Abstract: A method of preparing a separation column, or channel in a microfabricated device, includes the steps of: providing an unfilled column, or channel in a microfabricated device; activating the inner wall of the column or channel with an activating agent; filling the column with a polymerization solution including a mixture of monomers, at least one porogen and at least one polymerization initiator; and polymerizing the mixture to form a rigid porous monolithic polymer plug in the column or channel. The monomers include a mixture of divinylbenzene as major monomer and isodecylacrylate, and the at least one porogen includes isobutanol.