Development and evaluation of supercritical fluid chromatography/mass spectrometry for polar and high-molecular-weight coal components: Technical progress report, October 1, 1986-September 30, 1987

Technical Report · Mon Feb 01 04:00:00 EST 1988

DOI:https://doi.org/10.2172/5539304· OSTI ID:5539304

Chess, E K; Kalinoski, H T; Smith, R D

This program, Development and Evaluation of Supercritical Fluid Chromatography/Mass Spectrometry for Polar and High-Molecular-Weight Coal Components, is aimed at the development of new analytical technologies for the characterization of previously intractable complex mixtures. The specific goals of this program are twofold: (1) to develop and evaluate a combined high-resolution, capillary column, supercritical fluid chromatograph/high-performance mass spectrometer (SFC/MS) that is capable of analyzing high-molecular-weight materials, such as polar and heavy-end components found in coal conversion processes; and (2) to use this system to develop and evaluate analytical technology applicable to coal process development technology. Studies have been conducted to characterize the performance of the supercritical fluid chromatograph-mass spectrometer interface, and several modifications have been made to the probe, ion source, and associated hardware to improve performance and operator safety. Methods have been developed that allow the mass calibration of the magnetic sector mass spectrometer to 1400 daltons using desorption chemical ionization. Methodologies have been improved for fabricating capillary columns with bonded, crosslinked stationary phases suitable for use with polar fluids. Coal-derived materials and fossil-fuel-derived sediments have been investigated with supercritical fluid chromatograph/mass spectrometry and supercritical fluid extraction/mass spectrometry. Microbore packed columns coupled to a modified mass spectrometer interface allowed the chemical class fractionation of relatively polar complex mixtures derived from coal liquefaction. 6 refs., 12 figs.

• Research Organization: Pacific Northwest Lab., Richland, WA (USA)
• DOE Contract Number: AC06-76RL01830
• OSTI ID: 5539304
• Report Number(s): PNL-6168; ON: DE88006560
• Country of Publication: United States
• Language: English

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47 OTHER INSTRUMENTATION
ALCOHOLS
AMINES
AMMONIA
CALIBRATION
CHROMATOGRAPHY
COAL LIQUIDS
DOCUMENT TYPES
FLUIDS
GLYCOLS
HYDRIDES
HYDROGEN COMPOUNDS
HYDROXY COMPOUNDS
INTERFACES
LIQUIDS
MASS SPECTROSCOPY
NITROGEN COMPOUNDS
NITROGEN HYDRIDES
ORGANIC COMPOUNDS
PERFORMANCE TESTING
PROGRESS REPORT
SEPARATION PROCESSES
SPECTROSCOPY
SUPERCRITICAL FLUID CHROMATOGRAPHY
TEMPERATURE EFFECTS
TESTING