Overcoming the high-temperature two-dimensional gas chromatography limits to elute heavy compounds.

Overcoming high-temperature (HT) two-dimensional gas chromatography (GC × GC) limits is critical for the analysis of heavy hydrocarbons, particularly those contained in heavy petroleum fractions. To reach this goal, HT-GC × GC analysis was adapted from HT-GC Simulated Distillation (HT-GC SimDist) operating conditions as this analysis embraces compounds whose boiling point ranges from 35 °C to 700 °C and from a previous study that enabled the elution of linear alkane nC(60) and tetraaromatic compounds by HT-GC × GC. This paper shows that HT-GC × GC analysis using CO(2) cryogenic modulator and short wide bore columns with a thin film of stationary phase allows the elution of linear alkanes up to nC(68) (641 °C) as well as of highly aromatic hydrocarbons like coronene. Furthermore, compared to previous studies, an on-column injector was used to reduce discrimination of high boiling point compounds.

Global approach for the selection of high temperature comprehensive two-dimensional gas chromatography experimental conditions and quantitative analysis in regards to sulfur-containing compounds in heavy petroleum cuts.

Extending the knowledge on sulfur-containing compounds is crucial for the petroleum industry because they contribute to atmospheric pollution by combustion. Most of them are concentrated in heavy petroleum cuts, such as vacuum gas oils (VGOs). However, the resolution of the existing analytical methods does not allow a quantitative speciation of S-compounds contained in VGOs. Therefore, a high temperature GC×GC chromatograph hyphenated to a SCD was implemented in this study to obtain a quantitative S-compounds speciation. Firstly, various thermally stable stationary phases, in particular the new ionic liquid IL59 and Mega Wax-HT, were investigated in 1D-GC as a way to reduce the number of columns sets to be used in GC×GC. Consequently, several normal and reversed configurations of these columns were selected and tested in GC×GC. Then, a decision method was applied to facilitate the choice of the best combination of columns. Finally, the most adapted methods led to an innovative group type quantification and to a quantitative distribution of heavy sulfur species contained in a VGO sample. These results represent a major step towards the study of S-compounds in heavy petroleum cuts.