Development of heart-cutting multidimensional gas chromatography coupled to time of flight mass spectrometry for silicon speciation at trace levels in gasoline samples

作者：Chainet Fabien^*; Lienemann Charles Philippe; Ponthus Jeremie; Courtiade Marion; Donard Olivier Francois Xavier

来源：Journal of Chromatography A, 2012, 1264: 80-86.

DOI：10.1016/j.chroma.2012.09.020

• Gas chromatography
• Heart cutting
• Deans switch
• Silicon
• Trace level
• Characterization
• Gasoline

To improve the understanding of hydrotreatment (HDT) catalyst poisoning by silicon species, these molecules must be characterized in petroleum products using powerful analytical systems. Heart-cutting gas chromatography coupled to time of flight mass spectrometry (GC-GC/TOFMS) method equipped with a Deans switch (DS) system was developed for the direct characterization of target silicon compounds at trace level (mu g kg(-1)) in gasoline samples. This method was performed to identify silicon compounds never characterized before. After the selection of the second dimension column using GC-GC-FID, GC-GC/TOFMS was performed. The calibration curves obtained by the GC-GC/TOFMS method were linear up to 1000 mu g kg(-1). Limits of detection (LOD) were ranging from 5 to 33 mu g kg(-1) in spiked gasoline. The method provided sufficient selectivity and sensitivity to characterize known silicon compounds thanks to their specific ions and their retention times. The analysis of a naphtha sample by GC-GC/TOFMS has shown the presence of cyclic siloxanes (D-n) as major compounds of PDMS thermal degradation with the occurrence of linear siloxanes, especially hexamethyldisiloxane (L-2), which was never characterized in petroleum products but already known as severe poison for catalyst.

• 出版日期2012-11-16