Determination of sulfur and heavy metals in crude oil and petroleum products by energy-dispersive x-ray fluorescence spectrometry and fundamental parameter approach

Christensen, Leif Hoejslet.; Agerbo, Allan.

doi:10.1021/ac00235a016

Cited by 41 publications

(7 citation statements)

References 26 publications

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“…The new method is otherwise similar to the previous BFP approach and features (a) calculation of the effective sample thickness, (b) definition of two "representative light element" masses which approximate the absorption properties of the oxygen, carbon, or other nonobserved light elements, and (c) calculation of matrix corrections for self-absorption and enhancement. It is also similar in some respects to a previously reported method for oil analysis which used scatter intensities in matrix corrections (3).…”

supporting

confidence: 61%

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Multielement analysis of unweighed oil samples by x-ray fluorescence spectrometry with two excitation sources

Sanders¹,

Olsen²,

Weimer³

et al. 1983

Anal. Chem.

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supporting

confidence: 61%

“…Resonance-enhanced two-photon ionization has been applied for the trace determination of aromatic molecules in the gas phase (3)(4)(5). Winefordner and his co-workers have detected aromatic molecules and drugs in a liquid phase with limits of detection as low as 2 µg/L for clonazepam (6,7).…”

Section: Resultsmentioning

confidence: 99%

Multielement analysis of unweighed oil samples by x-ray fluorescence spectrometry with two excitation sources

Sanders¹,

Olsen²,

Weimer³

et al. 1983

Anal. Chem.

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“…The vacuum residue and its isolated maltenes and asphaltenes were subject to elemental analysis (C, H, N, S, V, Ni) as well as 1 H and 13 C NMR to determine the aliphatic and aromatic contents. The toluene soluble and insoluble product fractions obtained from the various runs were characterized by SARA analysis − and X-ray fluorescence spectroscopy, respectively. In this manner, the effects of adding activated carbon to preferentially concentrate asphaltenes and heavy metals and the resulting effects on product quality were discerned.…”

Section: Introductionmentioning

confidence: 99%

Thermal Cracking and Catalytic Hydrocracking of a Colombian Vacuum Residue and Its Maltenes and Asphaltenes Fractions in Toluene

León¹,

Guzmán

Laverde³

et al. 2017

Energy Fuels

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Thermal cracking and catalytic (molybdenum naphthenate) hydrocracking processes in toluene solvent were carried out in a batch reactor for a typical Colombian heavy vacuum residue and its corresponding separated maltenes and asphaltenes fractions. The thermal cracking and catalytic hydrocracking tests were performed at 430 °C and 13.5 MPa for 25 min in the presence of nitrogen and hydrogen, respectively. Additionally, catalytic hydrocracking was also conducted after conditioning the vacuum residue at 380 °C, and 12.2 MPa of H 2 for 60 min with activated carbon. The cracking and catalytic hydrocracking performances of the vacuum residue and its components (maltenes and asphaltenes) were assessed by evaluating the effects on the yield and quality of the products (gas, toluene-insoluble solid, and liquid) utilizing SARA (saturates, aromatics, resins, and asphaltenes) composition and removal of sulfur and heavy (Ni, V) metals analyses. The vacuum residue showed asphaltene conversions of 53.1 and 43.1 wt % (excluding the yield of toluene-insoluble solids) under conditions of thermal cracking and catalytic hydrocracking, respectively. When the vacuum residue was pretreated with activated carbon and then catalytically hydrocracked, the asphaltenes conversion was higher (68.7 wt %, excluding the yield of toluene-insoluble solids) when compared to that during thermal cracking and catalytic hydrocracking in the absence of such pretreatment. Overall, the results showed that the hydrocracking of a vacuum residue in toluene with a molybdenum naphthenate catalyst is effective in forming liquid products that are lighter and with a lower concentration of sulfur and Ni and V heavy metals. These heteroatoms are removed in the toluene-insoluble solid products that concentrate recalcitrant sulfur and nickel complex (i.e., porphyrinic) aromatic compounds to a greater extent. The primary function of the thermally activated carbon pretreatment was to increase the yield of lighter liquid products as a likely result of the conversion of more reactive vanadium-containing complex structures into simpler components that remain in the liquid product and which otherwise would have been rejected in the toluene-insoluble solid fractions.

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“…7 Differentiation between organic (sulfidic and thiophenic) and inorganic sulfur in petroleum samples, as well as quantification of both species, has been performed using X-ray absorption near-edge structure spectroscopy (XANES) and X-ray photoelectron spectroscopy (XPS). 8,9 Structural parameters such as the number of fused rings in the sulfur-containing aromatic systems and the degree of substitution are only partly accessible, and, generally, only bulk parameters are provided. Numerous studies analyzing heavy petroleum fractions with mass spectrometry (MS) and chromatographic methods have been published.…”

mentioning

confidence: 99%

“…Size exclusion chromatography (SEC) was used for molecular-weight analysis (bulk property), in combination with matrix-assisted laser desorption ionization−mass spectrometry (MALDI-MS) . Differentiation between organic (sulfidic and thiophenic) and inorganic sulfur in petroleum samples, as well as quantification of both species, has been performed using X-ray absorption near-edge structure spectroscopy (XANES) and X-ray photoelectron spectroscopy (XPS). , Structural parameters such as the number of fused rings in the sulfur-containing aromatic systems and the degree of substitution are only partly accessible, and, generally, only bulk parameters are provided.…”

mentioning

confidence: 99%

Characterization of High-Molecular-Weight Sulfur-Containing Aromatics in Vacuum Residues Using Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

2005

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Millions of tons of vacuum residues are produced in refineries every year and could be a potentially valuable resource for generating electricity and has possible application as heating and marine fuel. In this work, the polycyclic aromatic sulfur compounds (PASHs) from the aromatic fraction of vacuum residue before and after partial hydrodesulfurization (HDS) were derivatized by methylation to the methylsulfonium salts. Fourier transform ion cyclotron resonance mass spectrometry provided high-resolution data on these high-molecular-weight sulfur compounds. Compounds containing one and two S atoms were found to dominate, with masses up to ca. 900 Da. Classification according to hydrogen deficiency and the number of heteroatoms showed extensive series of homologues for double bond equivalents from 5 to 20. The sulfur-containing aromatics were separated using a palladium(II) complex as a liquid chromatographic phase into two compound groups: one containing compounds with an unconjugated thiophene ring and another with a condensed thiophene ring. This, combined with the mass spectrometry (MS) data, allows for the identification of several parent structures. Partial HDS removed primarily compounds with one S atom, whereas those with two S atoms were largely unaffected.

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Determination of sulfur and heavy metals in crude oil and petroleum products by energy-dispersive x-ray fluorescence spectrometry and fundamental parameter approach

Cited by 41 publications

References 26 publications

Multielement analysis of unweighed oil samples by x-ray fluorescence spectrometry with two excitation sources

Multielement analysis of unweighed oil samples by x-ray fluorescence spectrometry with two excitation sources

Thermal Cracking and Catalytic Hydrocracking of a Colombian Vacuum Residue and Its Maltenes and Asphaltenes Fractions in Toluene

Characterization of High-Molecular-Weight Sulfur-Containing Aromatics in Vacuum Residues Using Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

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