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Anal Chem


Title:muGC x muGC: comprehensive two-dimensional gas chromatographic separations with microfabricated components
Author(s):Collin WR; Bondy A; Paul D; Kurabayashi K; Zellers ET;
Address:"Department of Chemistry, University of Michigan , Ann Arbor, Michigan 48109-1055, United States"
Journal Title:Anal Chem
Year:2015
Volume:20150115
Issue:3
Page Number:1630 - 1637
DOI: 10.1021/ac5032226
ISSN/ISBN:1520-6882 (Electronic) 0003-2700 (Linking)
Abstract:"The development and characterization of a microanalytical subsystem comprising silicon-micromachined first- and second-dimension separation columns and a silicon-micromachined thermal modulator (muTM) for comprehensive two-dimensional (i.e., muGC x muGC) separations are described. The first dimension consists of two series-coupled 3.1 cm x 3.1 cm mucolumn chips with etched channels 3 m long and 250 mum x 140 mum in cross section, wall-coated with a poly(dimethylsiloxane) (PDMS) stationary phase. The second dimension consists of a 1.2 cm x 1.2 cm mucolumn chip with an etched channel 0.5 m long and 46 mum x 150 mum in cross section wall-coated with either a trigonal tricationic room-temperature ionic liquid (RTIL) or a commercial poly(trifluoropropylmethyl siloxane) (OV-215) stationary phase. The two-stage, cryogen-free muTM consists of a Si chip containing two series-coupled, square spiral channels 4.2 cm and 2.8 cm long and 250 mum x 140 mum in cross section wall-coated with PDMS. Conventional injection methods and flame ionization detection were used. Temperature-ramped separations of a simple alkane mixture using the RTIL-coated second-dimension ((2)D) mucolumn produced reasonably good peak shapes and modulation numbers; however, strong retention of polar compounds on the RTIL-coated (2)D mucolumn led to excessively broad peaks with low (2)D resolution. Substituting OV-215 as the (2)D mucolumn stationary phase markedly improved the performance, and a structured 22 min chromatogram of a 36-component mixture spanning a vapor pressure range of 0.027 to 13 kPa was generated with modulated peak fwhm (full width at half-maximum) values ranging from 90 to 643 ms and modulation numbers of 1-6"
Keywords:"Chromatography, Gas/*instrumentation/*methods Dimethylpolysiloxanes/*chemistry Flame Ionization Ionic Liquids Microtechnology/*instrumentation/*methods Temperature Volatile Organic Compounds/*analysis;"
Notes:"MedlineCollin, William R Bondy, Amy Paul, Dibyadeep Kurabayashi, Katsuo Zellers, Edward T eng Research Support, Non-U.S. Gov't Research Support, U.S. Gov't, Non-P.H.S. 2014/12/24 Anal Chem. 2015 Feb 3; 87(3):1630-7. doi: 10.1021/ac5032226. Epub 2015 Jan 15"

 
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