Compact, Automated, Inexpensive, and Field-Deployable Vacuum-Outlet Gas Chromatograph for Trace-Concentration...

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 sensitive and selective 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 °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-N₂ GC.