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Title: Supercritical fluid chromatography/supersonic jet spectroscopy: Progress report, 9/15/86-12/15/86

Abstract

Supersonic jet (SJ) expansions of gaseous molecules can result in much simplified and highly resolved laser-induced fluorescence spectra, allowing analysis of closely related components in a complex sample. We have previously demonstrated that large polycyclic aromatic hydrocarbon (PAH) molecules of low volatility can also be introduced into the jet by means of supercritical fluid (SF), rather than gaseous, carriers and very good spectral narrowing achieved. Last summer in our first attempts with total fluorescence detection in a coupled capillary SFC/SJ system, selective detection of perylene in an artificial mixture of ten PAH and in the coal tar extract sample was achieved. However, only rather poor chromatographic separation was obtained, due in part to a high linear velocity of the fluid through the chromatographic column with the short capillary nozzle which was employed. The extended pressure gradient with most of the restrictors commonly used with SFC lead to conditions within the restrictor where aggregation of solute molecules can occur which seriously degrade the spectral resolution. Successful SFC/SJ requires large but abrupt restriction. Since then we have worked on the problem of a nozzle design which provides low dead-volume and high restriction for efficient chromatographic separation without leading to solute clustering. Severalmore » nozzle types were investigated including pinhole, tapered tubular, and porous frit. Disappointing results were obtained with all three types. During this last quarter we have built a light-scattering apparatus and vacuum chamber which can be devoted to testing new nozzles while pursuing spectroscopic studies in our primary chamber. 8 refs., 3 figs.« less

Authors:
;
Publication Date:
Research Org.:
Brigham Young Univ., Provo, UT (USA). Dept. of Chemistry
OSTI Identifier:
6989239
Report Number(s):
DOE/PC/90534-1
ON: DE87004583
DOE Contract Number:  
FG22-86PC90534
Resource Type:
Technical Report
Resource Relation:
Other Information: Portions of this document are illegible in microfiche products
Country of Publication:
United States
Language:
English
Subject:
01 COAL, LIGNITE, AND PEAT; 37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; COAL TAR; QUALITATIVE CHEMICAL ANALYSIS; NOZZLES; DESIGN; PERYLENE; SUPERCRITICAL FLUID CHROMATOGRAPHY; POLYCYCLIC AROMATIC HYDROCARBONS; EXTRACTION; RESEARCH PROGRAMS; COAL EXTRACTS; EXPERIMENTAL DATA; FLUORESCENCE; JETS; LASERS; MIXTURES; SPECTROSCOPY; SUPERSONIC FLOW; AROMATICS; CHEMICAL ANALYSIS; CHROMATOGRAPHY; CONDENSED AROMATICS; DATA; DISPERSIONS; FLUID FLOW; HYDROCARBONS; INFORMATION; LUMINESCENCE; NUMERICAL DATA; ORGANIC COMPOUNDS; OTHER ORGANIC COMPOUNDS; SEPARATION PROCESSES; TAR; 010600* - Coal, Lignite, & Peat- Properties & Composition; 400102 - Chemical & Spectral Procedures

Citation Formats

Goates, S R, and Lee, M L. Supercritical fluid chromatography/supersonic jet spectroscopy: Progress report, 9/15/86-12/15/86. United States: N. p., 1986. Web.
Goates, S R, & Lee, M L. Supercritical fluid chromatography/supersonic jet spectroscopy: Progress report, 9/15/86-12/15/86. United States.
Goates, S R, and Lee, M L. Wed . "Supercritical fluid chromatography/supersonic jet spectroscopy: Progress report, 9/15/86-12/15/86". United States.
@article{osti_6989239,
title = {Supercritical fluid chromatography/supersonic jet spectroscopy: Progress report, 9/15/86-12/15/86},
author = {Goates, S R and Lee, M L},
abstractNote = {Supersonic jet (SJ) expansions of gaseous molecules can result in much simplified and highly resolved laser-induced fluorescence spectra, allowing analysis of closely related components in a complex sample. We have previously demonstrated that large polycyclic aromatic hydrocarbon (PAH) molecules of low volatility can also be introduced into the jet by means of supercritical fluid (SF), rather than gaseous, carriers and very good spectral narrowing achieved. Last summer in our first attempts with total fluorescence detection in a coupled capillary SFC/SJ system, selective detection of perylene in an artificial mixture of ten PAH and in the coal tar extract sample was achieved. However, only rather poor chromatographic separation was obtained, due in part to a high linear velocity of the fluid through the chromatographic column with the short capillary nozzle which was employed. The extended pressure gradient with most of the restrictors commonly used with SFC lead to conditions within the restrictor where aggregation of solute molecules can occur which seriously degrade the spectral resolution. Successful SFC/SJ requires large but abrupt restriction. Since then we have worked on the problem of a nozzle design which provides low dead-volume and high restriction for efficient chromatographic separation without leading to solute clustering. Several nozzle types were investigated including pinhole, tapered tubular, and porous frit. Disappointing results were obtained with all three types. During this last quarter we have built a light-scattering apparatus and vacuum chamber which can be devoted to testing new nozzles while pursuing spectroscopic studies in our primary chamber. 8 refs., 3 figs.},
doi = {},
url = {https://www.osti.gov/biblio/6989239}, journal = {},
number = ,
volume = ,
place = {United States},
year = {1986},
month = {1}
}

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