Sedimentation assisted preparation of ground particles of silica monolith and their C18 modification resulting in a chromatographic phase of improved separation efficiency

Abstract

The sedimentation procedure has been adopted in production of ground silica monolith particles to improve chromatographic separation efficiency of the resultant phase. First, silica monolith particles have been successfully prepared in a large scale by a sol-gel process followed by grinding. The particles after calcination were separated by sedimentation into three zones using an Imhoff sedimentation cone. The particles of the bottom zone were derivatized with a C18 ligand and end-capped. The sedimentation process was found to not only eliminate troublesome minute particles but also narrow down the particle size distribution. The resultant phase was packed in glass lined stainless steel micro-columns. The average number of theoretical plates (N) of the columns for a test mixture was 47,000 and 29,300 for the 300 and 150mm columns (1mm internal diameter), corresponding to 157,000/m and 195,000/m, respectively.