Title
Fast temperature programming in gas chromatography using resistive heating
Author
Dallüge, J.
Ou-Aissa, R.
Vreuls, J.J.
Brinkman, U.A.T.
Veraart, J.R.
TNO Voeding
Publication year
1999
Abstract
The features of a resistive-heated capillary column for fast temperature-programmed gas chromatography (GC) have been evaluated. Experiments were carried out using a commercial available EZ Flash GC, an assembly which can be used to upgrade existing gas chromatographs. The capillary column is placed inside a metal tube which can be heated, and cooled, much more rapidly than any conventional GC oven. The EZ Flash assembly can generate temperature ramps up to 1200 °/min and can be cooled down from 300 to 50 °C in 30 s. Samples were injected via a conventional split/splitless injector and transferred to the GC column. The combination of a short column (5 m x 0.25 mm i.d.), a high gas flow rate (up to 10 mL/min), and fast temperature programmes typically decreased analysis times from 30 min to about 2.5 min. Both the split and splitless injection mode could be used. With n-alkanes as test analytes, the standard deviations of the retention times with respect to the peak width were less than 15% (n = 7). First results on RSDs of peak areas of less than 3% for all but one n-alkane indicate that the technique can also be used for quantification. The combined use of a short GC column and fast temperature gradients does cause some loss of separation efficiency, but the approach is ideally suited for fast screening as illustrated for polycyclic aromatic hydrocarbons, organophosphorus pesticides, and triazine herbicides as test compounds. Total analysis times - which included injection, separation, and equilibration to initial conditions - were typically less than 3 min.
Subject
alkane
organophosphate insecticide
polycyclic aromatic hydrocarbon derivative
triazine derivative
analytic method
article
gas chromatography
heating
reaction analysis
screening test
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DOI
https://doi.org/10.1002/(sici)1521-4168(19990801)22:8<459::aid-jhrc459>3.0.co;2-g
TNO identifier
234886
ISSN
0935-6304
Source
HRC Journal of High Resolution Chromatography, 22 (8), 459-464
Document type
article