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Preparation of silanized silica with high ligand density. The effect of silane structure

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Summary

A wide-pore silica for HPLC with a particle size of 7.5 μm, specific surface area of 360m2/g, pore diameter of 20 nm and pore volume of 2.1 cm3/g was silanized with n-octadecyldimethyl-chlorosilane (ODMCS), n-octadecyldimethylmetoxysilane (ODMMS) and n-octadecyldimethyl-dimethylaminosilane (ODMAS), in sealed glass ampoules. The ligand density obtained with an excess of ODMCS and ODMMS was found to be limited by reaction equilibrium; at low (<50%) conversion of the surface silanols, the reaction displays pseudo-first-order kinetics. Silanization with ODMAS, which seems to be sterically controlled at higher conversions, yields a relatively high concentration of bonded octadecyl ligands (4.24μmol/m2).

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Authors and Affiliations

  1. Polymer Institute, CCR, Slovak Academy of Sciences, CS-842 36, Bratislava, Czechoslovakia

    B. Buszewski & D. Berek

  2. Water Research Institute, CS-160 62, Prague, Czechoslovakia

    L. Nondek

  3. Department of Organic Chemistry, Faculty of Chemical Technology, Slovak Technical University, CS-812 37, Bratislava, Czechoslovakia

    A. Jurášek

Authors
  1. B. Buszewski
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  2. L. Nondek
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  3. A. Jurášek
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  4. D. Berek
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Additional information

Present adress: Department of Chemical Physics, Institute of Chemistry, Maria Curie-Sktodowska University, Pl-20 031 Lublin, Poland.

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Buszewski, B., Nondek, L., Jurášek, A. et al. Preparation of silanized silica with high ligand density. The effect of silane structure. Chromatographia 23, 442–446 (1987). https://doi.org/10.1007/BF02311822

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  • DOI: https://doi.org/10.1007/BF02311822

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