0000000000049429

AUTHOR

Johan C. Kraak

Hydrodynamic chromatography of macromolecules on 2 μm non-porous spherical silica gel packings

Non-porous spherical 2μm silica gel particles have been tested as packing for hydrodynamic chromatography of macromolecules (HDC). Columns packed with these particles in 250×4.6mm i.d. columns can be operated very efficiently (e.g. a reduced plate height of about 2) when the detection cell is miniaturized. The packing is suitable for the separation of polystyrenes of Mw of 104–107 by hydrodynamic chromatography and the retention behaviour of polystyrenes agrees well with the known theoretical models. Preliminary results on the applicability of HDC for the separation of biopolymers are presented.

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The application of porous silica layers in open tubular columns for liquid chromatography

Two methods to realize a porous retentive silica layer on the inner wall of 10–25 µm fused silica capillaries for OTLC, etching and precipitation of silica from solution, have been investigated. Etching of the fused silica capillaries with 1M KOH, creates an activated surface, but the capacity of the silica layer is too small to serve as retentive layer in OTLC. Better prospects are offered by the precipitation of silica from a solution of polyethoxysiloxane, dynamically coated on the inner wall of the fused silica capillary. It appears to be possible to deposite a porous silica layer up to 0.8 µm thick (in a 25 µm capillary) by this method, which seems to be suitable for liquid-solid an dy…

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Hydrodynamic chromatography of macromolecules on small spherical non-porous silica particles

Abstract Non-porous silica spheres with sizes in the range 1.4–2.7 μm were applied as packings for the hydrodynamic chromatography (HDC) of macromolecules. Highly efficient columns, with a reduced plate height below 2, were packed with these small particles. Up to molecular weights of 10 6 the elution behaviour of polystyrenes agreed very well with existing theoretical models. However, for larger polystyrenes the flow-rate exerted an influence on the relative peak positions. The applicability of HDC to rapid separations of soluble macromolecules and inorganic colloids was demonstrated.

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Performance of porous silica layers in open-tubular columns for liquid chromatography

Abstract Progress has been made in the preparation of porous silica layers in fused-silica capillaries for open-tubular liquid chromatography. The porous silica layer is prepared by (i) static coating of the silica precursor, polyethoxysiloxane (PES), followed by (ii) converting the PES film into a porous silica layer with ammonia solution. The porous silica layer can be easily modified by silane reagents commonly used in packed column high-performance liquid chromatography. The performance of the silica layer with the different phase systems was tested with polyaromatic hydrocarbons and derivatized amino acids as samples.

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