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Title: Supercritical fluid chromatography/supersonic jet spectroscopy. Progress report, November 1, 1985-January 31, 1986

Technical Report ·
OSTI ID:6266530

Studies during this period focused on the group separation of aliphatics, olefins and aromatics in gasoline range samples. Preparations for the high temperature supercritical fluid fractionation apparatus are in progress and are expected to be finished during the next period. In addition, the same procedure used for the fractionation of complex mixtures by ring number was applied to a primarily aliphatic hydrocarbon sample, a Wyoming Recluse crude oil. The chromatogram shown in Figure 1 was obtained with dual ultraviolet absorbance (uv)/flame ionization detection (FID). The capillary gas chromatograms of the fractions collected during the supercritical fluid fractionation of the crude oil are shown in Figure 2. As described in the last report, separations of aliphatics from aromatics were achieved with columns packed with underivatized silica. The chemical class fractionation studies continued during this quarter with attempts to separate aliphatics from olefins. Table 1 lists the stationary phases which were tested for their ability to separate olefins from aliphatics. Some months ago, we reported on an initial demonstration of the feasibility of using supercritical fluids as a means of introducing sample molecules into a supersonic jet (SJ). Since then, we have been working on improving experimental conditions to give better cooling and to lower detection limits to the point that supersonic jet fluorescence spectroscopy could be coupled to capillary SFC. During this last period we have made much progress in both areas. We have obtained the dispersed fluorescence spectra of napthalene (308 nm excitation) in supercritical fluid/supersonic jet expansions for several carrier fluids (n-pentane, carbon dioxide, sulfur hexafluoride, and nitrous oxide) through a variety of pinhole and capillary nozzles. 4 refs., 5 figs., 1 tab.

Research Organization:
Brigham Young Univ., Provo, UT (USA). Dept. of Chemistry
DOE Contract Number:
FG22-83PC60807
OSTI ID:
6266530
Report Number(s):
DOE/PC/60807-10; ON: DE86007028
Resource Relation:
Other Information: Portions of this document are illegible in microfiche products
Country of Publication:
United States
Language:
English