Microfabricated thermal modulator for comprehensive two-dimensional micro gas chromatography: design, thermal modeling, and preliminary testing

In comprehensive two-dimensional gas chromatography (GCxGC), a modulator is placed at the juncture between two separation columns to focus and re-inject eluting mixture components, thereby enhancing the resolution and the selectivity of analytes. As part of an effort to develop a mu GCx mu GC prototype, in this report we present the design, fabrication, thermal operation, and initial testing of a two-stage microscale thermal modulator (mu TM). The mu TM contains two sequential serpentine Pyrex-on-Si microchannels (stages) that cryogenically trap analytes eluting from the first-dimension column and thermally inject them into the second-dimension column in a rapid, programmable manner. For each modulation cycle (typically 5 s for cooling with refrigeration work of 200 J and 100 ms for heating at 10 W), the mu TM is kept approximately at -50 degrees C by a solid-state thermoelectric cooling unit placed within a few tens of micrometres of the device, and heated to 250 degrees C at 2800 degrees C s(-1) by integrated resistive microheaters and then cooled back to -50 degrees C at 250 degrees C s(-1). Thermal crosstalk between the two stages is less than 9%. A lumped heat transfer model is used to analyze the device design with respect to the rates of heating and cooling, power dissipation, and inter-stage thermal crosstalk as a function of Pyrex-membrane thickness, air-gap depth, and stage separation distance. Experimental results are in agreement with trends predicted by the model. Preliminary tests using a conventional capillary column interfaced to the mu TM demonstrate the capability for enhanced sensitivity and resolution as well as the modulation of a mixture of alkanes.