A Graphitized-Carbon Monolithic Column
- 12 August 2003
- journal article
- research article
- Published by American Chemical Society (ACS) in Analytical Chemistry
- Vol. 75 (18), 4904-4912
- https://doi.org/10.1021/ac030146r
Abstract
The preparation of a novel carbon monolithic column for high performance liquid chromatography is described. A phenolic resin rod with embedded 10-μm silica beads was prepared by acid-catalyzed polymerization of a resorcinol/iron(III) complex and formaldehyde. This rod was carbonized and graphitized under inert atmosphere with a programmed temperature cycle from room temperature to 1250 °C. Subsequently, the silica beads along with iron catalysts were removed, leaving a porous carbon rod. Imaging of this monolithic rod by scanning and transmission electron microscopies revealed a highly interconnected bimodal porous structure. The porosity and pore size distribution of the mesopores were characterized by N2 absorption/desorption. Graphene sheets were found in the TEM images of the carbon rod, and the graphite index was characterized by Raman spectrum and X-ray diffraction. A monolithic column prepared with the aforementioned carbon rod was evaluated using a mixture of alkylbenzenes. It exhibited an excellent separation power and a low hydraulic resistance. The bundle-of-capillaries model was used to characterize the hydrodynamics of this monolith. Its permeability was found to agree well with the theoretical one.Keywords
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