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5.2.5. Long monolithic columns Since monolithic columns are known to exhibit a much higher permeability than packed columns having a similar separation power, their use to prepare long, highly efficient columns seems very attactive. Unfortunately, monolithic silica rods shrink during their preparation. This shrinking generates considerable internal stress in the material and at the interface between the rod and the silica tube in which it could be prepared. The interface does not stand the stress and snaps, causing leaks between the rod and the wall, letting the mobile phase bypass the monolithic bed and resulting in a large loss of retention and efficiency. Large monolith are prepared in a mold, in such a way that they do not stick to a wall, are dried, and then are encapsulated in a plastic (e.g., PEEK) tubing providing an excellent column. However, the rods are brittle. They cannot be prepared straight, so only relatively short columns are prepared in this way. Although they can be connected into longer columns, it does not seem practical to prepare long, highly efficient columns by connecting dozens of 10 cm long columns, especially due to the limited pressure that a PEEK tube can withstand. If the monolith is prepared in a capillary tube, however, the stress becomes insufficient to break the interface between the tube wall and the monolith and long capillary columns can be prepared [12,29]. Columns of various lengths and having 50¨C 100m i.d. were prepared. Their permeability is far higher than that of conventional columns packed with 5m particles but their efficiency is comparable with that of these columns. This would make possible the preparation and the use with conventional pumps of columns having lengths of several meters and very high efficiencies. |
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