Element-specific detector studies in derivitization of shale oil

Thesis/Dissertation · Wed Jan 01 04:00:00 EST 1986

OSTI ID:6901639

Stuff, J R

The investigation of an atmospheric pressure helium microwave induced plasma (MIP) detector for deuterium specific detection in gas chromatography (GC) was conducted. Several deuterated compounds were tested for linearity of response, minimal detectable amount, selectivity vs carbon and response related to chemical environment of the deuterium atoms. The investigation of the MIP as a fluorine specific detector for GC was conducted. A study of the substitution effect of various substituted benzenesulfonyl fluorides on the mass spectral (MS) breakdown of the sulfonyl fluoride group was conducted and the results compared to previous work done on sulphones and sulfonyl chlorides. The effect of sulfonation of an aromatic fraction of shale oil to form sulfonic acids was performed. The sulfonic acids were derivitized to form sulfonyl fluorides and the products identified by GC-MIP (fluorine specific) and GC-MS. The aromatics and polars fraction from a shale oil sample were derivitized with various chlorinating reagents in order to provide a means for distinguishing alkylated and non-alkylated aromatic ring systems. The products were identified by GC-MIP (C and Cl specific detection) and GC-MS. The continued development of flexible, soft glass capillary columns with an outer polyimide coating was conducted. Two columns of lengths 20 m and 15 m were coated internally with OV-101 (methyl silicone) stationary phase and one column with OV-3 (10% phenyl/methyl silicone) stationary phase. The columns were tested with various standard mixtures to characterize them and then were applied to the separation of various crude oils.

• Research Organization: Massachusetts Univ., Amherst (USA)
• OSTI ID: 6901639
• Country of Publication: United States
• Language: English

Related Subjects

04 OIL SHALES AND TAR SANDS
040500* -- Oil Shales & Tar Sands-- Properties & Composition
CHEMICAL REACTIONS
CHROMATOGRAPHY
DERIVATIZATION
DEUTERIUM
ELEMENTS
ENERGY SOURCES
FLUORINE
FOSSIL FUELS
FUELS
GAS CHROMATOGRAPHY
HALOGENS
HYDROGEN ISOTOPES
ISOTOPES
LIGHT NUCLEI
MASS SPECTROSCOPY
MEASURING INSTRUMENTS
MINERAL OILS
NONMETALS
NUCLEI
ODD-ODD NUCLEI
OILS
ORGANIC COMPOUNDS
OTHER ORGANIC COMPOUNDS
PERFORMANCE TESTING
SEPARATION PROCESSES
SHALE OIL
SPECIFICITY
SPECTROSCOPY
STABLE ISOTOPES
STRUCTURAL CHEMICAL ANALYSIS
SULFONATION
TESTING