Evaluation of a microfabricated thermal modulator for comprehensive two-dimensional microscale gas chromatography

Anal Chem. 2011 Jul 15;83(14):5556-62. doi: 10.1021/ac200336e. Epub 2011 Jun 22.

Abstract

A microfabricated thermal modulator (μTM) designed for ultimate use in a comprehensive two-dimensional microscale gas chromatography (μGC × μGC) system is evaluated. The 2-stage device measures 13 mm (l) × 6 mm (w) × 0.5 mm (h) and consists of two interconnected serpentine etched-Si microchannels suspended from a thin Pyrex cap and wall-coated with PDMS (polydimethylsiloxane). The chip is mounted within a few tens of micrometers of a thermoelectric cooler that maintains both stages at a baseline temperature between -35 and -20 °C in order to focus analytes eluting from an upstream separation column. Each stage is heated to 210 °C sequentially at a rate as high as 2400 °C/s by independent thin-film resistors to inject the analytes in consecutive fractions to a downstream column, and then cooled at a rate as high as -168 °C/s. The average power dissipation is only ∼10 W for heating and 21 W for cooling without using consumable materials. In this study, the outlet of the μTM is connected directly to a flame ionization detector to assess its performance. Following a demonstration of basic operation, the modulated peak amplitude enhancement (PAE) and full-width-at-half-maximum (fwhm) are evaluated for members of a series of n-alkanes (C(6)-C(10)) as a function of the rim and stage temperatures; modulation period, phase, and offset; analyte concentration; and carrier-gas flow rate. A PAE as high as 50 and a fwhm as narrow as 90 ms are achieved for n-octane under optimized conditions.

Publication types

  • Evaluation Study
  • Research Support, U.S. Gov't, Non-P.H.S.

MeSH terms

  • Alkanes / analysis*
  • Chromatography, Gas / instrumentation*
  • Chromatography, Gas / methods
  • Dimethylpolysiloxanes / chemistry
  • Equipment Design
  • Microtechnology
  • Reproducibility of Results
  • Temperature

Substances

  • Alkanes
  • Dimethylpolysiloxanes
  • baysilon