The present research is focused on the development of a flow-modulated comprehensive two-dimensional gas chromatography-triple quadrupole mass spectrometry (FM GC. ×. GC-MS/MS) method for the determination of classes of aromatic organic sulphur compounds (benzothiophenes, dibenzothiophenes, and benzonaphthothiophene) in heavy gas oil (HGO). The MS/MS instrument was used to provide both full-scan and multiple-reaction-monitoring (MRM) data. Linear retention index (LRI) ranges were used to define the MRM windows for each chemical class. Calibration solutions (internal standard: 1-fluoronaphthalene) were prepared by using an HGO sample, depleted of S compounds. Calibration information was also derived for the thiophene class (along with MRM and LRI data), even though such constituents were not present in the HGO. Linearity was satisfactory over the analyzed concentration range (1-100. mg/L); intra-day precision for the lowest calibration point was always below 17%. Accuracy was also satisfactory, with a maximum percentage error of 3.5% (absolute value) found among the S classes subjected to (semi-)quantification. The highest limit of quantification was calculated to be 299. μg/L (for the C1-benzothiophene class), while the lowest was 21. μg/L (for the C4-benzothiophene class).
Determination of aromatic sulphur compounds in heavy gas oil by using (low-)flow modulated comprehensive two-dimensional gas chromatography–triple quadrupole mass spectrometry
FRANCHINA, FLAVIO ANTONIO;
2015
Abstract
The present research is focused on the development of a flow-modulated comprehensive two-dimensional gas chromatography-triple quadrupole mass spectrometry (FM GC. ×. GC-MS/MS) method for the determination of classes of aromatic organic sulphur compounds (benzothiophenes, dibenzothiophenes, and benzonaphthothiophene) in heavy gas oil (HGO). The MS/MS instrument was used to provide both full-scan and multiple-reaction-monitoring (MRM) data. Linear retention index (LRI) ranges were used to define the MRM windows for each chemical class. Calibration solutions (internal standard: 1-fluoronaphthalene) were prepared by using an HGO sample, depleted of S compounds. Calibration information was also derived for the thiophene class (along with MRM and LRI data), even though such constituents were not present in the HGO. Linearity was satisfactory over the analyzed concentration range (1-100. mg/L); intra-day precision for the lowest calibration point was always below 17%. Accuracy was also satisfactory, with a maximum percentage error of 3.5% (absolute value) found among the S classes subjected to (semi-)quantification. The highest limit of quantification was calculated to be 299. μg/L (for the C1-benzothiophene class), while the lowest was 21. μg/L (for the C4-benzothiophene class).I documenti in SFERA sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
