Affiliations 

  • 1 Australian Centre for Research on Separation Science, School of Chemistry, Monash University,Wellington Road, Clayton, VIC 3800, Australia; Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Bangkok 10330, Thailand
  • 2 Australian Centre for Research on Separation Science, School of Chemistry, Monash University,Wellington Road, Clayton, VIC 3800, Australia
  • 3 Australian Centre for Research on Separation Science, School of Chemistry, Monash University,Wellington Road, Clayton, VIC 3800, Australia; School of Chemical Sciences, Universiti Sains Malaysia, 11800 Penang, Malaysia
  • 4 Australian Centre for Research on Separation Science, School of Chemistry, Monash University,Wellington Road, Clayton, VIC 3800, Australia. Electronic address: Philip.Marriott@monash.edu
J Chromatogr A, 2018 Apr 20;1546:97-105.
PMID: 29548566 DOI: 10.1016/j.chroma.2018.02.035

Abstract

Real-time interconversion processes produce unconventional peak broadening in gas chromatography (GC), and can be used to generate kinetic and thermodynamic data. In this study, an unusual separation situation in comprehensive two dimensional GC where two dimensional interconversion (i.e. a raised plateau in both first and second dimension, 1D and 2D) was observed in analysis of oxime isomers. This resulted in a characteristic and unusual rectangular peak shape in the two dimensional result. A related theoretical approach was introduced to explain the peak shape supported by simulation results which can be varied depending on concentration profiles and kinetics of the process. The simulated results were supported by experimental results obtained by a comprehensive heart-cut multidimensional GC (H/C MDGC) approach which was developed to clearly investigate isomerisation of E/Z oxime molecules in both 1D and 2D separations under different isothermal conditions. The carrier gas flow and oven temperature were selected according to initial results for 1D interconversion on a poly(ethyleneglycol) stationary phase, which was further used in both 1D and 2D separations to result in broad zones of oxime interconversion in both dimensions. The method involved repetitive injections of oxime sample, then sampling contiguous fractions of sample into a long 2D column which is intended to promote considerable interconversion. Comprehensiveness arises from the fact that the whole sample is sampled from the 1D to the 2D column, with the long 2D column replacing the short 2D column used in classical comprehensive two-dimensional gas chromatography, where the latter will not promote sufficient interconversion. Data processing and presentation permits a 'rectangular' distribution corresponding to the separated compounds, characteristic of this experiment.

* Title and MeSH Headings from MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine.

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