Integrated, multiple-stage chromatographic method for the separation and identification of polycyclic aromatic hydrocarbons in complex coal liquids

Lucke, R.B.; Later, Douglas W.; Wright, Cherylyn W.; Chess, Edward K.; Weimer, W.C.

doi:10.1021/ac00280a016

Cited by 37 publications

(8 citation statements)

References 32 publications

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“…Therefore, graphs constructed for the u c took account of the concentrations in sediments studied by the analytical protocol, as is illustrated in Figure 2. The expanded uncertainty (U) was calculated affecting the u c by a coverage factor (k) according to the Equation 6. This parameter describes an interval which is expected to include a large fraction of the distribution of values reasonably attributable to the measurand.…”

Section: Uncertainty Estimation From the Validation Datamentioning

confidence: 99%

“…4,5 For the pre-separation or fractionation of crude oil numerous procedures have been reported in the literature. These procedures include high-performance liquid chromatography separation, 6,7 supercritical fluid chromatography separation, 8,9 the classical adsorption chromatography on various adsorbents, including silica gel, 10 alumina, 11 silica-alumina combinations, 12,13 florisil, 14 and solid phase extraction (SPE). 15 This paper focus on the validation of an analytical methodology for the determination of petroleum hydrocarbons in marine sediment samples.…”

Section: Introductionmentioning

confidence: 99%

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Validation of an analytical methodology for the quantitative analysis of petroleum hydrocarbons in marine sediment samples

Damas¹,

Medina²,

Clemente³

et al. 2009

Quím. Nova

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Recebido em 18/2/08; aceito em 20/10/08; publicado na web em 25/3/09This work describes a validation of an analytical procedure for the analysis of petroleum hydrocarbons in marine sediment samples. The proposed protocol is able to measure n-alkanes and polycyclic aromatic hydrocarbons (PAH) in samples at concentrations as low as 30 ng/g, with a precision better than 15% for most of analytes. The extraction efficiency of fortified sediments varied from 65.1 to 105.6% and 59.7 to 97.8%, for n-alkanes and PAH in the ranges: C 16 -C 32 and fluoranthene -benzo(a)pyrene, respectively. The analytical protocol was applied to determine petroleum hydrocarbons in sediments collected from a marine coastal zone.

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Section: Uncertainty Estimation From the Validation Datamentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Validation of an analytical methodology for the quantitative analysis of petroleum hydrocarbons in marine sediment samples

Damas¹,

Medina²,

Clemente³

et al. 2009

Quím. Nova

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“…OF HEAVY PETROLEUM FEEDSTOCKS and coalderived liquids requires the conversion of high-molecular-weight compounds such as dibenzothiophene and the benzonaphthothiophenes (1)(2)(3). Several studies have investigated the mechanism of hydrodesulfurization of polynuclear thiophenes on cobalt or nickel molybdenum catalysts at high pressures (4)(5)(6).…”

Section: Hydrodesulfurizationmentioning

confidence: 99%

Desulfurization of Benzonaphthothiophenes and Dibenzothiophene with a Raney Nickel Catalyst

Nagai

Urimoto

Uetake

et al. 1987

Advances in Chemistry

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Desulfurization of polynuclear thiophenes was performed by contin uous stirring with a Raney nickel catalyst in ethanol at 0-78.8 °C. The major products were biphenyl in the desulfurization of diben zothiophene, α-phenylnaphthalene in the desulfurization of benzo[b]naphtho[1,2-d]thiophene, and β-phenylnaphthalene in the desulfurization of benzo[b]naphtho[2,3-d]thiophene and benzo[b]naphtho[2,1-d]thiophene. Observation of these products shows that the main reaction pathway is the extrusion of a sulfur atom to give the corresponding hydrocarbon. The π-electron densities of the sulfur atoms, which were calculated by using simple Hückel molecular orbital theory, are considered to be related to the adsorption of the sulfur compounds to the surface and consequently to the C-S bond-breaking rate.

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“…The PAH fractions of selected bp range (°F) materials, including SRC-II 800-850 and 850+; EDS 650-700, 700-750, 750-800 and 800+; and ITSL 850+ distillate of the TLP, were further separated by reverse-phase HPLC according to the method of Lucke et al (1985). Standard agar plate mutagenicity assays were performed as described by Ames et al (1975) using Salmonella typhimurium, TA98 microbial tester strain.…”

Section: Cww1-245amentioning

confidence: 99%

“…In general, initiation of mouse skin tumorigenicity by coal liquefaction materials has been associated with their neutral PAH constituency (Mahlum et al, 1983(Mahlum et al, , 1984. Therefore, the neutral PAH isolates of selected distillate cut materials from the EDS (Later et al , 1984), SRC-II (Lucke et al , 1985) and ITSL processes were subfractionated by reverse-phase HPLC. A combined capillary gas chromatogram and low-voltage mass spectrum of the EDS 800*'F+ HPLC Subfraction 2 of the PAH fraction is shown in Figure 10.…”

Section: Data Compiled Inmentioning

confidence: 99%

Fractionally distilled SRC-I, SRC-II, EDS, H-Coal and ITSL direct coal liquefaction process materials: a comparative summary of chemical analysis and biological testing

Wright¹,

Later²,

Dauble³

et al. 1985

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This document reports and compares the results compiled from chemical analyses and biological testing of coal liquefaction process materials which were fractionally distilled, after production, into various comparable boiling-point range cuts. Comparative analyses were performed on solvent refined coal (SRC)-I, SRC-II, H-Coal, EDS and integrated two-stage liquefaction (ITSL) distillate materials. Mutagenicity and carcinogenicity assays were conducted in conjunction with chromatographic and mass spectrometric analyses to provide detailed, comparative, chemical and biological assessments. Where possible, results obtained from the distillate cuts are compared to those from coal liquefaction materials with limited boiling ranges. Work reported here was conducted by investigators in the Biology and Chemistry Department at the Pacific

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Integrated, multiple-stage chromatographic method for the separation and identification of polycyclic aromatic hydrocarbons in complex coal liquids

Cited by 37 publications

References 32 publications

Validation of an analytical methodology for the quantitative analysis of petroleum hydrocarbons in marine sediment samples

Validation of an analytical methodology for the quantitative analysis of petroleum hydrocarbons in marine sediment samples

Desulfurization of Benzonaphthothiophenes and Dibenzothiophene with a Raney Nickel Catalyst

Fractionally distilled SRC-I, SRC-II, EDS, H-Coal and ITSL direct coal liquefaction process materials: a comparative summary of chemical analysis and biological testing

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