Department of Chemistry, National Central University, Chungli 320, Taiwan.
J Chromatogr A. 2013 Jun 14;1294:122-9. doi: 10.1016/j.chroma.2013.04.008. Epub 2013 Apr 10.
Ambient level hydrocarbons lighter than C6 were analyzed by the Deans switch-modulated comprehensive two-dimensional gas chromatography (GC×GC) method with flame ionization detection (FID). A thermal desorption (TD) device built in-house connects the GC×GC system to pre-concentrate the target compounds at ambient levels prior to GC analysis. Because the conventional orthogonality based on polarity difference for normal GC×GC separation does not provide sufficient retention for the target compounds of extremely high volatility, the orthogonality of non-polar vs. adsorptive force was adopted instead. The system employed a 100% polydimethyl siloxane column serving as the first-dimension column to provide separation based on dispersive interaction, with a short PLOT column serving as the second-dimension column to provide the needed retention based on gas-solid adsorption interactions. The shortest possible length of the PLOT column was tested to minimize the modulation period (PM) and wraparound and, at the same time, to maintain the desired resolution. The tests led to the final optimal parameters of 1.1m for the PLOT column length, 9s for the PM, 0.013 for the modulation duty cycle (DC) and a modulation ratio (MR) of 3.7 with minimal wraparound. Important criteria for quality assurance of precision and linearity are reported. The low cost and ease of construction and operation make the in-house Deans switch TD-GC×GC-FID system practical and useful for the analysis of light hydrocarbons in urban or industrial environments.
采用 Dean 切换调制全二维气相色谱(GC×GC)-火焰离子化检测(FID)法分析环境水平低于 C6 的轻碳氢化合物。一种内置的热解吸(TD)装置将 GC×GC 系统与预浓缩目标化合物在环境水平下进行连接,然后进行 GC 分析。由于传统的基于极性差异的正交性对于正常的 GC×GC 分离不能为极高挥发性的目标化合物提供足够的保留,因此采用了非极性与吸附力的正交性。该系统采用 100%聚二甲基硅氧烷柱作为第一维柱,提供基于分散相互作用的分离,采用短 PLOT 柱作为第二维柱,提供基于气固吸附相互作用的所需保留。测试了最短的 PLOT 柱长度,以最小化调制周期(PM)和缠绕,并同时保持所需的分辨率。测试得出最终的最佳参数为:PLOT 柱长度为 1.1m,PM 为 9s,调制占空比(DC)为 0.013,调制比(MR)为 3.7,缠绕最小。报告了保证精度和线性度的重要标准。该系统具有低成本、易于构建和操作的特点,使其成为用于分析城市或工业环境中轻烃的实用和有用的内置 Dean 切换 TD-GC×GC-FID 系统。