In situ crosslinked polybutadiene-encapsulated zirconia as a monolithic column for fast solvating gas chromatography
✍ Scribed by Qinglin Tang; Yufeng Shen; Naijing Wu; Milton L. Lee
- Publisher
- John Wiley and Sons
- Year
- 1999
- Tongue
- English
- Weight
- 169 KB
- Volume
- 11
- Category
- Article
- ISSN
- 1040-7685
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✦ Synopsis
A new monolithic column type was developed by crosslinking polymerencapsulated packing materials in polymer-coated fused silica open tubular columns in situ using a free radical reaction. A 25 cm = 250 m i.d. PSB-Octyl fused silica capillary column coated with a 0.25-m film of polyoctylmethylsiloxane was packed Ž with 3% polybutadiene-encapsulated zirconia packing materials 2.5 m, 250 A, 2 y1
. 30 m g . The packing material was immobilized using a dynamic crosslinking reaction at 260ЊC with azo-tert-butane as a free radical initiator. A scanning electron micrograph of the crosslinked packing in the column showed that the particles were interconnected to each other and attached to the capillary wall, forming a monolith. This monolithic column was found to be stable in carbon dioxide mobile phase at 200 atm column inlet pressure and 260ЊC. The column efficiency, solute retention, and permeability of the monolithic column were similar to those measured for columns freshly packed, but not crosslinked, with the same material under the same conditions. The potential use of these monolithic columns for fast solvating gas chromatography was demonstrated by the rapid separation of a mixture of hydrocarbons.