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Date of Award

9-1983

Degree Type

Thesis

Degree Name

Doctor of Philosophy (PhD)

Department

Chemistry

Supervisor

Dr. M.A. Quilliam

Abstract

Analytical methodology has been developed for the determination of nitro polycyclic aromatic hydrocarbons (nitro-PAHs), polycyclic aromatic hydrocarbons (PAHs) and other PAH derivatives in diesel exhaust and urban airborne particulate samples. Samples were Soxhlet extracted with methylene chloride for twenty-four hours and the organic extract filtered to remove particulate matter. This extract was taken through a three stage clean-up procedure. Very polar materials were initially removed using a silica Sep-Pak. The aromatic compounds were than separated from the aliphatic substances by Sephadex LH-20 chromatography. Normal phase semi-preparative high performance liquid chromatography was used for the final fractionation of the aromatic compounds. Three fractions, containing PAHs (Fraction A), nitro-PAHs (Fraction B) and dinitro-PAHs (Fraction C), were collected for further analysis. Two diesel exhaust (Oldsmobile and Peugeot) and four airborne particulate (Toronto and Hamilton, Ontario) samples were taken through this procedure.

Capillary column gas chromatography (GC) with flame ionization and nitrogen-selective detection was used for the detection and quantitation of nitro-PAHs. Confirmation of the identity of nitro-PAHs was done by capillary column GC-MS in the selected-ion-monitoring mode and other compounds were identified by capillary column GC-MS in the full scanning mode of operation.

Nitro-PAHs including 1-nitropyrene, nitro(phenanthrenes/anthracenes), methylnitro(phenanthrenes/anthracenes), nitrobenzo[a]fluorene and 6-nitrobenzo[a]pyrene were confirmed and quantitated in the samples using 1-nitronaphthalene as an internal standard. PAHs, found in Fraction A, and oxygenated-PAHs (e.g., ketone- and quinonederivatives of PAHs) found in Fractions B and C were tentatively identified and their levels estimated.

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