Among a number of gas analyzers, portable gas chromatography (GC) systems created by the integration of microfabricated components are promising candidates for rapid and on-site analysis of a number of complex chemical mixtures. This Feature provides a snapshot of the progress made in developing micro gas chromatography (μGC) systems in the last 4 decades. In particular, we discuss the development of microfabricated preconcentrators, separation columns, and detectors. Furthermore, we review different stationary phase materials used to coat the separation columns and the major efforts toward the development of an integrated μGC.

Micro Gas Chromatography: An Overview of Critical Components and Their Integration

In recent years, the need for measurement and detection of samples in situ or with very small volume and low concentration (low and sub-parts per billion) is a cause for miniaturizing systems via microelectromechanical system (MEMS) technology. Gas chromatography (GC) is a common technique that is widely used for separating and measuring semi-volatile and volatile compounds. Conventional GCs are bulky and cannot be used for in situ analysis, hence in the past decades many studies have been reported with the aim of designing and developing chip-based GC. The focus of this review is to follow and investigate the development and the achievements in the field of chip-based GC and its components from the beginning up to the present.

Through the years with on-a-chip gas chromatography: a review

Silica sputtering as a novel collective stationary phase deposition for microelectromechanical system gas chromatography column: feasibility and first separations.

A controllable and high-yield surface functionalization of silicon microchannels using layer-by-layer (LbL) self-assembly of SiO2 nanoparticles (SNPs) is presented. The application of SNPs (45 nm average diameter) coating as a stationary phase for chromatographic separation is also demonstrated with surface functionalization using chloroalkylsilanes. This method facilitates a simple, low-cost, and parallel processing scheme that also provides homogeneous and stable nanoparticle-based stationary phases with ease of control over the coating thickness. The SNP-functionalized microfabricated columns with either single capillary channels (1 m long, 150 μm wide, 240 μm deep) or very narrow multicapillary channels (25 cm long, 30 μm wide, 240 μm deep, 16 parallel channels) successfully separated a multicomponent gas mixture with a wide range of boiling points with high reproducibility.

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Highly stable surface functionalization of microgas chromatography columns using layer-by-layer self-assembly of silica nanoparticles.

In a previous study, a new stationary phase deposition technique for micromachined gas chromatography columns was presented. The rerouting of the sputtering technique to this purpose enabled collective and reproducible fabrication of microcolumns in a silicon wafer. Silica-sputtered micromachined columns showed promising separations of light alkanes in isothermal conditions. In order to go beyond the limitations of isothermal separations, the columns were equipped with sputtered platinum filaments to enable high-speed and low-power temperature programming. The separation performances of temperature-programmed silica- or graphite-sputtered microcolumns were investigated: a separation of light alkanes (C1–C5) was completed in 9 s, and heavier alkanes (until C9), cyclic, isomeric, and unsaturated hydrocarbons were also successfully separated. Versatility of these microcolumns was demonstrated with a high-temperature C1–C2 separation and a C1–C5 separation with nitrogen as carrier gas instead of helium. By ma...

Temperature-programmed sputtered micromachined gas chromatography columns: an approach to fast separations in oilfield applications.

This paper reports on a gas sample injection system for gas chromatography, with the specificity of being potentially able to sustain the harsh environment of natural gas. This device integrates six low-leak microvalves made from polyetheretherketone (PEEK) membranes on silicon substrates. We report on the design, operation principle, fabrication, and intrinsic characteristics of the micro injector as well as its measured behavior in a compact gas chromatograph. The overall size of the micro injector - 7 mm × 3 mm × 1.2 mm - is among the smallest reported in the literature, and it permits the injection of a 250-nL sample volume. Characterization revealed a transition time of less than 35 ms between the sampling mode and the injection mode of the microinjector, with an expected potential of high precision on injection sample volume, owing to the very low leakage levels. Continuous operation and reproducible measurements are demonstrated when using the micro injector in a miniaturized chromatographic system. Comparison with commercially available injectors revealed similar quality of gas sample injection.

Micro gas chromatography sample injector for the analysis of natural gas

We present the use of poly ether ether ketone (PEEK) as a membrane material for a new type of gas microvalve, which is suitable for the harsh environments of natural gas. The design, fabrication, and experimental characterization of the PEEK-based microvalves are presented first, revealing leakage levels of less than 230 nL·min-1 under nitrogen and helium. Then, the main mechanical properties of the PEEK membranes are derived from both static and dynamic measurements, leading to a Young's modulus of 3.1 GPa and an inplane anisotropic stress field, with both tensile and compressive components in two perpendicular directions and whose magnitudes are + 33.9 MPa and -6.8 MPa, respectively. A blister test gave an adhesion energy estimated between 61 and 158 J·m-2. Finally, temperature cycles have been conducted on the microvalve, showing a resistance of up to 300°C, together with an improved closing of the membrane.

Microvalves for Natural-Gas Analysis With Poly Ether Ether Ketone Membranes

In the context of refinery gas testing, we studied the potential of a micro-gas chromatograph (μGC). For this purpose, we fabricated a new type of gas microvalve, based on a polyetheretherketone (PEEK) membrane, which is suitable for the harsh environment of natural gas. Experimental results are presented along with simulations to describe and discuss the static and dynamic behaviors of such a device.

Micro gas chromatograph for harsh refinery gas environment: Microvalves based on PEEK membranes

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Papers

Silica sputtering as a novel collective stationary phase deposition for microelectromechanical system gas chromatography column: feasibility and first separations.

Micro gas chromatography sample injector for the analysis of natural gas

Microvalves for Natural-Gas Analysis With Poly Ether Ether Ketone Membranes

Micro gas chromatograph for harsh refinery gas environment: Microvalves based on PEEK membranes