HEAVY OIL PROCESS MONITOR: AUTOMATED ON-COLUMN ASPHALTENE PRECIPITATION AND RE-DISSOLUTION

Technical Report · Thu Jun 01 04:00:00 EDT 2006

DOI:https://doi.org/10.2172/886851· OSTI ID:886851

Schabron, John F ^[1]; Rovani, Jr, Joseph F; Sanderson, Mark

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1. Western Research Institute

About 37-50% (w/w) of the heptane asphaltenes from unpyrolyzed residua dissolve in cyclohexane. As pyrolysis progresses, this number decrease to below 15% as coke and toluene insoluble pre-coke materials appear. This solubility measurement can be used after coke begins to form, unlike the flocculation titration, which cannot be applied to multi-phase systems. Currently, the procedure for the isolation of heptane asphaltenes and the determination of the amount of asphaltenes soluble in cyclohexane spans three days. A more rapid method to measure asphaltene solubility was explored using a novel on-column asphaltene precipitation and re-dissolution technique. This was automated using high performance liquid chromatography (HPLC) equipment with a step gradient sequence using the solvents: heptane, cyclohexane, toluene:methanol (98:2). Results for four series of original and pyrolyzed residua were compared with data from the gravimetric method. The measurement time was reduced from three days to forty minutes. The separation was expanded further with the use of four solvents: heptane, cyclohexane, toluene, and cyclohexanone or methylene chloride. This provides a fourth peak which represents the most polar components, in the oil.

• Research Organization: Western Research Institute
• Sponsoring Organization: USDOE
• DOE Contract Number: FC26-98FT40322
• OSTI ID: 886851
• Country of Publication: United States
• Language: English

Related Subjects

01 COAL, LIGNITE, AND PEAT
02 PETROLEUM
ASPHALTENES
COKE
CYCLOHEXANE
CYCLOHEXANONE
FLOCCULATION
HEPTANE
HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY
METHYLENE CHLORIDE
PETROLEUM
PRECIPITATION
PYROLYSIS
SOLUBILITY
SOLVENTS
TITRATION
TOLUENE
VISCOSITY