A method for direct coupling of supercritical fluid extraction and supercritical fluid chromatography with application to the analysis of nonvolatile coal derived products

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Virginia Tech


In recent years supercritical fluid chromatography has gained attention as an alternative technique to high performance liquid chromatography for the analyses of nonvolatile or thermally labile compounds, whose analysis with gas chromatography is impossible. The work presented here demonstrates a system that allows supercritical fluid extraction of the sample with subsequent direct introduction of a fraction of. this extract onto the column for analysis with supercritical fluid chromatography. Such a procedure has several inherent advantages to traditional sampling, where extraction or dissolution of the sample is done in a liquid. A valving scheme is described to accomplish this task and is evaluated for use with several different samples, including fuels and food products, with direct comparisons made between traditional sampling and direct on-line extraction. In most cases, the chromatograms were very similar, however later eluting components were sometimes lower in concentration with this method when compared to traditional sampling techniques.

The apparatus was demonstrated in the analysis of high boiling coal derived material. Analysis of this material is accomplished by preliminary class separation with subsequent supercritical fluid extraction and analysis by packed column supercritical fluid chromatography. Detection included variable wavelength UV and FTIR spectrometry. The coal derived products studied were taken from a bench scale coal liquefaction reactor, in which the same catalyst was used for twenty-five consecutive days. The changes that occur as the catalyst decays were determined chromatographically for a portion of the high boiling products. The changes were noted best in the aromatic fraction analysis, where a trend towards molecules with higher numbers of condensed rings was observed as the catalyst decayed.