title: New benchmark for basic and neutral nitrogen compounds speciation in middle distillates using comprehensive two-dimensional gas chromatography.
abstract: This paper reports an analytical method for the comprehensive two-dimensional gas chromatography (GC x GC) separation and identification of nitrogen compounds (N-compounds) in middle distillates according to their types (basicity). For the evaluation of the best chromatographic conditions, a non-polar x polar approach was chosen. The impact of the second dimension (stationary phase and column length) on the separation of basic and neutral N-compounds was evaluated by mean of two-dimensional resolution. This study revealed that the implementation of polar secondary column having free electron pairs improves drastically the separation of N-compounds. Indeed, the presence of permanent dipole-permanent dipole interactions between neutral N-compounds and the stationary phase was enlightened. The comparison of two different nitrogen chemiluminescence detectors (NCD) was also evaluated for GC x GC selective monitoring of N-compounds. Owing to higher resolution power and enhanced sensitivity achieved using developed chromatographic and detection conditions, it was possible to identify univocally and to quantitate N-compounds (i) by class of compounds and (ii), within a class, by carbon number. Finally, quantitative comparison of GC x GC-NCD with conventional gas chromatography illustrates the benefits of GC x GC leading to an excellent correlation with results obtained by American Society for Testing Materials (ASTM) methods for the determination of basic/neutral nitrogen ratio in diesel samples.
authors: Institut Français du Pétrole, BP3, 69390 Vernaison, France.
authors: Frédérick
authors: F
authors: Adam
authors: Fabrice
authors: F
authors: Bertoncini
authors: Nicolas
authors: N
authors: Brodusch
authors: Emmanuelle
authors: E
authors: Durand
authors: Didier
authors: D
authors: Thiébaut
authors: Didier
authors: D
authors: Espinat
authors: Marie-Claire
authors: MC
authors: Hennion
mesh_terms: D002849:Chromatography, Gas / Q000379:methods*; D008163:Luminescent Measurements; D013058:Mass Spectrometry; D015394:Molecular Structure; D017672:Nitrogen Compounds / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results
chemical_list: D017672:Nitrogen Compounds