A new method of preparing stationary phases for packed capillary colum
n supercritical fluid chromatography (SFC) is presented. Surface deact
ivation of silica particles was carried out by dehydrocondensation of
the silicon hydride groups in polymethylhydrosiloxane with the silanol
groups on the silica surface. The deactivated particles were then coa
ted with a thin film of SE-54 stationary phase. The coated layer was i
mmobilized by a crosslinking reaction between the methyl groups of the
surface-bonded polymethylhydrosiloxane and the SE-54 stationary phase
using dicumyl peroxide as a free radical initiator. With these two re
actions, the polar groups on the silica surface were more completely c
apped than with bonding only a monomolecular polymeric layer on the si
lica surface. The SFC performance of the newly developed packing mater
ials was evaluated using a standard polarity mixture, a series of fatt
y acid methyl esters, a peppermint oil, and several high-molecular-mas
s and complex polymers.