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Horizontal polymerization of mixed trifunctional silanes on silica. 2. Application to chromatographic silica gel

Journal Article · · Analytical Chemistry (Washington); (United States)
DOI:https://doi.org/10.1021/ac00054a029· OSTI ID:6078345
;  [1]
  1. Univ. of Delaware, Newark (United States)
A new surface bonding scheme for monolayers on silica recently reported was designed to combine the superior hydrolytic stability of self-assembled monolayers with the selectivity and reproducibility of monomeric stationary phases. In this work, the scheme is shown to work very effectively for chromatographic silica gel. A mixture of CH[sub 3](CH[sub 2])[sub 17]SlCl[sub 3] and CH[sub 3](CH[sub 2])[sub 2]SlCl[sub 3] is horizontally polymerized onto 40- and 50-[mu]m-diameter porous silica gel particles. [sup 13]C NMR and microanalysis are used to establish that a coverage consistent with horizontal polymerization is achieved. The chromatographic retention behavior of a set of test solutes is shown to be similar to that for conventional monomeric C[sub 18] phases. The repeated synthesis of the new phase is shown to give reproducible retention times for benzo[a]pyrene and aniline. The hydrolytic stability is demonstrated to be greatly improved over that of a monomeric C[sub 18] stationary phase: the new phase is stable to at least 2,400 column volumes of pH 1.8 solution and stable to at least 900 column volumes of pH 10.0 solution. 20 refs., 6 figs., 3 tabs.
OSTI ID:
6078345
Journal Information:
Analytical Chemistry (Washington); (United States), Journal Name: Analytical Chemistry (Washington); (United States) Vol. 65:6; ISSN 0003-2700; ISSN ANCHAM
Country of Publication:
United States
Language:
English