There are a number of inherent problems associated with the analysis of polycyclic aromatic compounds (PAC) in airborne particulate matter. The compounds of interest constitute a very small fraction of the total sample, but consist of hundreds of different components. Therefore, analytical techniques with very high resolving power are required. To try to address these problems, methods have been developed and improved to isolate, and subsequently profile, and identify the PAC present in typical airborne particulate samples.
Since no single chromatographic technique can provide the desired resolution, a multi-stage clean-up scheme was required prior to analysis. Two methods were investigated in this study. Both methods used a Soxhlet extraction followed by fractionation using an adsorption chromatography step (silica or alumina) and Sephadex LH-20 to isolate the PAC fraction from the other organic constituents.
Another problem associated with the analysis of PAC in airborne particulate matter was because of the method of sample collection. It was believed that there were changes in the chemical composition of the particulate and hence the PAC, during sample collection using a Hi-Vol sampler. Artifacts were being formed by reaction of gaseous pollutants with the particulate collected on the filter. An experiment was established to show that the addition of a denuder bundle to a Hi-Vol sampler could reduce this artifact formation during sampling by removing the reactive gases prior to the surface of the filter. The value of the
denuder bundle was evaluated by comparison of the PAC from the denuder Hi-Vol with a standard Hi-Vol. Normal-phase HPLC coupled with mass spectrometry was shown to be a good method to compare the PAC in these samples. Some differences between standard and denuder Hi-Vol samples were observed in laboratory experiments, while the results from
field sampling were inconclusive. The use of a parallel column gas chromatography-mass
spectrometry (GC-MS) (also called third order chromatography) technique was investigated to determine its viability for the identification of the diverse range of PAC present in environmental samples. The PAC . in the NBS urban dust sample (SRM 1649) was analyzed to evaluate the method. To aid in data processing, a semi-automated peak detection
routine has been developed. This routine used programs to aid in the data processing by simplifying peak detection and allow calculation of the retention indices of the components. Using the information supplied by the retention indices and the mass spectra, a data base was developed that was applied to a typical airborne particulate sample. / Thesis / Doctor of Philosophy (PhD)
| Identifer | oai:union.ndltd.org:mcmaster.ca/oai:macsphere.mcmaster.ca:11375/29255 |
| Date | 02 1900 |
| Creators | Marr, Julie-Anne Carroll |
| Contributors | Quilliam, M. A., Chemistry |
| Source Sets | McMaster University |
| Language | English |
| Detected Language | English |
| Type | Thesis |
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