Supercritical fluid chromatography/supersonic jet spectroscopy

Technical Report · Sun Jan 01 04:00:00 EST 1989

OSTI ID:6695302

Goates, S R; Lee, M L

Supersonic jet spectroscopy (SJS) was successfully coupled to supercritical fluid chromatography (SFC) and developed as high resolution technique for the analysis of complex samples. Direct supersonic expansion of the supercritical fluid was shown to be compatible with micro-bore and larger column SFC; high pressure sheath-flow expansions allowed capillary SFC to be performed with SJS. Selective, sensitive detection was demonstrated with both techniques for a coal tar sample. Design and characterization of nozzle performance was an important effort in the development of the SFC/SJS technique, including study of the direct expansion process, modification of the sheath-flow approach to make it applicable to supercritical fluid experiments, testing of several variations of pulsed nozzles, and investigation of back-pressure regulation of flow in capillary SFC to improve efficiency and resolution. Finally, improvements to signal detection and alternative detection schemes were investigated in efforts to enhance sensitivity and information content of the measurement. Perylene and benzo(a)pyrene were selectively detected in a coal tar samples at detection limits of 0.5 ng and 40 ng, respectively. Back-pressure regulation of eluent flow using the sheath-flow nozzle was investigated as a means of control in capillary SFC. Pre-restrictor detection was employed in the evaluation of the effect of regulated flow on chromatographic separations. Chromatographic resolution was improved when a constant linear velocity was maintained. 49 refs., 11 figs.

• Research Organization: Brigham Young Univ., Provo, UT (USA). Dept. of Chemistry
• Sponsoring Organization: DOE/FE
• DOE Contract Number: FG22-86PC90534
• OSTI ID: 6695302
• Report Number(s): DOE/PC/90534-15; ON: DE90015220
• Country of Publication: United States
• Language: English

Related Subjects

01 COAL, LIGNITE, AND PEAT
010600* -- Coal
Lignite
& Peat-- Properties & Composition
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400102 -- Chemical & Spectral Procedures
AROMATICS
CARBONACEOUS MATERIALS
CHROMATOGRAPHY
COAL
COAL TAR
CONDENSED AROMATICS
DESIGN
DOCUMENT TYPES
ENERGY SOURCES
FOSSIL FUELS
FUELS
HYDROCARBONS
MATERIALS
NOZZLES
ORGANIC COMPOUNDS
OTHER ORGANIC COMPOUNDS
PERYLENE
POLYCYCLIC AROMATIC HYDROCARBONS
PROGRESS REPORT
SEPARATION PROCESSES
SPECTRA
SPECTROSCOPY
SUPERCRITICAL FLUID CHROMATOGRAPHY
TAR