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Compact, Automated, Inexpensive, and Field-Deployable Vacuum-Outlet Gas Chromatograph for Trace-Concentration Gas-Phase Organic Compounds

机译:紧凑,自动化,廉价和现场可展开的真空出口气相色谱仪,用于痕量气相有机化合物

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摘要

The identification and quantification of gas phase organic compounds, such as volatile organic compounds (VOCs), frequently use gas chromatography (GC), which typically requires high-purity compressed gases. We have developed a new instrument for trace-concentration measurements of VOCs and intermediate-volatility compounds of up to 14 carbon atoms in a fully automated (computer-free), independent, low-cost, compact GC-based system for the quantitative analysis of complex mixtures without the need for compressed, high-purity gases or expensive detectors. Through adsorptive analyte preconcentration, vacuum GC, photoionization detectors, and need-based water-vapor control, we enable measurements with picogram-level limits of detection (i.e., under 15 ppt in a 4 L sample for most compounds). We validate performance against a commercial pressurized GC, including resolving challenging isomers of similar volatility, such as ethylbenzene and m/p-xylene. We employ vacuum GC across the whole column with filtered air as a carrier gas, producing long-term system stability and performance over a wide range of analytes. Through theory and experiments, we present variations in analyte diffusivities in the mobile phase, analyte elution temperatures, optimal linear velocities, and separation-plate heights with vacuum GC in air at different pressures, and we optimize our instrument to exploit these differences. At 2-6 psia, the molecular diffusion coefficients are 6.4-2.1 times larger and the elution temperatures are 39-92 degrees C lower than with pressurized GC with helium (at 30 psig) depending on the molecular structure, and we find a wide range of optimal linear velocities (up to 60 cm s(-1)) that are faster with broader tolerances than with pressurized-N-2 GC.
机译:气相有机化合物的鉴定和定量,例如挥发性有机化合物(VOC),经常使用气相色谱(GC),其通常需要高纯度压缩气体。我们开发了一种新的仪表,用于在全自动(无计算机),独立,低成本,紧凑的GC基础上的全自动(无电脑),独立,低成本,基于紧凑的GC系统中的漏孔和中间挥发性化合物的微量仪表。用于定量分析复杂的混合物,无需压缩,高纯度气体或昂贵的探测器。通过吸附分析物预浓缩,真空GC,光离子化探测器和基于需求的水蒸气控制,我们能够测量与小型检测的皮科水平限制(即,对于大多数化合物的4L样品中的15个PPT)进行测量。我们验证了对商业加压GC的性能,包括分解相似挥发性的挑战异构体,例如乙苯和m / p-二甲苯。我们在整个柱上使用真空GC,过滤空气作为载气,在各种分析物中产生长期系统稳定性和性能。通过理论和实验,我们在不同压力下在空气中具有真空GC的流动相,分析物洗脱温度,最佳线性速度和分离板高度的分析物扩散性的变化,我们优化了我们的仪器利用这些差异。在2-6psia,分子扩散系数较大6.4-2.1倍,并且洗脱温度低于用氦气(30psig)的加压gc,取决于分子结构,并且我们发现广泛最佳的线性速度(高达60cm S(-1)),具有比加压-N-2 GC更宽的公差更快。

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  • 来源
    《Analytical chemistry》 |2019年第2期|共10页
  • 作者单位

    Yale Univ Sch Engn &

    Appl Sci Dept Chem &

    Environm Engn New Haven CT 06511 USA;

    Yale Univ Sch Engn &

    Appl Sci Dept Chem &

    Environm Engn New Haven CT 06511 USA;

    Yale Univ Sch Engn &

    Appl Sci Dept Chem &

    Environm Engn New Haven CT 06511 USA;

    Yale Univ Sch Engn &

    Appl Sci Dept Chem &

    Environm Engn New Haven CT 06511 USA;

    Yale Univ Sch Engn &

    Appl Sci Dept Chem &

    Environm Engn New Haven CT 06511 USA;

    Yale Univ Sch Engn &

    Appl Sci Dept Chem &

    Environm Engn New Haven CT 06511 USA;

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  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 分析化学;
  • 关键词

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