Valve-based comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometric detection: instrumentation and figures-of-merit

• Published in: Journal of Chromatography A 2003-11, Vol.1019 (1), p.79-87
• Main Authors: Sinha, Amanda E., Prazen, Bryan J., Fraga, Carlos G., Synovec, Robert E.
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Chemistry; Chromatographic methods and physical methods associated with chromatography; Dimethyl methyl phosphonate; Dimethyl phosphite; Exact sciences and technology; Gas chromatographic methods; Gas chromatography, comprehensive two-dimensional; Gas Chromatography-Mass Spectrometry - methods; Instrumentation; Mass spectrometry; Modulator, valve-based; Sensitivity and Specificity; Time-of-flight mass spectrometry; Triethylphosphorothioate
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2003.08.047

A valve-based comprehensive two-dimensional gas chromatograph coupled to a time-of-flight mass spectrometer (GC×GC/TOFMS) is demonstrated. The performance characteristics of the instrument were evaluated using a complex sample containing a mixture of fuel components, natural products, and organo-phosphorous compounds. The valve-based GC×GC, designed to function with an extended temperature of operation range, is shown to have high chromatographic resolution, high separation efficiency and low detection limits. Typical peak widths at base are nominally from 100 to 300 ms on column 2 and nominally 10 s on column 1. The injected mass and injected concentration limit of detection (LOD), defined as 3 standard deviations above the mean baseline noise, for three organo-phosphorous compounds (triethylphosphorothioate (TEPT), dimethyl methyl phosphonate (DMMP) and dimethyl phosphite (DMP)) in a complex environmental sample were from 6 to 38 pg, and 3 to 17 ng/ml, respectively. The temperature program for the environmental sample ranged from 40 to 230 °C, a temperature range capable of analyzing semi-volatile compounds. A new compact, stand-alone, valve-pulse generator device has been implemented and is also reported. The valve-based GC×GC instrument, therefore, offers a simple, rugged and less expensive alternative to thermally modulated instruments.