Stadermann Michael, McBrady Adam D, Dick Brian, Reid Vanessa R, Noy Aleksandr, Synovec Robert E, Bakajin Olgica
Chemistry & Material Science, Lawrence Livermore National Laboratory, Livermore, California 74550, USA.
Anal Chem. 2006 Aug 15;78(16):5639-44. doi: 10.1021/ac060266+.
The key to rapid temperature programmed separations with gas chromatography are a fast, low-volume injection and a short microbore separation column with fast resistive heating. One of the major problems with the reduction of column dimensions for micro gas chromatography is the availability of a stationary phase that provides good separation performance. In this report, we present the first integration of single-wall carbon nanotubes (SWNTs) as a stationary phase into 100 mum x 100 mum square and 50-cm-long microfabricated channels. The small size of this column with integrated resistive heater and the robustness of the SWNT phase allow for fast temperature programming of up to 60 degrees C/s. A combination of the fast temperature programming and the narrow peak width of small-volume injections that can be obtained from a high-speed, dual-valve injection system allows for rapid separations of gas mixtures. We demonstrate highly reproducible separations of four-compound test mixtures on these columns in less than 1 s using fast temperature programming.
实现气相色谱快速程序升温分离的关键在于快速、小体积进样以及配备快速电阻加热装置的短微径分离柱。微型气相色谱柱尺寸减小面临的主要问题之一是找到一种能提供良好分离性能的固定相。在本报告中,我们首次将单壁碳纳米管(SWNTs)作为固定相集成到100μm×100μm方形且50厘米长的微加工通道中。这种集成了电阻加热器的小尺寸色谱柱以及SWNT固定相的稳健性使得程序升温速度可达60℃/秒。快速程序升温和从小体积进样中获得的窄峰宽(可通过高速双阀进样系统实现)相结合,能够快速分离气体混合物。我们通过快速程序升温在不到1秒的时间内,在这些色谱柱上实现了四种化合物测试混合物的高度可重复分离。