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Effect of Thermal Desorption Kinetics on Vapor Injection Peak Irregularities by a Microscale Gas Chromatography Preconcentrator

机译:微型气相色谱预浓缩器对热解吸动力学对蒸汽注入峰不规则性的影响

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摘要

Microscale gas chromatography ((mu)GC) is an emerging analytical technique for in situ analysis and on-site monitoring of volatile organic compounds (VOCs) in moderately complex mixtures. One of the critical subcomponents in a (mu)GC system is a microfabricated preconcentrator (mu-preconcentrator), which enables detection of compounds existing in indoor/ambient air at low ((approx)sub ppb) concentrations by enhancing their signals. The prevailing notion is that elution peak broadening and tailing phenomena resulting from undesirable conditions of a microfabricated separation column (mu-column) are the primary sources of poor chromatographic resolution. However, previous experimental results indicate that the resolution degradation still remains observed for a mu-column integrated with other (mu)GC subcomponents even after setting optimal separation conditions. In this work, we obtain the evidence that the unoptimized mu-preconcentrator vapor release/injection performance significantly contributes to decrease the fidelity of (mu)GC analysis using our state-of-the-art passive preconcentrator microdevice. The vapor release/injection performance is highly affected by the kinetics of the thermal desorption of compounds trapped in the microdevice. Decreasing the heating rate by 20percent from the optimal rate of 90 deg Cs~(-1) causes a 340percent increase in peak tailing as well as 70percent peak broadening (30percent peak height reduction) to the microscale vapor injection process.
机译:微型气相色谱法(μGC)是一种新兴的分析技术,用于对中度复杂混合物中的挥发性有机化合物(VOC)进行原位分析和现场监控。微型气相色谱仪(μ-preconcentrator)是μGC系统中的关键子组件之一,它可以通过增强信号来检测低浓度((约)ppb以下)室内/环境空气中存在的化合物。普遍的观点是,由微细分离柱(μ柱)的不良条件引起的洗脱峰加宽和拖尾现象是色谱分离度差的主要来源。但是,先前的实验结果表明,即使在设置最佳分离条件后,对于与其他(mu)GC子组分集成的mu柱,仍然观察到分辨率下降。在这项工作中,我们获得的证据表明,使用我们最先进的无源预浓缩器微型设备,未优化的mu-预浓缩器蒸气释放/进样性能会显着降低muGC的保真度。蒸气释放/注入性能受微器件中捕获的化合物热脱附的动力学影响很大。将加热速率从90℃Cs〜(-1)的最佳速率降低20%,会导致微型尾气注入过程的峰拖尾增加340%,峰展宽70%(峰高降低30%)。

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