RESUMEN
Micro gas chromatography (µGC) using microfabricated silicon columns has been developed in response to the requirement for portable on-site gas analysis. Although different stationary phases have been developed, repeatable and reliable surface coatings in these rather small microcolumns remains a challenge. Herein, a new stationary phase coating strategy using magnetic beads (MBs) as carriers for micro column is presented. MBs modified with organopolysiloxane (MBs@OV-1) and a metal organic framework (MBs@HKUST-1) are deposited in on-chip microcolumns assisted with a magnetic field with an optimized modification process. MBs@OV-1 column showed a minimum HETP of 0.074 cm (1351 plates/m) of 62 cm/s. Mixtures of volatile organic compounds are successfully separated using MBs carried stationary phase which demonstrates that this technique has good chromatographic column efficiency. This method not only provides a novel coating process, washing and characterization of the stationary phases but also establishes a straightforward strategy for testing new absorbent materials for µGC systems.
Asunto(s)
Estructuras Metalorgánicas , Cromatografía de Gases/métodos , Silicio , Dimetilpolisiloxanos/química , Fenómenos MagnéticosRESUMEN
Carbon nanotube (CNT)-based chemiresistors are promising gas detectors for gas chromatography (GC) due to their intrinsic nanoscale porosity and excellent electrical conductivity. However, fabrication reproducibility, long desorption time, limited sensitivity, and low dynamic range limit their usage in real applications. This paper reports a novel on-chip monolithic integrated multimode CNT sensor, where a micro-electro-mechanical system-based bulk acoustic wave (BAW) resonator is embedded underneath a CNT chemiresistor. The device fabrication repeatability was improved by on-site monitoring of CNT deposition using BAW. We found that the acoustic stimulation can accelerate the gas desorption rate from the CNT surface, which solves the slow desorption issue. Due to the different sensing mechanisms, the multimode CNT sensor provides complementary responses to targets with improved sensitivity and dynamic range compared to a single mode detector. A prototype of a chromatographic system using the multimode CNT sensor was prepared by dedicated design of the connection between the device and the separation column. Such a GC system is used for the quantitative identification of a gas mixture at different GC conditions, which proves the feasibility of the multimode CNT detector for chromatographic analysis. The as-developed CMOS compatible multimode CNT sensor offers high sensing performance, miniaturized size, and low power consumption, which are critical for developing portable GC.
Asunto(s)
Sistemas Microelectromecánicos , Nanotubos de Carbono , Nanotubos de Carbono/química , Reproducibilidad de los Resultados , Cromatografía de Gases , Gases/análisisRESUMEN
A microfluidic film bulk acoustic wave resonator gas sensor (mFBAR) adapted specifically as an in-line detector in gas chromatography was described. This miniaturized vapor sensor was a non-destructive detector with very low dead volume (0.02 µL). It was prepared by enclosing the resonator in a microfluidic channel on a chip with dimensions of only 15 mm × 15 mm × 1 mm. The device with polymer coating showed satisfactory performance in the detection of organophosphorus compound, demonstrating a very low detection limit (a dozen parts per billion) with relatively short response time (about fifteen seconds) toward the simulant of chemical warfare agent, dimethyl methylphosphonate. The in-line detection of the mFBAR sensor with FID was constructed and employed to directly measure the concentration profile on the solid surface by the mFBAR with the controlled concentration profile in the mobile phase at the same time. The difference of peak-maximum position between mobile phase and solid phase could be a convenient indicator to measure mass transfer rate. With the response of the mFBAR and FID obtained in one injection, an injection mass-independent parameter can be calculated and used to identify the analyte of interest.