A graphitized-carbon monolithic column

被引:134
作者
Liang, CD
Dai, S [1 ]
Guiochon, G
机构
[1] Univ Tennessee, Dept Chem, Knoxville, TN 37996 USA
[2] Oak Ridge Natl Lab, Div Chem Sci, Oak Ridge, TN 37831 USA
关键词
D O I
10.1021/ac030146r
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
The preparation of a novel carbon monolithic column for high performance liquid chromatography is described. A phenolic resin rod with embedded 10-mum 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 degreesC. 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 N-2 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.
引用
收藏
页码:4904 / 4912
页数:9
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