Analysis of heavy oils: Method development and application to Cerro Negro heavy petroleum detailed separation and analysis of acidic compounds

Technical Report · Sun Oct 01 04:00:00 EDT 1989

DOI:https://doi.org/10.2172/5696052· OSTI ID:5696052

Green, J. B.; Yu, S. K.T.; Green, J. A.; Doughty, D. A.; Vogh, J. W.; Grigsby, R. D.

An HPLC method for fractionation of whole acid concentrates into nominal compound class subfractions is described. The method utilizes silica columns and gradient elution with eluents containing a strong base, tetramethyl-ammonium hydroxide. The performance of the method is evaluated through analysis of subfractions obtained from a coal liquid, Wilmington, CA, petroleum and Cerro Negro heavy oil. Methods developed specifically for analysis of whole acid concentrates and subfractions are described in detail. These include: (1) an infrared method for determination of total hydroxyl and carboxyl groups after their conversion to trifluoroacetate and 2,2,2-trifluoresters, respectively. (2) an NMR method for functional group analysis based on methylation of acidic groups with {sup 13}C-enriched methyl iodide, (3) a nonaqueous titration procedure employing the potassium salt of dimethyl sulfoxide as a titrant for acidic compounds, (4) GC/MS analysis of hydroxyaromatic compounds after their conversion to trifluoroacetate esters, and (5) probe microdistillation high resolution mass spectrometric analysis of acid fractions exhibiting low volatility. 146 refs., 38 figs., 27 tabs.

• Research Organization: National Inst. for Petroleum and Energy Research, Bartlesville, OK (USA)
• Sponsoring Organization: DOE/FE
• DOE Contract Number: FC22-83FE60149
• OSTI ID: 5696052
• Report Number(s): NIPER-322; ON: DE89000769
• Country of Publication: United States
• Language: English

Related Subjects

02 PETROLEUM
023000* -- Petroleum-- Properties & Composition
CHEMICAL ANALYSIS
CHEMICAL REACTIONS
CHROMATOGRAPHY
DATA
DERIVATIZATION
ENERGY SOURCES
ESTERS
EXPERIMENTAL DATA
FOSSIL FUELS
FRACTIONATION
FUELS
INFORMATION
INFRARED SPECTRA
MAGNETIC RESONANCE
MASS SPECTRA
NUCLEAR MAGNETIC RESONANCE
NUMERICAL DATA
ORGANIC ACIDS
ORGANIC COMPOUNDS
PETROLEUM
RESONANCE
SEPARATION PROCESSES
SPECTRA
TITRATION