Design, fabrication, and microfabricated columns evaluation of for gas chromatography

Design, fabrication, and microfabricated columns evaluation of for gas chromatography
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DOI:
10.1021/ac030367x
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发表时间:
2004-05-01
影响因子:
7.4
通讯作者:
Sacks, R
Sacks, R
中科院分区:
化学1区
文献类型:
--
作者:
Lambertus, G;Elstro, A;Sacks, R

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描述了在硅衬底上蚀刻的气相色谱柱的设计、制造和性能。深反应离子蚀刻形成3米长,150微米宽,240微米深的矩形截面通道。将玻璃盖板阳极结合到基板的剩余表面,形成气密通道。对于一些柱,在用玻璃板密封通道之前氧化硅通道。将熔融二氧化硅毛细管连接管密封到3.2-cm X 3.2-cm衬底芯片边缘上的端口中。采用动态涂敷法在非极性二甲基聚硅氧烷或中等极性三氟丙基甲基聚硅氧烷固定相上沉积一层存款。在具有分流进样和火焰离子化检测的常规台式GC仪器中评价柱。使用氢气和空气作为载气,通过使用相当于理论塔板的高度对平均载气速度的图来评价柱效率。在平均载气速度下测量的理论塔板数给出最小塔板高度,对于二甲基聚硅氧烷柱为4600至8200个塔板,对于三氟丙基甲基聚硅氧烷柱为3500至5500个塔板。以空气为载气时,最小塔板高度明显较小。对于非极性相,对于两种载气,未氧化的表面比氧化的表面给出了类似于1500个板。对于极性相,氧化表面比未氧化表面多出约200个板。20组分的多功能混合物的等温色谱图和正构烷烃混合物的程序升温色谱图。
The design, fabrication, and performance of gas chromatography columns etched in silicon substrates are described. Deep reactive-ion etching formed the 3-m-long, 150-mum-wide, 240-mum-deep rectangular cross section channels. A glass cover plate was anodically bonded to the remaining surface of the substrate forming the gastight channel. For some of the columns, the silicon channels were oxidized before the channels were sealed with the glass plates. Fused-silica capillary connecting tubes were sealed into ports on the edge of the 3.2-cm x 3.2-cm substrate chips. Dynamic coating was used to deposit a film of nonpolar dimethyl polysiloxane or moderately polar trifluoropropyhnethyl polysiloxane stationary phase. The columns were evaluated in a conventional benchtop GC instrument with split injection and flame ionization detection. Column efficiency was evaluated by the use of plots of height equivalent to a theoretical plate versus average carrier gas velocity using both hydrogen and air as carrier gases. The number of theoretical plates measured at the average carrier gas velocity giving the minimum plate height ranged from 4600 to 8200 plates for the dimethyl polysiloxane columns and from 3500 to 5500 plates for the trifluoropropyhnethyl polysiloxane columns. Minimum plate height was significantly smaller with air as carrier gas. For the nonpolar phase, the nonoxidized surface gave similar to1500 plates more than the oxidized surface for both carrier gases. For the polar phase, the oxidized surface gave similar to200 plates more than the nonoxidized surface. Isothermal chromatograms of a 20-component multifunctional mixture and temperature-programmed chromatograms of a normal alkane mixture are presented.