High performance liquid chromatographic separation of polycyclic aromatic hydrocarbons on microparticulate pyrrolidone and application to the analysis of shale oil

Mourey, Thomas H.; Siggia, Sidney.; Uden, P. C.; Crowley, R. J.

doi:10.1021/ac50056a026

Cited by 34 publications

(3 citation statements)

References 36 publications

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“…Comparison of these standards with the oil samples revealed that the shale aromatic fractions were composed mainly of 1-4 ring systems. The finding corroborated that previously noted by Mourey et al (15). Four major citrus limonoids are separated in less than 15 min on a nitrile (CN) column in the normal phase mode using a ternary solvent system.…”

Section: Resultssupporting

confidence: 91%

“…The solvent system was chloroform-acetonitrile (95:5 v/v). However, because of the low sensitivity and the poor thermal stability of the refractive index detector, the method was abandoned in favor of a reverse phase system employing a water-methanol solvent system with chemically bonded nitrile (CN) column packing material and a variable wavelength UV detector set at 210 nm (15). There were several disadvantages with this procedure that made it unsuitable for…”

Section: Resultsmentioning

confidence: 99%

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Class separation and characterization of shale oil by liquid chromatography and capillary column gas chromatography

Crowley¹,

Siggia²,

Uden³

1980

Anal. Chem.

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Section: Resultssupporting

confidence: 91%

Section: Resultsmentioning

confidence: 99%

Class separation and characterization of shale oil by liquid chromatography and capillary column gas chromatography

Crowley¹,

Siggia²,

Uden³

1980

Anal. Chem.

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“…NMP, a dipolar aprotic solvent with a moderately high dielectric constant of 4.09D, seems to be an effective solvent to cleave some noncovalent bonds due to the strong interaction with polar sites in coals such as hydroxyl groups. Moreover, NMP has a good affinity for aromatic rings. , So, NMP can dissolve much more coal molecules and radicals than other good organic solvents for coal, for example, pyridine. Moreover, at 175−300 °C NMP dissolves them much more than at room temperature, and the resulting separation of the radicals from coal networks prevents retrogressive reactions such as radical additions to aromatic rings of coal networks, which would occur in a poor solvent.…”

Section: Resultsmentioning

confidence: 99%

Coal Dissolution by Heat Treatments in N-Methyl-2-pyrrolidinone, 1,4,5,8,9,10-Hexahydroanthracene, and Their Mixed Solvents: A Large Synergistic Effect of the Mixed Solvents

Ashida

Iino

et al. 1999

Energy Fuels

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Heat treatments of coals of various ranks were carried out in a dipolar aprotic solvent of N-methyl-2-pyrrolidinone (NMP) and a strong hydrogen-donating solvent of 1,4,5,8,9,10hexahydroanthracene (HHA) at 175-300 °C under N 2 atmosphere. Dissolution yields were obtained using carbon disulfide/N-methyl-2-pyrrolidinone (CS 2 /NMP) mixed solvent (1:1 by volume) as an extraction solvent for the heat-treated coals. Considerable high dissolution yields were obtained for several coals even at temperatures as low as 175-300 °C. For the lower rank coals (C wt %, daf < 85 wt %) used, the dissolution yields in NMP and HHA increased with increasing temperature from 175 °C to 300 °C. The dissolution yields (38.2-78.1 wt %, daf) obtained in NMP were higher than those obtained in HHA. While, for Upper Freeport coal of higher rank (C% > 85 wt %, daf), a very high dissolution yield of 82.5 wt % was obtained in NMP at 175 °C, but it did not increase with increasing temperature to 300 °C and was lower than that in HHA. Similar results were observed for the other higher rank coal. NMP/HHA mixed solvents were found to show a large synergistic effect on the dissolution yields for all the coals used. An amount of 96.4 wt % of Banko coal was dissolved after the heat treatment in NMP/HHA mixed solvent (9/1 by weight) at 300 °C, which is much higher than 59.1 wt % in NMP and 44.5 wt % in HHA alone. It is also found that the extent of such synergistic effects is highly coal-rankdependent. The mechanisms for the dissolution reaction in NMP, HHA, and NMP/HHA mixed solvents were discussed.

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Oil Shale and Shale Oil Analysis

Miknis

Netzel

2000

Encyclopedia of Analytical Chemistry

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An oil shale can be defined as a compact rock of sedimentary origin with an ash content of more than 33% and containing organic matter that yields oil when destructively distilled, but not appreciably when extracted with ordinary solvents. This is an operational definition. There is no geological or chemical definition of an oil shale. The term is used mostly in an economic sense so that any shallow rock that yields a commercial amount of oil upon pyrolysis may be considered an oil shale. Oil shale deposits occur in at least 50 countries and the estimated potential world supply of oil from shale is 5 × 10 12 barrels. The organic matter in an oil shale is mostly in the form of kerogen, which is defined as that fraction of the organic matter in a sedimentary rock that is insoluble in common petroleum solvents. The insolubility of kerogen is the main reason why an oil shale must be heated to produce liquid products. The amount of shale oil that can be produced by heating an oil shale is normally obtained from a Fischer assay. However, the Fischer assay is somewhat time‐consuming and does not provide information about what chemical properties of oil shales are important for producing liquids. Consequently, a number of alternative procedures have been developed to analyze oil shales. These procedures, along with methods of analyzing shale oils, are described in the following sections.

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High performance liquid chromatographic separation of polycyclic aromatic hydrocarbons on microparticulate pyrrolidone and application to the analysis of shale oil

Abstract: A chemically bonded pyrrolidone substrate is used for the high performance liquid chromatographic separation of polycyclic aromatic hydrocarbons. The cyclic amide phase interacts electronically with the polycyclic aromatic hydrocarbons in

Cited by 34 publications

References 36 publications

Class separation and characterization of shale oil by liquid chromatography and capillary column gas chromatography

Class separation and characterization of shale oil by liquid chromatography and capillary column gas chromatography

Coal Dissolution by Heat Treatments in N-Methyl-2-pyrrolidinone, 1,4,5,8,9,10-Hexahydroanthracene, and Their Mixed Solvents: A Large Synergistic Effect of the Mixed Solvents

Oil Shale and Shale Oil Analysis

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