Separation of large coal molecules using high resolution supercritical fluid chromatography. Annual report Mar 83-Feb 84
Technical Report
·
OSTI ID:6653957
Two new stationary phases have been synthesized for capillary supercritical fluid chromatography (SFC). A methyl-2-phenylethyl polysiloxane is autocrosslinkable with the application of heat, and no chemical free-radical initiators are needed. This should simplify the preparation of small diameter capillary columns which are needed for SFC. A polarizable biphenyl polysiloxane has also been synthesized. This phase offers unique selectivity for polycyclic aromatic compounds containing polar substituents. Elevated coating bath temperatures, mixed coating solution solvents, and new azo compounds for free-radical initiation have significantly aided in the preparation of small diameter columns. Columns of 50 micrometer i.d. have been prepared that demonstrate on the order of 3500 theoretical plates/meter. Pure n-pentane appears to be the most suitable mobile phase for the chromatography of coal-derived materials. The addition of various modifiers such as benzene, isopropanol, and dichloromethane showed no significant increase in solving power. A supercritical fluid chromatograph has been interfaced to a quadrupole mass spectrometer. Although, the mass spectrometer can be operated in both electron impact and chemical ionization modes, greater sensitivity is obtained in the chemical ionization mode.
- Research Organization:
- Brigham Young Univ., Provo, UT (USA). Dept. of Chemistry
- OSTI ID:
- 6653957
- Report Number(s):
- PB-84-198563
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
01 COAL, LIGNITE, AND PEAT
010600* -- Coal
Lignite
& Peat-- Properties & Composition
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400105 -- Separation Procedures
AROMATICS
CARBONACEOUS MATERIALS
CHEMICAL ANALYSIS
CHROMATOGRAPHY
COAL
ENERGY SOURCES
FOSSIL FUELS
FUELS
HYDROCARBONS
IONIZATION
MASS SPECTROSCOPY
MATERIALS
MOLECULAR STRUCTURE
MOLECULAR WEIGHT
ORGANIC COMPOUNDS
ORGANIC SILICON COMPOUNDS
POLYCYCLIC AROMATIC HYDROCARBONS
SEPARATION PROCESSES
SILOXANES
SOLVENTS
SPECTROSCOPY
010600* -- Coal
Lignite
& Peat-- Properties & Composition
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400105 -- Separation Procedures
AROMATICS
CARBONACEOUS MATERIALS
CHEMICAL ANALYSIS
CHROMATOGRAPHY
COAL
ENERGY SOURCES
FOSSIL FUELS
FUELS
HYDROCARBONS
IONIZATION
MASS SPECTROSCOPY
MATERIALS
MOLECULAR STRUCTURE
MOLECULAR WEIGHT
ORGANIC COMPOUNDS
ORGANIC SILICON COMPOUNDS
POLYCYCLIC AROMATIC HYDROCARBONS
SEPARATION PROCESSES
SILOXANES
SOLVENTS
SPECTROSCOPY