Assessing the reliability of wall-coated microfabricated gas chromatographic separation columns

被引:57
作者
Serrano, Gustavo [1 ,2 ]
Reidy, Shaelah M. [2 ,3 ]
Zellers, Edward T. [1 ,2 ,3 ]
机构
[1] Univ Michigan, Dept Environm Hlth Sci, Ann Arbor, MI 48109 USA
[2] Univ Michigan, Engn Res Ctr Wireless Integrated Microsyst, Ann Arbor, MI 48109 USA
[3] Univ Michigan, Dept Chem, Ann Arbor, MI 48109 USA
来源
SENSORS AND ACTUATORS B-CHEMICAL | 2009年 / 141卷 / 01期
基金
美国国家科学基金会;
关键词
MEMS; Gas chromatography; Microcolumn; Micro-GC; Stationary phase; Deactivation; Thermal stability; VOLATILE ORGANIC-COMPOUNDS; SILICA CAPILLARY COLUMNS; VACUUM-OUTLET GC; MOBILITY SPECTROMETER; HIGH-PERFORMANCE; AIR; MEMS; DEACTIVATION; PHASE; SELECTIVITY;
D O I
10.1016/j.snb.2009.05.003
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
This study addresses several aspects of etched-silicon/glass microfabricated channels that affect their performance as micro-gas chromatographic (mu GC) separation columns, including the consistency of stationary phase deposition, deactivation of surface-adsorption sites on the microcolumn walls, and the stability of the stationary phase following repeated thermal cycling. Convolved square-spiral micro-columns 0.5-3-m long with cross sections of 150 mu m x 240 mu m consisting of deep-reactive-ion-etched (DRIE) Si with anodically bonded Pyrex caps are used. Replicate devices with wall-coated films of the non-polar polydimethylsiloxane (PDMS) or the moderately polar poly(trifluoropropylmethyl)siloxane (PTFPMS) deposited statically to a nominal thickness of 0.15 mu m provide minimum plate heights that are reproducible to 5% in air or helium carrier gases. Using split-flow injection, 4900 theoretical plates/m can be produced and a 19-vapor mixture can be separated on a 0.5-m PDMS-coated Column in air in less than 3.5 min. Significant reductions in peak tailing of polar analytes are afforded by surface pre-treatment or post-treatment with the deactivation agent hexamethyldisilazane (HMDS). In addition, retention times remain stable and peak widths remain stable or decrease after prolonged pre-conditioning at 200 degrees C in air. Non-pretreated PTFPMS-coated microcolumns can produce 2300 plates/m and also retain high resolution after pre-conditioning at 200 degrees C in air. Marginal improvements in separation efficiency are achieved by pre-treatment with trifluoropropylmethylcyclotrisiloxane. Results demonstrate that efficient mu GC columns with polar and non-polar stationary phases can be made reproducibly and operated at elevated temperatures in air. (C) 2009 Elsevier B.V. All rights reserved.
引用
收藏
页码:217 / 226
页数:10
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