Development of chromatographic and mass spectrometric techniques for the analysis of complex mixtures containing aromatic compounds.

• Main Author: Perreault, Helene.
• Other Authors: Ph.D.
• Format: Text
• Language: English
• Published: Dalhousie University 2014
• Subjects: Chemistry; Analytical; Engineering; Petroleum; Environmental Sciences; Canada; Fort McMurray
• Online Access: http://hdl.handle.net/10222/55303

Polycyclic aromatic compounds (PACs) are of great interest because they are widespread in the environment and comprise many potent mutagens and carcinogens. The main objective of this work was to characterize the PAC content of complex matrices. The materials studied in this work were a contaminated estuary sediment sample (Sydney Tar Pond, Nova Scotia), as well as samples obtained at three different stages of the processing of oil sands into synthetic crude oil (Syncrude Canada Ltd., Fort McMurray, Alberta). The characterization of the PAC content of each sample required development and application of specific sampling, extraction, fractionation and final analysis techniques. The application and development of open column chromatographic fractionation methods and chromatographic/mass spectrometric techniques was emphasized. The fractionation methods used varied depending on the origin of the samples. Gas chromatography, high performance liquid chromatography and supercritical fluid chromatography combined with mass spectrometry (GC/MS, HPLC/MS and SFC/MS) were used for final analysis of the PAC fractions. All three techniques were suitable for the analysis of the sediment sample; however, GC/MS failed in the characterization of oil sand-derived samples due to the low volatility of their components. The sediment material was found to contain mainly unsubstituted polycyclic aromatic hydrocarbons (PAHs), whereas the oil sand-derived samples contained alkylated-PAHs and alkylated carbazoles as the predominant species. Mass spectrometric selectivity enhancement for the detection of polycyclic aromatic hydrocarbons containing a nitrogen atom was also investigated using three different methods, each using the half-integral mass of the doubly charged molecular ions as the selectivity factor. Thesis (Ph.D.)--Dalhousie University (Canada), 1992.