Development and evaluation of supercritical fluid chromatography/mass spectrometry for polar and high-molecular-weight coal components: Technical progress report for the period October 1, 1985 - September 30, 1986

Technical Report · Sun Feb 01 04:00:00 EST 1987

DOI:https://doi.org/10.2172/6828356· OSTI ID:6828356

Chess, E K; Kalinoski, H T; Wright, B W; Smith, R D

Technical progress toward the programmatic goals of developing and evaluating SFC/MS for the analysis of higher-molecular-weight compounds was made in the following areas: Studies have been conducted to characterize the requirements for and to facilitate the transfer of thermal energy to the capillary flow restrictor region. Such studies have resulted in a new interface probe design which allows better transport of higher molecular weight, less volatile compounds decreasing the mass discrimination at the supercritical fluid chromatograph mass spectrometer interface region. Calibration of the magnetic sector mass spectrometer to 1400 daltons has been developed. A digital syringe pump controller, interfaced to an Apple IIe computer allows much finer and more reproducible control of the pressure (density) of the supercritical fluid mobile phase. Nonpolar supercritical fluid mobile phases have been modified by the addition of small amounts of polar fluids to create fluids with higher solvating powers than, but with similar operating parameters. An in-depth knowledge of the fluid behavior is required for successful utilization of these modified fluids. Polar-modified fluids have been used with three types of supercritical fluid introduction to the mass spectrometer: direct fluid injection, supercritical fluid chromatography, and supercritical fluid extraction. Capillary columns evaluated for stability indicated that our present methods for preparing columns are sufficient, for many of the stationary phase and supercritical fluid combinations tested, to create columns that can be used successfully with supercritical fluid chromatography. 9 refs., 11 figs.

• Research Organization: Pacific Northwest Lab., Richland, WA (USA)
• DOE Contract Number: AC06-76RL01830
• OSTI ID: 6828356
• Report Number(s): PNL-6140; ON: DE87006602
• Country of Publication: United States
• Language: English

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47 OTHER INSTRUMENTATION
ACETONE
ACETONITRILE
ALCOHOLS
AROMATICS
BENZENE
CALIBRATION
CHEMICAL ANALYSIS
CHROMATOGRAPHY
COAL LIQUIDS
CRITICAL PRESSURE
CRITICAL TEMPERATURE
ETHANOL
ETHERS
ETHYL ETHER
EVALUATION
FLUIDS
FRACTIONATION
HYDROCARBONS
HYDROXY COMPOUNDS
INTERFACES
KETONES
LIQUIDS
METHANOL
METHYLENE CHLORIDE
NITRILES
ORGANIC CHLORINE COMPOUNDS
ORGANIC COMPOUNDS
ORGANIC HALOGEN COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
ORGANIC SOLVENTS
PERFORMANCE TESTING
PHYSICAL PROPERTIES
POLAR COMPOUNDS
QUANTITATIVE CHEMICAL ANALYSIS
SEPARATION PROCESSES
SOLVENTS
SUPERCRITICAL FLUID CHROMATOGRAPHY
TESTING
THERMODYNAMIC PROPERTIES
TRANSITION TEMPERATURE