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High-performance, static-coated silicon microfabricated columns for gas chromatography.

Authors
Reidy-S; Lambertus-G; Reece-J; Sacks-R
Source
Anal Chem 2006 Apr; 78(8):2623-2630
NIOSHTIC No.
20031920
Abstract
A procedure is described for the preparation of high-performance etched silicon columns for gas chromatography. Rectangular channels, 150 mum wide by 240 mum deep are fabricated in silicon substrates by gas-phase reactive ion etching. A 0.1-0.2-mum-thick film of dimethyl polysiloxane stationary phase is deposited on the channel walls by filling the channel with a dilute solution in 1:1 n-pentane and dichloromethane and pumping away the solvent. A thermally activated cross-linking agent is used for in situ cross-linking. A 3-m-long microfabricated column generated approximately 12 500 theoretical plates at optimal operating conditions using air as carrier gas. A kinetic model for the efficiency of rectangular cross-section columns is used to evaluate column performance. Results indicate an additional source of gas-phase dispersion beyond longitudinal diffusion and nonequilibrium effects, probably resulting from numerous turns in the gas flow path through the channel. The columns are thermally stable to at least 180 degrees C using air carrier gas. Temperature programming is demonstrated for the boiling point range from n-C5 to n-C12. A 3.0-m-long column heated at 10 degrees C/min obtains a peak capacity of over 100 peaks with a resolution of 1.18 and a separation time of approximately 500 s. With a 0.25-m-long column heated at 30 degrees C/min, a peak capacity of 28 peaks is obtained with a separation time of 150 s. Applications are shown for the analysis of air-phase petroleum hydrocarbons and the high-speed analysis of chemical warfare agent and explosive markers.
Keywords
Organic-compounds; Analytical-chemistry; Analytical-methods; Analytical-processes; Analytical-instruments; Gases; Chemical-warfare-agents; Chemical-reactions; Explosive-gases
Contact
Department of Chemistry, University of Michigan, Ann Arbor, Michigan 48109
CODEN
ANCHAM
Publication Date
20060415
Document Type
Journal Article
Funding Type
Grant
Fiscal Year
2006
NTIS Accession No.
NTIS Price
Identifying No.
Grant-Number-R01-OH-003692
Issue of Publication
8
ISSN
0003-2700
Source Name
Analytical Chemistry
State
MI
Performing Organization
University of Michigan, Ann Arbor
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