Gas chromatography is widely used to identify and quantify volatile organic compounds for applications ranging from environmental monitoring to homeland security. We investigate a new architecture for microfabricated gas chromatography systems that can significantly improve the range, speed, and efficiency of such systems. By using a cellular approach, it performs a partial separation of analytes even as the sampling is being performed. The subsequent separation step is then rapidly performed within each cell. The cells, each of which contains a preconcentrator and separation column, are arranged in progression of retentiveness. While accommodating a wide range of analytes, this progressive cellular architecture (PCA) also provides a pathway to improving energy efficiency and lifetime by reducing the need for heating the separation columns. As a proof of concept, a three-cell subsystem (PCA3mv) has been built; it incorporates a number of microfabricated components, including preconcentrators, separation columns, valves, connectors, and a carrier gas filter. The preconcentrator and separation column of each cell are monolithically implemented as a single chip that has a footprint of 1.8 × 5.2 cm2. This subsystem also incorporates two manifold arrays of microfabricated valves, each of which has a footprint of 1.3 × 1.4 cm2. Operated together with a commercial flame ionization detector, the subsystem has been tested against polar and nonpolar analytes (including alkanes, alcohols, aromatics, and phosphonate esters) over a molecular weight range of 32–212 g/mol and a vapor pressure range of 0.005–231 mmHg. The separations require an average column temperature of 63–68 °C within a duration of 12 min, and provide separation resolutions >2 for any two homologues that differ by one methyl group.

Microscale gas chromatographs (μGCs) promise infield analysis of volatile organic compounds (VOCs) in environmental and industrial monitoring, healthcare, and homeland security applications. As a step toward addressing challenges with performance and manufacturability, this study reports a highly integrated monolithic chip implementing a multisensing progressive cellular architecture. This architecture incorporates three μGC cells that are customized for different ranges of analyte volatility; each cell includes a preconcentrator and separation column, two complementary capacitive detectors, and a photoionization detector (PID). An on-chip carrier gas filter scrubs ambient air for the analysis. The monolithic chip, with all 16 components, is 40.3 × 55.7 mm 2 in footprint. To accommodate surface adsorptive and low-volatility analytes, the architecture eliminates the commonly used inlet valve, eliminating the need for chemically inactive surfaces in the valves and pumps, allowing the use of standard parts. Representative analysis is demonstrated from a nonpolar 14-analyte mixture, a polar 12-analyte mixture, and a 3-phosphonate ester mixture, covering a wide vapor pressure range (0.005−68.5 kPa) and dielectric constant range (1.8−23.2). The three types of detectors show highly complementary responses. Quantitative analysis is shown in the tens to hundreds ppb range. With 200 mL samples, the projected detection limits reach 0.12− 4.7 ppb. Limited tests performed at 80% humidity showed that the analytes with vapor pressures <12 kPa were unaffected. A typical full run takes 28 min and consumes 2.3 kJ energy for the fluidic elements (excluding electronics). By eliminating chip-to-chip fluidic interconnections and requiring just one custom-fabricated element, this work presents a path toward high-performance and highly manufacturable μGCs.

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This paper reports a multi-valve module with high chemical inertness and embedded flow heating for microscale gas chromatography (µGC) systems. The multi-valve module incorporates a monolithically microfabricated die stack, polyimide valve membranes, and solenoid actuators. The design incorporates three valves within a single module of volume 30.2 cm3, which is suitable for the small form factor of µGC systems. The die stack uses fused silica wafers and polyimide valve membranes that enhance chemical inertness. The monolithic die stack requires only three lithographic masks to pattern fluidic microchannels, valve seats, and thin-film metal heaters and thermistors. The performance of fabricated multi-valve modules is compared to a commercial valve in tests using multiple volatile organic compounds, including alkanes, alcohols, ketones, aromatic hydrocarbons, and phosphonates. The valves show almost no distortion of chromatographic peaks. The experimentally measured ratio of flow conductance is 3.46 × 103, with 4.15 sccm/kPa in the open state and 0.0012 sccm/kPa in the closed state. The response time is <120 ms.