • 1
    Electronic Resource
    Electronic Resource
    s.l. : American Chemical Society
    The @journal of physical chemistry 〈Washington, DC〉 89 (1985), S. 4338-4342 
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1572-8943
    Keywords: catalytic hydrosilylation ; functional olefins ; immobilization ; silica surface
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract By means of hydrosilylation reactions between functional olefins and triethoxysilane in the presence of Speier's catalyst and sol-gel transformations of the reaction products, a number of optically active and complexing alkenes (quinine, quinidine, cinchonine, cinchonidine, alprenolol, N-allylrhodanine and hemin) were immobilized on the surface of silica. The structures of the compounds formed and the nature of their bonding with the surface were studied by DRIFT and NMR spectroscopies. The concentrations of olefins anchored to the surface layer of the silica matrix were estimated by UV spectroscopy.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 25 (1988), S. 969-973 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carboxylic acid phase ; Addition reactions ; Synthesis of new bonded phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The allyl bonded phase is used as an intermediate in the synthesis of a weak cation exchange material. The double bond is first converted to an aldehyde by an ozonation reaction and then subsequent oxidation to the carboxylate group is accomplished with dichromate. Diffuse reflectance Fourier transform infrared spectroscopy (DRIFT) is used to monitor the conversion process. The presence of the aldehyde functional group is confirmed by reaction with 2,4-dinitrophenylhydrazine. ESCA spectra reveal no residual chromium on the silica surface. The product is tested chromatographically by the retention of alkylarylketones, the ion-exchange behavior of both monovalent and divalent cations, the retention of nucleosides and bases, and the separation of a mixture of hemoglobins.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 28 (1989), S. 565-568 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; New bonded phases ; Alumina ; Protein separation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Several reactions are tested for the chemical modification of alumina. These include the following: chlorination of the surface hydroxyls followed by reaction with an organolithium compound; chlorination of the surface hydroxyls followed by reaction with a Grignard reagent; chlorination of the surface hydroxyls followed by reaction with an amine; chlorination of the surface hydroxyls followed by reaction with an alcohol; direct reaction of the alumina with an organochloroalane and direct reaction of the alumina with an alcohol. Only the first reaction gave a product which contained enough bonded organic material to be easily detected by FTIR. Preliminary stability tests show that the product of the first reaction retains the bonded organic material when exposed to nonpolar and polar organic solvents as well as aqueous solutions of pH 1.0, 7.0 and 12.0. Chromatographic testing establishes reversed-phase behavior for alkylarylketones as solutes and the bonded phase displays good biocompatibility for a series of protein standards.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 30 (1990), S. 442-446 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Allyl bonded phase ; Hydrosilylation reaction ; Synthesis of new bonded phases ; Propyldimethylphenylsilane phase
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A propyldimethylphenylsilane stationary phase was prepared by a hydrosilylation reaction on the double bond of an allyl bonded phase intermediate. The carbon load on the silica was between 8.8–9.0%. Evaluation of the material by FTIR indicated high conversion of the double bond by the hydrosilylation reaction. The bonded material displayed reversedphase properties as determined by the retention behavior of alkylarylketones but it was less hydrophobic than either C-8 or C-18. The stability at both low and high pH was excellent. Separations of pharmaceutical compounds, a mixture of anilines, and a mixture of dopamine and epinephrine were satisfactory.
    Type of Medium: Electronic Resource
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  • 6
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Octadecyl titania ; Hydride surface ; Hydrosilation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The silanization/hydrosilation bonding method is tested on both a laboratory synthesized and commercial titania. The laboratory titania made by the sol-gel process shows evidence of residual organic material that is removed by an initial acid hydolysis followed by bonding of the hydride (triethoxysilane) under acidic conditions. DRIFT and solid state CP-MAS NMR studies are used to confirm the formation of the hydride layer on the titania and the success of the hydrosilation process for attaching an organic moiety (1-octadecene) to the surface. Chromatographic testing, primarily on the commercial titania based C-18 phase, indicates good reverse phase properties and few residual OH groups, either Ti−OH or Si−OH, as determined by the symmetrical peak shapes obtained for anilines and alkylphenylamines using mobile phases with no buffers or masking agents in the aqueous component.
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Liquid crystal bonded phase ; Polycyclic aromatics ; Carvone and pulegone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A chromatographic and thermodynamic study of the compound [4-(allyloxy)benzoyl]-4-methoxyphenyl (ABMP) as a model of a chemically bonded liquid crystal stationary phase for HPLC was undertaken. A number of polycyclic aromatic hydrocarbons (PAHs) and two small solutes, carvone and pulegone, were studied under varying solvent and temperature conditions. Plots of log k′ vs. % organic in the mobile phase were not completely linear in all cases. The van't Hoff plots revealed at least one phase transition. The enthalpies of solute transfer from the mobile phase to the ABMP phase were determined for several PAHs. All tests indicate that ABMP possess liquid crystal properties when bonded to particulate silica.
    Type of Medium: Electronic Resource
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  • 8
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Bonded liquid crystals ; Polymeric stationary phases ; Variable temperature studies
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Using two polycyclyic aromatic hydrocarbons as solutes, a comparison is made between a bonded liquid crystal stationary phase and a conventional polymeric C-18 phase. The bonded nematic liquid crystal phase was the silanized form of 4-[4-(allyloxy)benzoyl-oxy]biphenyl and the polymeric phase was Vydac 201TP. Both phases display shape and planarity selectivity as indicated by the results of the variable temperature and mobile phase composition studies. The slot theory of retention can be used to explain these results. However, the liquid crystal phase is more sensitive to molecular geometry, probably due to its more ordered structure on the surface. Variable temperature experiments which compare retention during both heating and cooling provides additional support for this conclusion. With the polymeric bonded C-18 phase, each solute had identical retention at the same temperature during both the heating and cooling cycles. On the bonded liquid crystal phase, measurable differences in retention were observed at identical temperatures depending on whether the column was heated or cooled. This effect is attributed to a degree of partially reversible disordering which occurs as the column temperature was increased. However, conditioning with the appropriate mobile phase can restore the original retention characteristics of the bonded liquid crystal phase.
    Type of Medium: Electronic Resource
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  • 9
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemically bonded phases ; Non-silica based supports ; Hydrosilation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A process for bonding a monolayer of silane to the surface of alumina, zirconia, thoria and titania by reaction with the hydrolysis product of triethoxysilane is described. The hydride containing material is then further reacted with a terminal olefin in the presence of a platinum catalyst to produce a chemically modified oxide surface which could be used as a chromatographic stationary phase. The success of this reaction is monitored by diffuse reflectance infrared Fourier transform and cross-polarization magic-angle spinning nuclear magnetic resonance spectroscopy as well as by differential scanning calorimetry. On all four oxides both the hydride intermediate and the alkyl bonded product are successfully formed via the silanization/hydrosilation reaction sequence.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 23 (1987), S. 3-6 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Allyl bonded phases ; Addition Reactions ; Synthesis of new bonded phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The presence of the double bond on the allyl moiety has been utilized as a site for addition reactions which could produce new stationary phases. Bromination and hydrobromination reactions have been employed to prove the feasibility of making modifications to the allyl bonded phase. Both retention volumes and thermodynamic parameters for the solutes studied change upon conversion to one of the brominated phases. Sample size studies are consistent with a bonded phase adsorption mechanism. FTIR spectra also confirm the modifications which have occurred on the allyl bonded material.
    Type of Medium: Electronic Resource
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