Abstract
A method was developed for identifying and determining benzo(a)pyrene in a filtered retort water sample from an in situ oil shale process by employing liquid-liquid extraction, dry-column chromatography, thin-layer chromatography and fluorescence spectrometry. The accuracy and precision of the method were good, and the limit of detection was approximately 0.08 ppB. Irreproducible results were obtained with unfiltered retort water samples. Programmed multiple development was used to a limited extent in the separation of polycyclic aromatic hydrocarbons from a shale oil sample. However, results indicated that this separation technique should be investigated further in the separation of polycyclic aromatic hydrocarbons. Benzo(a)pyrene was determined in several shale oil samples by methods developed previously. Polycyclic aromatic hydrocarbons were characterized in several shale oil samples using open-column, dry-column and thin-layer chromatography as separation steps. Visible fluorescence from the separated components on chromatoplates was measured directly to obtain fluorescence profiles of the components on the chromatoplates. Several comparisons were made among the shale oil samples as to the relative amounts of 6-, 5-, 4- and 3-ring polycyclic aromatic hydrocarbons. The theoretical and practical analytical aspects of the room temperature phosphorescence of nitrogen heterocycles were investigated. Intense room temperature phosphorescence was obtained from several nitrogen heterocycles when these compounds were absorbed on silica gel. Theoretical explanations were given for the intense phosphorescence. Benzo(f)quinoline and phenanthridine were separated from a shale oil sample by open-column and high performance liquid chromatography, and then identified by room temperature phosphorescence.
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