0000000000139625
AUTHOR
A. A. Kurganov
Effect of polystyrene coating on pore, structural and chromatographic properties of silica packings
Abstract A series of mesoporous and macroporous silicas with a mean pore diameter (PD), between 6 and 200 nm were reacted with a copolymer of styrene and vinyl-methyldiethoxysilane. The mass load of coated silicas corresponded to the monolayer capacity of the polymer calculated on the basis of the molecular cross-sectional area, except for the two mesoporous silcias of PD = 6 and 7.5 nm. Depending on the pore size, changes occurred in the specific surface area, as, between the native and the coated product. A comparison of the specific pore volume, νp, of silicas before and after polymer immobilization indicated a major loss of νp for the two mesoporous silicas whereas this effect was much …
Fast Response Heating Module for Temperature Programmed GC Analysis in Microreaction Systems
For monitoring the reactant and product concentrations of a gas phase microreactor for ethylene oxide synthesis the development of a miniaturised device for fast GC analysis suitable for operation in conjunction with the microreactor is advantageous. Therefore, a method employing short (0.2 – 0.4 m) packed capillary columns was developed. Highly crosslinked polystyrene microspheres proved to be the most suitable adsorbent enabling a high separation efficiency. For fast temperature programming design concepts for an efficient heating module capable to be used with short capillary columns were developed. In principle, planar as well as cylindrical designs are suitable for integration of a res…
Separation of unmodified α-amino acid enantiomers by reverse phase HPLC
A novel chiral phase system is presented for the resolution of unmodified α-amino acid racemates which is composed of a reverse phase packing coated with N-alkyl-L-hydroxyproline (where alkyl is n-C7H15-, n-C10H21- and n-C16H33-) and a hydro-organic eluent containing copper(II)acetate. The factors controlling retention and enantioselectivity such as concentration of Cu(II)ion and pH of the eluent, addition of NH4Ac to the eluent, type and content of organic solvent of hydro-organic eluent and column temperature were examined. The extremely high enantioselectivity observed (α up to 16) is assumed to be caused by a three site sorbate-sorbent interaction involving bidentate coordination of two…
Reversed-phase high-performance liquid chromatography of proteins and polypeptides on polystyrene-coated silica supports
Abstract A new type of hydrolytically stable reversed-phase packing material prepared by multi-point covalent binding of polystyrene chains onto the surface of porous silica was examined in the high-performance liquid chromatography of proteins and polypeptides. Whereas wide-pore material was shown to give a rapid and efficient resolution of proteins, packings with smaller pores provided better selectivities for peptides.
Ion-exchange high-performance liquid chromatography of nucleotides and polypeptides on new types of ion-exchange sorbents, based on polystyrene-coated silicas.
A novel type of ion exchanger was prepared by multipoint covalent binding of polystyrene chains onto the surface of porous silica followed by polymer-analogous modification of the bonded layer. Both anion and cation exchangers were synthesized and examined in the separation of nucleotides and proteins. Rapid and efficient separation of basic polypeptides on strong anion exchangers and that of acidic polypeptides on strong cation exchangers could be achieved. For the separation of complete mixtures of polypeptides the application of zwitter-ionic ion exchangers can be recommended.
Effect of the hydrophobic spacer in bonded [Cu(l-hydroxyprolyl)alkyl]+ silicas on retention and enantioselectivity of α-amino acids in high-performance liquid chromatography
Abstract The following chiral ligands were bonded to silica: [Cu( l -hydroxyprolyl)methyl) + on LiChrosorb Si 60 (1), [Cu( l -hydroxyprolyl)methyl] + on LiChrosorb Si 100 (2) and [Cu( l -hydroxyprolyl) n -octyl] + on LiChrosorb Si 100 (3). The packings contained residual iodomethyl- and ω-iodooctyl groups at the surface. Studies on packing 1 and 2 under comparable conditions in eluents containing 10 -4 M copper acetate showed a higher retention on 1 than on 2 but a much better enantioselectivity in the latter case. The retention of enantiomers on all packings examined was found to be governed by the eluent pH and methanol content as well as by the concentration of ammonium acetate. The vari…