Total-transfer, valve-based comprehensive two-dimensional gas chromatography
Total-transfer, valve-based comprehensive two-dimensional gas chromatography
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全转移、基于阀门的综合二维气相色谱法
DOI：
10.1016/j.aca.2005.08.072
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发表时间：
2006
影响因子：
6.2
通讯作者：
R. Synovec
中科院分区：
文献类型：
--
作者：
Rachel E. Mohler;B. Prazen;R. Synovec
基于阀门的综合二维气相色谱 (GC×GC) 是最紧凑、坚固且廉价的 GC×GC 仪器设计之一。基于阀门的调制配置的主要缺点在于检测灵敏度降低。这种灵敏度损失是因为在典型的操作条件下，转移到第二根柱（即柱 2）的第一根柱（即柱 1）流出物的比例可能约为 5-10%。为了解决这种灵敏度损失问题，我们开发了一种独特的全传输（即 100%）基于阀门的 GC×GC，且不会增加仪器的复杂性。新的仪器设计依赖于简单地阻塞高速六通隔膜阀的适当端口之一，该阀门用作色谱柱 1 和 2 之间的调制器。调制周期和色谱柱 1 和 2 之间的压头差是两个主要变量，通过控制它们可以提供良好的检测灵敏度以及从色谱柱 1 到色谱柱 2 的 100% 传质。调制周期越长，检测灵敏度越好。辛烷的检测限为 0.03ng/μl。这种灵敏的 GC×GC 配置还显示出可以提供可接受的分离峰容量，对真正的复杂样品（汽油和桉树油）实现了良好的分离，其中化合物分布在大部分二维分离空间中。原则上，这种全传输、基于阀门的 GC×GC 比目前可用的 GC×GC 仪器更便携且更便宜。
Valve-based comprehensive two-dimensional gas chromatography (GC×GC) is one of the most compact, robust, and inexpensive GC×GC instrument designs. The major drawback of a valve-based modulation configuration lies in diminished detection sensitivity. This loss in sensitivity is because under typical operating conditions the fraction of the first column (i.e., column 1) effluent transferred to the second column (i.e., column 2) is likely to be ∼5–10%. To address this loss in sensitivity, we report the development of a unique total-transfer (i.e., 100%) valve-based GC×GC, without adding complexity to the instrumentation. The new instrument design relies upon simply blocking one of the appropriate ports of the high-speed six-port diaphragm valve that is used as the modulator between columns 1 and 2. The modulation period and difference in head pressure between columns 1 and 2 are found to be the two primary variables that are controlled to provide good detection sensitivity and 100% mass transfer from column 1 to column 2. The detection sensitivity is better with a longer the modulation period. A limit of detection of 0.03ng/μl was obtained for octane. This sensitive GC×GC configuration is also shown to provide acceptable separation peak capacity, with good separations achieved for real complex samples: gasoline and Eucalyptus oil, where compounds were spread out over much of the two-dimensional separation space. In principle, this total-transfer, valve-based GC×GC is more portable and less expensive than currently available GC×GC instrumentation.
影响因子：
7.4
作者：
GIDDINGS, JC
通讯作者：
GIDDINGS, JC