Synthesis and characterization of endcapped C 18 stationary phases using a silica hydride intermediate

Abstract

The effect of endcapping on an octdecyl bonded phase synthesized by the silanization/hydrosilation method is investigated. The endcapping reagent is a 1:1 molar ratio of trimethylchlorosilane (TMCS) and hexamethyldisilizane (HMDS). Two approaches for endcapping are possible for this synthetic method that produces a silica hydride intermediate: bonding of TMCS–HMDS after silanization (on the hydride intermediate) or after hydrosilation (on the C 18 product stationary phase). The use of TMCS–HMDS is designed to eliminate the few remaining silanols on the silica hydride intermediate. The endcapping process is characterized spectroscopically by diffuse reflectance infrared Fourier transform (DRIFT), 29Si cross polarization magic angle spinning nuclear magnetic resonance spectroscopy (CP-MAS-NMR) and 13C-CP-MAS-NMR. The octadecyl bonded phases are characterized chromatographically by measuring the capacity factors of several hydrophobic and basic test solutes as well as the separation factors among various solute pairs. Finally, long-term stability tests are done on both products at high and low pH.