Sample preparation procedure for the determination of polycyclic aromatic hydrocarbons in petroleum vacuum residue and bitumen |
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Authors: | Gilgenast Ewelina Boczkaj Grzegorz Przyjazny Andrzej Kamiński Marian |
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Institution: | (1) Chemical Faculty, Department of Chemical and Process Engineering, Gdansk University of Technology, Narutowicza St. 11/12, 80-233 Gdansk, Poland;(2) Chemistry & Biochemistry Department, Kettering University, 1700 West Third Avenue, Flint, MI 48504, USA; |
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Abstract: | This paper describes a novel method of sample preparation for the determination of trace concentrations of polycyclic aromatic
hydrocarbons (PAHs) in high-boiling petroleum products. Limits of quantitation of the investigated PAHs in materials of this
type range from tens of nanograms per kilogram to <20 μg/kg. The studies revealed that in order to separate most of interferences
from the analytes without a significant loss of PAHs, it is necessary to use size exclusion chromatography as the first step
of sample preparation, followed by adsorption using normal-phase liquid chromatography. The use of orthogonal separation procedure
described in the paper allows the isolation of only a group of unsubstituted and substituted aromatic hydrocarbons with a
specific range of molar mass. The lower the required limit of quantitation of PAHs, the larger is the scale of preparative
liquid chromatography in both steps of sample preparation needed. The use of internal standard allows quantitative results
to be corrected for the degree of recovery of PAHs during the sample preparation step. Final determination can be carried
out using HPLC-FLD, GC-MS, or HPLC-UV–VIS/DAD. The last technique provides a degree of identification through the acquired
UV–VIS spectra. |
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