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使用热梯度气相色谱进行峰扫描和门控。

Peak sweeping and gating using thermal gradient gas chromatography.

机构信息

Department of Chemistry and Biochemistry, Brigham Young University, Provo, UT 84602, USA.

出版信息

J Chromatogr A. 2013 Feb 22;1278:160-5. doi: 10.1016/j.chroma.2013.01.010. Epub 2013 Jan 9.

DOI:10.1016/j.chroma.2013.01.010
PMID:23352829
Abstract

When axial temperature gradients are applied in gas chromatography (GC), i.e., "thermal gradient GC" (TGGC), the temperature changes both in time and position, T(t,L), along the column, allowing unique control of the movement and elution of sample components. One method of performing TGGC involves introducing a sample into a column with a preset decreasing temperature gradient along its length, waiting for a short time until the sample separates along the gradient, and then raising the temperature to sweep all of the compounds out of the column and into the detector (i.e., "peak sweeping"). This method of operation is demonstrated here using a simple laboratory apparatus based on simultaneous resistive heating and convective cooling. An experimental comparison between isothermal GC (ITGC), temperature programmed GC (TPGC) and TGGC shows that TGGC is essentially equivalent in performance to TPGC operation when using the same column length (peak capacity production rate of 106, 381 and 469 min(-1), respectively); however, narrower peaks and higher signal-to-noise are achieved in TGGC. Furthermore, TGGC helps to minimize band broadening and peak tailing that arise from column adsorption and less than perfect sample injection. The low thermal mass of the TGGC system allows rapid column heating (4000°C/min) and cooling (3500°C/min) for selective separation (i.e., "peak gating") of compounds in a mixture without sacrificing the resolution of earlier or later eluting compounds.

摘要

当在气相色谱(GC)中应用轴向温度梯度时,即“热梯度 GC”(TGGC),温度会随时间和位置而变化,T(t,L),沿柱变化,从而可以独特地控制样品组分的运动和洗脱。执行 TGGC 的一种方法是将样品引入具有沿其长度预设降低温度梯度的柱中,等待短时间,直到样品沿梯度分离,然后升高温度以将所有化合物从柱中扫出并进入检测器(即“峰扫出”)。这里使用基于电阻加热和对流冷却的简单实验室仪器演示了这种操作方法。等温 GC(ITGC)、程序升温 GC(TPGC)和 TGGC 的实验比较表明,当使用相同的柱长时,TGGC 在性能上与 TPGC 操作基本等效(峰容量生产率分别为 106、381 和 469 min(-1));然而,TGGC 可实现更窄的峰和更高的信噪比。此外,TGGC 有助于最小化由于柱吸附和不完全样品注入引起的带宽展宽和峰拖尾。TGGC 系统的低热质量允许对混合物中的化合物进行快速选择性分离(即“峰门控”),而不会牺牲较早或较晚洗脱化合物的分辨率,柱加热(4000°C/min)和冷却(3500°C/min)速度非常快。

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