Comprehensive Two-Dimensional Gas Chromatographic Separations with a Microfabricated Thermal Modulator
| Autor: | Dibyadeep Paul, Gustavo Serrano, Sung-Jin Kim, Katsuo Kurabayashi, Edward T. Zellers |
|---|---|
| Rok vydání: | 2012 |
| Předmět: |
Volatile Organic Compounds
Chromatography Gas Thermoelectric cooling Chromatography Chemistry Capillary action Temperature Analytical chemistry Reproducibility of Results Equipment Design engineering.material Analytical Chemistry Kinetics chemistry.chemical_compound Boiling point Coating Phase (matter) Thermal engineering Microtechnology Two-dimensional gas Ethylene glycol |
| Zdroj: | Analytical Chemistry. 84:6973-6980 |
| ISSN: | 1520-6882 0003-2700 |
| DOI: | 10.1021/ac300924b |
| Popis: | Rapid, comprehensive two-dimensional gas chromatographic (GC × GC) separations by use of a microfabricated midpoint thermal modulator (μTM) are demonstrated, and the effects of various μTM design and operating parameters on performance are characterized. The two-stage μTM chip consists of two interconnected spiral etched-Si microchannels (4.2 and 2.8 cm long) with a cross section of 250 × 140 μm(2), an anodically bonded Pyrex cap, and a cross-linked wall coating of poly(dimethylsiloxane) (PDMS). Integrated heaters provide rapid, sequential heating of each μTM stage, while a proximate, underlying thermoelectric cooler provides continual cooling. The first-dimension column used for GC × GC separations was a 6 m long, 250 μm i.d. capillary with a PDMS stationary phase, and the second-dimension column was a 0.5 m long, 100 μm i.d. capillary with a poly(ethylene glycol) phase. Using sets of five to seven volatile test compounds (boiling point ≤174 °C), the effects of the minimum (T(min)) and maximum (T(max)) modulation temperature, stage heating lag/offset (O(s)), modulation period (P(M)), and volumetric flow rate (F) on the quality of the separations were evaluated with respect to several performance metrics. Best results were obtained with a T(min) = -20 °C, T(max) = 210 °C, O(s) = 600 ms, P(M) = 6 s, and F = 0.9 mL/min. Replicate modulated peak areas and retention times were reproducible to5%. A structured nine-component GC × GC chromatogram was produced, and a 21 component separation was achieved in3 min. The potential for creating portable μGC × μGC systems is discussed. |
| Databáze: | OpenAIRE |
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