Design and implementation of comprehensive gas chromatography with cryogenic modulation

Russell M. Kinghorn, Philip J. Marriott, Peter A. Dawes

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Abstract

Comprehensive gas chromatography is the realization of true continuous multidimensional (dual column) gas chromatography. The key requirement in the comprehensive GC experiment is that the second dimension analysis is completed in a rapid time-frame compared to the elution of components in the first dimension, and that the two coupled dimensions represent 'orthogonal' analyses towards the analytes to be separated. The former normally necessitates pulsing of contiguous segments of each chromatographic band from the first to the second dimensions. The two dimensions should be in fluid communication. The comprehensive GC × GC experiment passes all the column flow from the first column to the second column, leading to no sample loss, but this also requires a suitable method for time- or zone-compression of the band to be pulsed to the second column. The final pulse should be narrow, and should be delivered to the second column quickly. A simple procedure can achieve this using the cryogenic modulator that has been recently described by this group. The system uses a cryogenic trap which can be moved away from the cooled zone of the column faster than 10 ms. A fast-acting pneumatic ram achieves this performance. The cooled column heats up to the prevailing oven temperature within 10-15ms. Molecules as volatile as C5 alkanes or small aromatics will be fully retained by the trap within the period of modulation used for GC × GC. The technique is simple to implement and requires no special column connections. Using a gas chromatograph which allows control of external events and can acquire from a detector at 50 Hz or faster, and a timing controller for modulation, the comprehensive result can easily and effectively be achieved.

Original languageEnglish
Pages (from-to)245-252
Number of pages8
JournalJournal of Separation Science
Volume23
Issue number3
DOIs
Publication statusPublished - 1 Dec 2000
Externally publishedYes

Keywords

  • Comprehensive gas chromatography
  • Cryogenic modulation
  • GC × GC
  • LMCS

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