A new type of monolithic stationary phase was prepared within the confines
of fused-silica tubing by in situ polymerization of divinylbenzene or ethyl
ene dimethacrylate either with styrene or butyl methacrylate. The porosity
of the monolith was dictated by silica beads packed in the capillary prior
to flushing the column with the monomeric solution. Subsequent washing of t
he polymeric rod with sodium hydroxide rendered a porous monolith that was
used for both micro-LC and capillary electrochromatography. The novelty of
the approach presented herein lies in preparing the polymer within the conf
ines of a fused-silica capillary. The challenges posed in this new context
and their resolution are presented in detail. In addition, this study propo
ses that in addition to tailoring the pore size, the silica beads, through
their surface chemistry, can influence the surface characteristics of the f
inished polymer monolith. For example, the data suggests that octadecyl mod
ified silica particles interacted with hydrophobic moieties of monomers bef
ore initiation of polymerization, thus dictating their orientation in the r
esulting polymer. (C) 2001 Elsevier Science B.V. All rights reserved.