Reproducibility and Efficiency of Columns Packed with 10 Silica in Liquid Chromatography

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Abstract
Stainless steel tubes are drilled and afterwards packed with 10 µ silica. Such columns (i.d., 4.2 mm) are packed by a balanced density method within 15–30 minutes. The peaks are more symmetrical and the reproducibility of column packing is much better if drilled tubes rather than undrilled are used. The use of dispersing agents with high viscosities (40–60 cP) and with densities around 1 g/ml is proposed. This viscosity packing method is especially advantageous if reversed or chemically bonded stationary phases are used or if the adsorption of bromine (from tetrabromoethane) is to be avoided. The efficiencies of columns packed in different tube materials (glass included) are compared by tabulating the constants of the h = A + Cu equation. With a linear velocity of 2 cm sec, up to 100 theoretical plates are generated per second. In excellent columns packed with silica the efficiencies are, to a rough approximation, independent of the capacity ratios of the compounds to be separated.

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