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

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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 ... continued below

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Schabron, John F.; Jr, Joseph F. Rovani & Sanderson, Mark June 1, 2006.

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Description

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.

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  • Report No.: none
  • Grant Number: FC26-98FT40322
  • DOI: 10.2172/886851 | External Link
  • Office of Scientific & Technical Information Report Number: 886851
  • Archival Resource Key: ark:/67531/metadc891706

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Office of Scientific & Technical Information Technical Reports

Reports, articles and other documents harvested from the Office of Scientific and Technical Information.

Office of Scientific and Technical Information (OSTI) is the Department of Energy (DOE) office that collects, preserves, and disseminates DOE-sponsored research and development (R&D) results that are the outcomes of R&D projects or other funded activities at DOE labs and facilities nationwide and grantees at universities and other institutions.

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  • June 1, 2006

Added to The UNT Digital Library

  • Sept. 23, 2016, 2:42 p.m.

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  • Dec. 7, 2016, 3:12 p.m.

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Schabron, John F.; Jr, Joseph F. Rovani & Sanderson, Mark. HEAVY OIL PROCESS MONITOR: AUTOMATED ON-COLUMN ASPHALTENE PRECIPITATION AND RE-DISSOLUTION, report, June 1, 2006; United States. (digital.library.unt.edu/ark:/67531/metadc891706/: accessed October 23, 2017), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.