Silica-based monolithic capillary columns-Effect of preparation temperature on separation efficiency

J Chromatogr A. 2010 Sep 3;1217(36):5737-40. doi: 10.1016/j.chroma.2010.07.010. Epub 2010 Jul 15.

Abstract

The temperature effects during the sol-gel process and ageing of the silica-based monolith on the structure and separation efficiency of the capillary columns (100microm i.d., 150mm) for HPLC separations were studied. The tested columns were synthesized from a mixture of tetramethoxysilane, polyethylene glycol and urea under the acidic conditions. The temperature was varied from 40 degrees C to 44 degrees C and formation of bypass channels between the silica mold and the capillary wall was examined. The temperature of 43 degrees C was estimated as optimal for preparation of efficient silica capillary columns which were subsequently modified by octadecyldimethyl-N,N-diethylaminosilane or covered by poly(octadecyl methacrylate) and tested using standard mixture of alkylbenzenes under the isocratic conditions.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Benzene Derivatives / chemistry
  • Chromatography, High Pressure Liquid / methods*
  • Hydrogen-Ion Concentration
  • Microscopy, Electron, Scanning
  • Phase Transition
  • Polyethylene Glycols / chemistry
  • Silanes / chemistry
  • Silicon Dioxide / chemistry*
  • Temperature
  • Urea / chemistry

Substances

  • Benzene Derivatives
  • Silanes
  • Polyethylene Glycols
  • tetramethoxysilane
  • Silicon Dioxide
  • Urea