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用于低资源台式全二维气相色谱仪的柱上加热及电阻加热、液冷式热调制器。

At-column heating and a resistively heated, liquid-cooled thermal modulator for a low-resource bench-top GC x GC.

作者信息

Libardoni Mark, Hasselbrink Ernest, Waite J Hunter, Sacks Richard

机构信息

Department of Chemistry, University of Michigan, Ann Arbor, MI, USA.

出版信息

J Sep Sci. 2006 May;29(7):1001-8. doi: 10.1002/jssc.200500298.

Abstract

A transportable GC x GC instrument is under development for on-site applications that would benefit from the enhanced resolution and powers of detection, which can be achieved by this method. In the present study, a low-resource GC x GC instrument using an electrically heated and liquid-cooled single-stage thermal modulator that requires no cryogenic materials is evaluated. The instrument also uses at-column heating, thus eliminating the need for a convection oven to house the two columns. The stainless-steel modulator tube is coated with PDMS, which can be heated to 350 degrees C for sample injection into the second-dimension column. The modulator is cooled to -30 degrees C by a 100 mL/min flow of PEG by means of a commercial liquid chiller and a small recirculating pump. Resistive heating of the modulator tube is provided by a programmable power supply, which uses a voltage program that results in increasing modulator temperature during an analysis. This, together with more rapid cooling by the use of a liquid cooling medium, results in reduced solute breakthrough following each heating cycle as the modulator cools to a temperature where quantitative trapping resumes. As a result, modulated peak widths at half-height of less than 40 ms are observed. Design and performance details are presented along with chromatograms of gasoline and an essential oil sample.

摘要

一种可移动的全二维气相色谱仪正在研发中,用于现场应用,这种应用可受益于该方法所能实现的更高分辨率和检测能力。在本研究中,对一种低资源全二维气相色谱仪进行了评估,该仪器使用电加热和液冷的单级热调制器,无需低温材料。该仪器还采用柱上加热,因此无需使用对流烘箱来放置两根色谱柱。不锈钢调制管涂有聚二甲基硅氧烷(PDMS),可加热到350摄氏度,以便将样品注入第二维色谱柱。通过商用液体冷却器和小型循环泵,借助100毫升/分钟的聚乙二醇(PEG)流将调制器冷却至零下30摄氏度。调制管的电阻加热由可编程电源提供,该电源使用电压程序,在分析过程中使调制器温度升高。这与使用液体冷却介质进行更快冷却相结合,使得在调制器冷却至定量捕集恢复的温度时,每个加热循环后的溶质穿透减少。结果,观察到半高调制峰宽小于40毫秒。文中介绍了该仪器的设计和性能细节,以及汽油和香精油样品的色谱图。

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