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Characterization of Petroleum Heavy Oil Fractions Prepared by Preparatory Liquid Chromatography with Thin-Layer Chromatography, High-Resolution Mass Spectrometry, and Gas Chromatography with an Atomic Emission Detector
In
this study, a preparatory-scale fractionation method was developed.
To verify the effectiveness of this method, an oil sample was fractionated
into five fractions, referred to as saturate, aro1, aro2, polar1,
and polar2; these fractions were completely characterized by thin-layer
chromatography–flame ionization detection (TLC–FID),
field desorption (FD) and (+) atmospheric pressure photoionization
(APPI) high-resolution mass spectrometry (HR-MS), and gas chromatography
with an atomic emission detector (GC–AED). TLC–FID analysis
was used to compare the results obtained by the fractionation method
to those obtained from the conventional saturates, aromatics, resins,
and asphaltenes (SARA) method. FD–MS was employed to characterize
the hydrocarbon class compounds in the saturate and aro1 fractions.
As observed from the FD–MS spectra, non-aromatic hydrocarbon
compounds were abundant in saturates, while mono- and diaromatic compounds
were abundant in the aro1 fraction. This result is in good agreement
with those obtained by HR-MS. (+) APPI HR-MS analysis of fractions
showed that aromaticity increases from saturates to the polar1 fraction
but decreases in the polar2 fraction. Heteroatom class distributions
investigated by (+) APPI HR-MS showed that non-basic nitrogen compounds
were abundant in polar1, while non-aromatic sulfur compounds were
abundant in the polar2 fraction. From the results obtained by the
GC–AED analysis of fractions, nickel porphyrin compounds were
concentrated in the polar1 fraction. Hence, the combined results clearly
demonstrate that the fractionation method is effective for isolating
fractions on a preparative scale