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US 12,768,821 B2Granted
Method for separation and quantitation of heavy polycyclic aromatic hydrocarbons (HPAHs) using aromatic-selective size exclusion chromatography
AssigneeSaudi Arabian Oil Company
InventorsSaroj Kumar Panda, Ahmed M. Aldawood, Omer Refa Koseoglu
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Abstract
Heavy polycyclic aromatic hydrocarbons (HPAHs) are analyzed using aromatic-selective size exclusion chromatography for the separation and quantitation of HPAHs. This method is suitable to determine the concentration of HPAHs in mixtures that include coronene and other HPAHs including 8 or more rings, such as contained in hydrocracker bottoms, or in pyrolysis oil or tar.
Claims20
A method for separation and quantitation of heavy polycyclic aromatic hydrocarbons (HPAHs) in a sample comprising:
- providing the sample containing HPAHs, wherein HPAHs comprise polycyclic aromatics with at least 7 aromatic rings;
- diluting the sample in a sample dilution solvent by a dilution factor and filtering the diluted sample to recover a prepared sample solution;
- analyzing the prepared sample solution with a high-performance liquid chromatography (HPLC) system for aromatic-selective size exclusion chromatography (ASSEC),
- wherein the HPLC system comprises
- one or more HPLC columns packed with a stationary phase selected from the group consisting of silica, amino-bonded silica, and cyano-bonded silica,
- an elution solvent, and
- an HPLC detector;
- wherein ASSEC includes
- introducing a mobile phase of the injected prepared sample solution and the elution solvent into the HPLC column,
- flowing the mobile phase through the stationary phase for separation of HPAHs through the HPLC column based on molecular affinity relative to the stationary phase and based on size exclusion relative to the pore dimensions and particle size of the stationary phase and relative to interstitial volume of the HPLC column,
- discharging sample elute as a sample analyte and measuring responses for at least one characteristic of the sample analyte with the HPLC detector, and
- obtaining a chromatogram of the sample analyte based on the measured responses by the HPLC detector;
- identifying one or more peaks of the chromatogram of the sample analyte associated with HPAH compounds;
- calculating a peak characteristic from the one or more peaks of the chromatogram of the sample analyte associated with HPAH compounds;
- quantitating HPAHs in the sample containing HPAHs with a HPAH standards function obtained from regression of peak characteristics of plural reference HPAH standard solutions each having a reference HPAH compound comprising coronene, and using the peak characteristic and the dilution factor.
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Dependencies are inferred from the claim text.