Comprehensive two-dimensional liquid chromatography of heavy oil

Heavy oil refers to the part of crude oil that is not amenable to further distillation. Processing of these materials to useful products provides added value, but requires advanced technology as well as extensive characterization in order to optimize the yield of the most profitable products. The use of comprehensive two-dimensional liquid chromatography (LC × LC) was investigated for the characterization of de-asphalted short residue, also called maltenes. Initial studies were performed on a polycyclic aromatic hydrocarbon standard, an aromatic extract of hydrowax, and the fractions obtained after sol- vent fractionation of the maltenes. Cyanopropyl- and octadecyl-silica were used as first-dimension and second-dimension columns, respectively. The analysis of the maltenes and fractions thereof required a change in first-dimension stationary phase to biphenyl as well as an increase in modifier strength to improve recovery. The extensive characterization of maltenes with LC × LC within four hours was demonstrated. The Program for the Interpretive Optimization of Two-dimensional Resolution (PIOTR) has been applied to aid the method development, but due to the absence of specific peaks in the chromatograms it was challenging to apply to the maltenes or its fractions. Nonetheless, an approach is suggested for resolution optimization in cases such as the present one, in which regions of co-elution are observed, rather than clearly separated peaks

Development and evaluation of an interface for coupled capillary supercritical-fluid chromatography / magnetic sector mass spectrometry : application to thermally instable and high molecular mass compounds

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Development and evaluation of an interface for coupled capillary supercritical fluid chromatography/magnetic sector mass spectrometry : application to thermally unstable and high molecular mass compounds

An interface for coupling supercritical fluid chromatography to a magnetic sector mass spectrometer was developed and evaluated. The interface is based on direct introduction of the mobile phase, carbon dioxide, into the ion-source of the mass spectrometer. The SFC-MS system was optimized with respect to the signal-to-noise ratio. Under optimized conditions, the estimated detection limit for n-pentadecane is approximately 30 ppm. Spectra obtained in the electron-impact ionization mode show a very good similarity with library spectra. The performance of the SFC-MS system was evaluated by the analysis of a number of test mixtures. A sample containing several low molecular mass, thermally unstable compounds, which could neither be analyzed by GC-MS nor by LC-MS, was analyzed. Also for the analysis of high molecular mass compounds, the coupled system showed a good performance