Separation of basic compounds with maintenance of adequate peak shape has been among the most taxing of HPLC applications. Also, complete chemical class fractionation of various fuel oils has been difficult with the methods currently in use. A novel stationary phase based on newly developed surface bonding organophosphate chemistry was developed to address both of these HPLC problems using relatively simple operational procedures. The stationary phase was synthesized, characterized, and packed into a 4.6 x 250 mm HPLC column prior to conducting the HPLC investigations. Studies to investigate the peak shape of basic compounds, the separation of individual basic compounds, class fractionation using model fuel oil compounds, and class fractionation of actual fuel oil samples were conducted. The stationary phase produced chromatographic peaks of basic compounds which demonstrated minimal tailing. Chromatographic separations of various basic compounds were performed to demonstrate the increased resolution possible with a column exhibiting these characteristics. The class fractionation of fuel oils was demonstrated first using model compounds followed by the fractionation of actual fuel oil samples. Recovery studies were also performed for the fuel oil fractionation. The novel stationary phase produced exhibited characteristics which are desirable for the stated applications. Minimal tailing was produced without the use of buffers or the degradation of the column while performing chromatographic separations of basic compounds. A four class fractionation of fuel oil was produced using a linear binary gradient. Both of these results are significant advances in addressing the two stated chromatographic problems.
| Identifer | oai:union.ndltd.org:UMASS/oai:scholarworks.umass.edu:dissertations-8387 |
| Date | 01 January 1992 |
| Creators | Stewart, Charles W. |
| Publisher | ScholarWorks@UMass Amherst |
| Source Sets | University of Massachusetts, Amherst |
| Language | English |
| Detected Language | English |
| Type | text |
| Source | Doctoral Dissertations Available from Proquest |
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