A totally new solid stationary phase deposition technique for micro machined gas chromatography (GC) columns fabrication was proposed: to overcome the limitations of conventional liquid (or occasionally solid) stationary phases in terms of very volatile compounds retention and/or clean room batch production, an approach consisting of the collective direct deposition of the adsorbent in micro columns channels by sputtering was performed. The process was fully compatible with clean room fabrication flow and industry-ready, with very good precision results. Silica, alumina, graphite and magnesia were proven able to separate volatile hydrocarbons. Various types of columns (structure, stationary phase) were fabricated in the form of 2x2 cm² silicon-Pyrex chips, and their thermodynamic and kinetic evaluations were reported. Retentions were observed to increase from magnesia to graphite through alumina and silica and with phase ratio decrease, as expected; very satisfying efficiencies were obtained: more than 5700 plates, and 250 µm-high plates. The possibility to use such columns for fast in-situ and autonomous monitoring of light hydrocarbons in oilfield environments was demonstrated by the implementation of a chip temperature-programming system and various versatility tests (high temperatures, carrier gas, humidity): a complete C1-C9 linear alkanes separation was performed in less than 15 seconds, as well as complex mixtures fast separations (isomers, unsaturated), and an industrial confidential application was developed and patented. Therefore, sputter-deposited stationary phase micro columns opened numerous perspectives for the developments of miniaturized GC apparatuses.
| Identifer | oai:union.ndltd.org:CCSD/oai:tel.archives-ouvertes.fr:tel-00987621 |
| Date | 05 February 2014 |
| Creators | Haudebourg, Raphael |
| Publisher | Université Pierre et Marie Curie - Paris VI |
| Source Sets | CCSD theses-EN-ligne, France |
| Language | English |
| Detected Language | English |
| Type | PhD thesis |
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