Dow Chemical Canada ULC, Highway 15, Fort Saskatchewan, Alberta T8L 2P4, Canada; Australian Centre for Research on Separation Science (ACROSS), University of Tasmania, Private Bag 75 Hobart 7001 Australia.
Dow Chemical Canada ULC, Highway 15, Fort Saskatchewan, Alberta T8L 2P4, Canada.
J Chromatogr A. 2020 Jan 4;1609:460460. doi: 10.1016/j.chroma.2019.460460. Epub 2019 Aug 14.
Fast gas chromatography that leverages the high chromatographic efficiency of narrow bore capillary column technology and temperature programming was successfully integrated with a third-generation low void-volume, 3D-printed two-stage microreactor. Effective management of extra-column effect and the capability to perform post-column backflushing were achieved with the incorporation of a recently commercialized, electronically controlled pneumatic switching device and a deactivated metal three-way microdevice. With this configuration, narrow bore capillary columns having internal diameters between 0.10 and 0.15 mm can be employed to produce chromatographic peaks in the domain of fast gas chromatography, with peak widths at half-height ranging from 0.42 s to 0.92 s for probe compounds having k over a range from 1.7 for toluene to 60 with the last analyte (nC) eluted in less than 12 min. The carbon independent response capability of the 3D-printed microreactor affords unique and advantaged differentiators, for instance, conducting measurement of the target analytes using one single carbon-containing compound for calibration with an acceptable accuracy of ±10%, achieving a higher degree of accuracy by eliminating the need for multi-level and multi-compound calibration, and improving sensitivity for compounds that are not efficiently ionized by flame ionization detection. Using this platform, repeatability of retention times for 14 probe compounds was less than 0.1% RSD (n = 10), and less than 1.0% RSD (n = 10) for area counts. The utility of the analytical approach was illustrated with relevant, challenging applications.
利用窄口径毛细管柱技术的高效色谱效率和程序升温的快速气相色谱成功地与第三代低死体积、3D 打印的两段式微反应器集成。通过采用最近商业化的电子控制气动切换装置和钝化金属三通微器件，实现了额外柱效的有效管理和进行柱后反冲洗的能力。在此配置中，可以使用内径在 0.10 至 0.15 毫米之间的窄口径毛细管柱，以在快速气相色谱的范围内产生色谱峰，对于 k 值范围从 1.7 到 60 的探针化合物，半峰宽在 0.42 到 0.92 秒之间，最后一个分析物 (nC) 在 12 分钟内洗脱。3D 打印微反应器的碳独立响应能力提供了独特的优势，例如，使用单个含碳化合物进行目标分析物的测量，校准精度可达到 ±10%，通过消除多级和多化合物校准的需要，实现更高的精度，并且提高了火焰电离检测不易离子化的化合物的灵敏度。使用该平台，14 种探针化合物的保留时间重复性小于 0.1%RSD（n=10），峰面积计数的重复性小于 1.0%RSD（n=10）。该分析方法的实用性通过相关的挑战性应用得到了说明。
