0000000000049431
AUTHOR
U. Esser
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.
Evaluation of advanced silica packings for the separation of biopolymers by high-performance liquid chromatography
Abstract The linear solvent strength model of Snyder was applied to describe fast protein separations on 2.1-μm non-porous, silica-based strong anion exchangers. It was demonstrated on short columns packed with these anion exchangers that (i) a substantially higher resolution of proteins and nucleotides was obtained at gradient times of less than 5 min than on porous anion exchangers; (ii) the low external surface area of the non-porous anion exchanger is not a critical parameter in analytical separations and (iii) μg-amounts of enzymes of high purity and full biological activity were isolated.
Packing technology, column bed structure and chromatographic performance of 1-2-μm non-porous silicas in high-performance liquid chromatography
This work is aimed at further elucidating the aggregation behaviour of micron- and submicron-size non-porous silicas and the column performance of 1–2-μm C18 silicas in reversed-phase high-performance liquid chromatography of low-molecular weight compounds. It is demonstrated that highly ordered, dense, porous aggregates of such silica beads were obtained by gravity settling and centrifugation. The slurry techniques applied at constant flow-rate and a pressure up to 50 MPa provided less-ordered aggregates, but generated an acceptable performance of columns when 1–2-μm C18 silica beads were employed. To operate columns of 53 mm × 4.6 mm I.D., the maximum flow-rate needs to be ca. 2.5 ml/min …
Hysteresis in nitrogen sorption and mercury porosimetry on mesoporous model adsorbents made of aggregated monodisperse silica spheres
Abstract An elucidation of the hysteresis phenomena in nitrogen sorption (NS) and mercury porosimetry (MP) on porous aggregates of non-porous silica spheres of particle diameter 90–1000 nm is presented. First, it is demonstrated that highly ordered and dense aggregates of a porosity of 26–30% are formed by gravity settling and centrifugation. A hexagonal and cubic close-packed structure within the layers and a vertical stacking between the layers were observed. Minor deteriorations were seen between the ordered domains. Second, the pore size distribution (PSD) curves calculated from the adsorption branch of the nitrogen isotherms by means of the Cohan equation and from the desorption branch…