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气相色谱-电晕放电离子迁移谱仪的设计。

Design for gas chromatography-corona discharge-ion mobility spectrometry.

机构信息

Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran.

出版信息

Anal Chem. 2012 Nov 20;84(22):10077-84. doi: 10.1021/ac3025398. Epub 2012 Oct 29.

Abstract

A corona discharge ionization-ion mobility spectrometry (CD-IMS) with a novel sample inlet system was designed and constructed as a detector for capillary gas chromatography. In this design, a hollow needle was used instead of a solid needle which is commonly used for corona discharge creation, helping us to have direct axial interfacing for GC-IMS. The capillary column was passed through the needle, resulting in a reaction of effluents with reactant ions on the upstream side of the corona discharge ionization source. Using this sample introduction design, higher ionization efficiency was achieved relative to the entrance direction through the side of the drift tube. In addition, the volume of the ionization region was reduced to minimize the resistance time of compounds in the ionization source, increasing chromatographic resolution of the instrument. The effects of various parameters such as drift gas flow, makeup gas flow, and column tip position inside the needle were investigated. The designed instrument was exhaustively validated in terms of sensitivity, resolution, and reproducibility by analyzing the standard solutions of methyl isobutyl ketone, heptanone, nonanone, and acetophenone as the test compounds. The results obtained by CD-IMS detector were compared with those of the flame ionization detector, which revealed the capability of the proposed GC-IMS for two-dimensional separation (based on the retention time and drift time information) and identification of an analyte in complex matrixes.

摘要

设计并构建了一种带有新型进样系统的冠状放电离子化-离子迁移谱(CD-IMS),作为毛细管气相色谱的检测器。在该设计中,使用空心针代替了通常用于产生冠状放电的实心针,有助于我们实现 GC-IMS 的直接轴向接口。毛细管柱穿过针,导致流出物与冠状放电电离源上游侧的反应离子发生反应。使用这种进样设计,与通过漂移管侧面进入的方向相比,实现了更高的离子化效率。此外,将离子化区域的体积减小到最小,以最大限度地减少化合物在离子源中的阻力时间,提高仪器的色谱分辨率。研究了各种参数的影响,例如漂移气体流量、补充气体流量以及针内的柱端位置。通过分析作为测试化合物的甲基异丁基酮、庚酮、壬酮和苯乙酮的标准溶液,对设计的仪器进行了灵敏度、分辨率和重现性的全面验证。将 CD-IMS 检测器获得的结果与火焰离子化检测器的结果进行了比较,结果表明,所提出的 GC-IMS 具有对复杂基质中分析物进行二维分离(基于保留时间和漂移时间信息)和识别的能力。

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