New method for development of carbon clad silica phases for liquid chromatography: Part I. Preparation of carbon phases

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Owing to its combination of unique selectivity and mechanical strength, commercial carbon clad zirconia (C/ZrO 2) has been widely used for many applications, including fast two-dimensional liquid chromatography (2DLC). However, the low surface area available (only 20-30m 2/g for commercial porous ZrO 2) limits its retentivity. We have recently addressed this limitation by developing a carbon phase coated on the high surface area of HPLC grade alumina (C/Al 2O 3). This material provides higher retentivity and comparable selectivity, but its use is still limited by how few HPLC quality types of alumina particles (e.g., particle size, surface area, and pore size) are available. In this work, we have developed useful carbon phases on silica particles, which are available in various particle sizes, pore sizes and forms of HPLC grade. To make the carbon phase on silica, we first treat the silica surface with a monolayer or less of metal cations that bind to deprotonated silanols to provide catalytic sites for carbon deposition. After Al (III) treatment, a carbon phase is formed on the silica surface by chemical vapor deposition at 700°C using hexane as the carbon source. The amount of Al (III) on the surface was varied to assess its effect on carbon deposition, and the carbon loading was varied at different Al (III) levels to assess its effect on the chromatographic properties of the various carbon adsorbents. We observed that use of a concentration of Al (III) corresponding to a full monolayer leads to the most uniform carbon coating. A carbon coating sufficient to cover all the Al (III) sites, required about 4-5 monolayers in this work, provided the best chromatographic performance. The resulting carbon phases behave as reversed phases with reasonable efficiency (50,000-79,000plates/m) for non-aromatic test species.

Original languageEnglish (US)
Pages (from-to)1359-1366
Number of pages8
JournalJournal of Chromatography A
Issue number10
StatePublished - Mar 11 2011

Bibliographical note

Funding Information:
The authors acknowledge the financial support from the National Institute of Health ( GM 054585 ). We also thank Agilent Technologies (Palo Alto, CA, USA) and ZirChrom Separations Inc. (Anoka, MN, USA) for the donation of porous silica and carbon clad zirconia, respectively, and University of Minnesota Surface Characterization Facility for the use of nitrogen sorptometer.


  • Carbon clad silica
  • Chemical vapor deposition
  • HPLC
  • Hydrolysis of urea
  • Stationary phase


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