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High Performance Liquid Chromatography of Petroleum Asphaltenes and Capillary Electrophoresis of Glycosaminoglycan Carbohydrates

Loegel, Thomas N.
http://rave.ohiolink.edu/etdc/view?acc_num=miami1354241855

Abstract Details

2012, Doctor of Philosophy, Miami University, Chemistry and Biochemistry.
Separations involving structurally similar high molecular weight compounds have become an important challenge in analytical chemistry. Specific compounds in asphaltenes, the heaviest component of petroleum, have yet to be positively separated and identified. Separation difficulties such as mobile phase and column compatibility force the selection of uncommon solvents and stationary phases. Liquid chromatographic separation of asphaltenes using a cyano-propyl and amino-propyl column with an optimized reverse phase gradient using UV and ¿¿¿¿¿¿¿uorescence as well as mass spectrometry (MS) detection has been demonstrated. The degree of asphaltene aggregation can be followed. Extensive work has determined that the solvent N-methyl-2-pyrrolidinone is a suitable chromatographic solvent but limits the interpretation of MS spectra. The cyano-propyl column is found to be less prone to degradation but the amino-propyl column produced more selective separations. With both columns the molecular weight distribution determined by mass spectrometry is fairly constant, indicating that the retention mechanism is not size-exclusion but more likely partitioning/adsorption. Characterization of different asphaltene samples using the more stable polymeric amino-propyl column is also shown. Improved analytical methods for glucosaminoglycans, such as the anticoagulant heparin, have become quite urgent to prevent any future adulteration cases. Capillary electrophoresis of heparin, dermatan sulfate, and over-sulfated chondroitin sulfate using ethylenediamine as an ion pairing reagent showed a marked change in peak migration order. Other glycosaminoglycans, including chondroitin sulfate and hyaluronic acid, were separated from heparin. Progress toward the characterization of a low cost teaching gas chromatography instrument for the use in a multi-analysis student data collection system has also been made.
Neil Danielson, PhD (Advisor)
André Sommer, PhD (Committee Chair)
Jon Scaffidi, PhD (Committee Member)
Richard Taylor, PhD (Committee Member)
Paul James, PhD (Committee Member)
202 p.
Energy; Petroleum Engineering; Petroleum Production
glucosaminoglycans; asphaltenes; PAHs; HPLC; Fuel; Petroleum; Heparin; Gas Chromatography

Recommended Citations

Citations

  • Loegel, T. N. (2012). High Performance Liquid Chromatography of Petroleum Asphaltenes and Capillary Electrophoresis of Glycosaminoglycan Carbohydrates [Doctoral dissertation, Miami University]. OhioLINK Electronic Theses and Dissertations Center. http://rave.ohiolink.edu/etdc/view?acc_num=miami1354241855

    APA Style (7th edition)

  • Loegel, Thomas. High Performance Liquid Chromatography of Petroleum Asphaltenes and Capillary Electrophoresis of Glycosaminoglycan Carbohydrates. 2012. Miami University, Doctoral dissertation. OhioLINK Electronic Theses and Dissertations Center, http://rave.ohiolink.edu/etdc/view?acc_num=miami1354241855.

    MLA Style (8th edition)

  • Loegel, Thomas. "High Performance Liquid Chromatography of Petroleum Asphaltenes and Capillary Electrophoresis of Glycosaminoglycan Carbohydrates." Doctoral dissertation, Miami University, 2012. http://rave.ohiolink.edu/etdc/view?acc_num=miami1354241855

    Chicago Manual of Style (17th edition)

miami1354241855
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© 2012, some rights reserved.Creative Commons License High Performance Liquid Chromatography of Petroleum Asphaltenes and Capillary Electrophoresis of Glycosaminoglycan Carbohydrates by Thomas N. Loegel is licensed under a Creative Commons Attribution-NonCommercial-NoDerivs 3.0 Unported License. Based on a work at etd.ohiolink.edu.
This open access ETD is published by Miami University and OhioLINK.