Polycyclic aromatic hydrocarbons (PAHs) in harbour sediment have been determined by means of Shpol'skii fluorometry. Fundamental aspects of this cryogenic high resolution technique are discussed. It provides characteristic spectra of aromatic molecules that can be successfully employed for identification purposes. Extra selectivity is obtained by making use of selective excitation, even with a broad-banded light source. Highly specific quantitative determinations can be achieved, due to the quasi-linear character of the spectra. Deuterated PAHs are suitable as internal standards. Calibration curves with linearity from 10#x2212;5-10#x2212;6M down to the detection limit are found, yielding a dynamic range from 2 to 4 decades for the compounds investigated. The reproducibility of the quantitative experiment lies between 6 and 20 per cent. The results obtained with Shpol'skii spectroscopy are in good agreement with data found by a standard method of analysis employing fluorescence detected HPLC.
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