Application of isotope-ratio-monitoring gas chromatography/mass spectrometry to study carbonization reactions of FCCU slurry oils

T. R. Filley, R. M. Filley, Semih Eser, Katherine Haines Freeman

Research output: Contribution to journalArticle

Abstract

Delayed coking of Fluid Catalytic Cracking Unit (FCCU) slurry oils produces needle cokes which are used in the manufacture of graphite electrodes for electric-arc furnaces. The structure and properties of needle cokes depend on the formation of a liquid crystalline phase (carbonaceous mesophase) during delayed coking. Thermal reactivity of individual compounds in slurry oils effectively controls the initial carbonization reactions, and, thus, the degree of mesophase development. In this study, isotope-ratio-monitoring gas chromatography mass-spectromelry was used in conjunction with a 13C-labeled dopant (4-methyldibenzothiophene) to determine the distribution of the labeled methyl group on the GC-amenable products from carbonization of three different FCCU slurry oils. Selective removal of the unreacted dopant and its methylated analogs from the reaction products by ligand exchange chromatography allowed the isotope analyses of selected aromatic compounds. The 13C enrichment of selected aromatic compounds, including some isomers, was determined to compare the relative thermal reactivities of different compounds as well as the reactivities of different sites on a given aromatic compound.

Original languageEnglish (US)
Pages (from-to)938-940
Number of pages3
JournalAm Chem Soc Div Fuel Chem Prepr
Volume42
Issue number3
StatePublished - 1997

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Fluid catalytic cracking
Aromatic compounds
Carbonization
Gas chromatography
Isotopes
Mass spectrometry
Coking
Needles
Monitoring
Doping (additives)
Graphite electrodes
Electric arcs
Chromatography
Reaction products
Isomers
Ion exchange
Furnaces
Ligands
Crystalline materials
Liquids

All Science Journal Classification (ASJC) codes

  • Energy(all)

Cite this

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title = "Application of isotope-ratio-monitoring gas chromatography/mass spectrometry to study carbonization reactions of FCCU slurry oils",
abstract = "Delayed coking of Fluid Catalytic Cracking Unit (FCCU) slurry oils produces needle cokes which are used in the manufacture of graphite electrodes for electric-arc furnaces. The structure and properties of needle cokes depend on the formation of a liquid crystalline phase (carbonaceous mesophase) during delayed coking. Thermal reactivity of individual compounds in slurry oils effectively controls the initial carbonization reactions, and, thus, the degree of mesophase development. In this study, isotope-ratio-monitoring gas chromatography mass-spectromelry was used in conjunction with a 13C-labeled dopant (4-methyldibenzothiophene) to determine the distribution of the labeled methyl group on the GC-amenable products from carbonization of three different FCCU slurry oils. Selective removal of the unreacted dopant and its methylated analogs from the reaction products by ligand exchange chromatography allowed the isotope analyses of selected aromatic compounds. The 13C enrichment of selected aromatic compounds, including some isomers, was determined to compare the relative thermal reactivities of different compounds as well as the reactivities of different sites on a given aromatic compound.",
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journal = "Am Chem Soc Div Fuel Chem Prepr",
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AU - Filley, T. R.

AU - Filley, R. M.

AU - Eser, Semih

AU - Freeman, Katherine Haines

PY - 1997

Y1 - 1997

N2 - Delayed coking of Fluid Catalytic Cracking Unit (FCCU) slurry oils produces needle cokes which are used in the manufacture of graphite electrodes for electric-arc furnaces. The structure and properties of needle cokes depend on the formation of a liquid crystalline phase (carbonaceous mesophase) during delayed coking. Thermal reactivity of individual compounds in slurry oils effectively controls the initial carbonization reactions, and, thus, the degree of mesophase development. In this study, isotope-ratio-monitoring gas chromatography mass-spectromelry was used in conjunction with a 13C-labeled dopant (4-methyldibenzothiophene) to determine the distribution of the labeled methyl group on the GC-amenable products from carbonization of three different FCCU slurry oils. Selective removal of the unreacted dopant and its methylated analogs from the reaction products by ligand exchange chromatography allowed the isotope analyses of selected aromatic compounds. The 13C enrichment of selected aromatic compounds, including some isomers, was determined to compare the relative thermal reactivities of different compounds as well as the reactivities of different sites on a given aromatic compound.

AB - Delayed coking of Fluid Catalytic Cracking Unit (FCCU) slurry oils produces needle cokes which are used in the manufacture of graphite electrodes for electric-arc furnaces. The structure and properties of needle cokes depend on the formation of a liquid crystalline phase (carbonaceous mesophase) during delayed coking. Thermal reactivity of individual compounds in slurry oils effectively controls the initial carbonization reactions, and, thus, the degree of mesophase development. In this study, isotope-ratio-monitoring gas chromatography mass-spectromelry was used in conjunction with a 13C-labeled dopant (4-methyldibenzothiophene) to determine the distribution of the labeled methyl group on the GC-amenable products from carbonization of three different FCCU slurry oils. Selective removal of the unreacted dopant and its methylated analogs from the reaction products by ligand exchange chromatography allowed the isotope analyses of selected aromatic compounds. The 13C enrichment of selected aromatic compounds, including some isomers, was determined to compare the relative thermal reactivities of different compounds as well as the reactivities of different sites on a given aromatic compound.

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