The Dow Chemical Company

Rudolph H Stehl

Terry J Nestrick

Improved packings for columns useful in gas chromatography are made by a multistep process whereby polysiloxane molecules having various organic substituents are chemically bonded to the surface of a siliceous support. The process comprises one or more cycles of successive reactions with an activated support surface of silicon tetrachloride, an organic dichlorosilane, silicon tetrachloride a second time, a polysiloxane polyol, with intermediate hydrolyses where appropriate to provide reactive terminal silanol groups and a final capping reaction with an organic monochlorosilane. The packing as so prepared is further improved by coating with a conventional stationary phase.

Chromatographic column packing having a bonded organosiloxane coating

Highly effective chromatographic column packings are prepared by reacting hydroxyl groups on a silica surface with SiCl.sub.4 and then reacting the chlorosilylated surface with a polyglycol or polymeric glycol ester in a slurry reaction. Residual chlorosilane groups on the reacted surface are neutralized by reaction with methanol or other lower alkanol. The resulting modified silica has a bonded, essentially monomolecular organic surface film which provides thermal stability, uniform efficiency, and rapid analysis when the material is used as a column packing in gas-liquid chromatography.

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Midland, MI, United States of America

Rudolph H Stehl