Quantitative carbon-13 and proton nuclear magnetic resonance spectroscopy of crude oil and petroleum products. I. Some rules for obtaining a set of reliable structural parameters

Gillet, Stéphane; Rubini, P.; Delpuech, Jean‐Jacques; Escalier, Jean-Claude; Valentin, Patrice

doi:10.1016/0016-2361(81)90183-6

Cited by 112 publications

(51 citation statements)

References 21 publications

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“…In liquid and solid-state NMR, for example, different types of structural entities can be identified and quantified [20]. Therefore, the liquid extracts (HS, HIS-TS and TIS-THFS) were further characterized by 1 H and 13 C NMR to examine the distribution of carbon and hydrogen according to various structural groups found in aliphatic and aromatic moieties [21][22][23][24]. As for the pilot plant-produced sediment sample and its THFIS residue solid-state 13 C NMR was applied.…”

Section: Nmrmentioning

confidence: 99%

Investigation of the mechanism of sediment formation in residual oil hydrocracking process through characterization of sediment deposits

2005

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Section: Nmrmentioning

confidence: 99%

Investigation of the mechanism of sediment formation in residual oil hydrocracking process through characterization of sediment deposits

2005

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“…UV-fluorescence spectra before or after light exposure were not significantly different; similarly, 1 H NMR and 13 C NMR spectra were unchanged. With reference to current knowledge [17,[22][23][24][25][26][27][28][29][30], these negative data suggested that hydrocarbon skeletons underwent little alteration if any during light exposure. Table III presents the relative changes in gravimetric distribution of asphaltenes among the different eluted fractions.…”

Section: Spectral Analysismentioning

confidence: 99%

A fraction to fraction study of photo-oxidation of BAL 150 crude oil asphaltenes

et al. 1998

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IntroductionAmong several intricate physical, physico-chemical, and biological factors, natural light plays an important role [1][2][3][4][5][6] in the mitigation of oil spills at sea or ground surface. Nevertheless, little is known about the contribution of photooxidation to the lengthy degradation of asphaltenes [7][8][9][10][11], the most recalcitrant fraction to weathering processes. Their extremely complex composition probably accounts for this lack of data, by making gradual changes outstandingly difficult to investigate.The chemical nature of asphaltenes is poorly defined. In fact, they correspond to a solubility class of constituents: these precipitated from crude oils by adding at least 40 volumes of normal alkanes (nC 5 to nC 7 ). Asphaltenes contain lamellar macromolecules resulting from the condensation of polyaromatic, naphthenic and heterocyclic nuclei, bearing alkyl side chains and sometimes functionalized. Their molecular weight varies from several hundreds to several thousands [12,13]. Cross linked by alkyl, sulphur and oxygen bridges, the polycyclic sheets constitute a matrix that traps various aliphatic hydrocarbons, and form micelles spread among the other petroleum constituents (hydrocarbons and resins).Addressing chemical changes in such structures is a technical challenge, and hence separating samples into different fractions is an unescapable step before analysis. To investigate the effects of light in asphaltenes isolated from Blend Arabian Light crude oil, samples were fractionated by sequential elution solvent chromatography [14]. This technique, suitable for liquid coals [15][16], and adapted to crude oil asphaltenes [17] was selected, for it separates compounds according to functionalities. Subsequent analyses involved gravimetry, elemental analysis, NMR, UV-fluorescence and chiefly FTIR spectroscopy. Materials and methodsThe effects of light exposure were studied in asphaltenes separated from Blend Arabian Light topped at 150°C (BAL 150). In addition, a number of asphaltenes from several other crude oils (Rospo Mare, Ekofisk, Oman, Handil, Irak, Saoudian (PBS), Kuwait, Shengli, Bach Ho, Zarzaïtine, Blend Arabian Medium and Bunker C) were fractionated and investigated to elucidate some FTIR data. Precipitation of asphaltene fractionsAsphaltenes were precipitated in compliance with the NFT 60-115 AFNOR standard [18]. Crude oil (5 g) was mixed to n-heptane (200 mL) in a 250 mL round bottom flask, heated to reflux (90°C) under agitation during 2.5 hr, and then allowed to settle for 12 hr at room temperature. This solution was filtered on a glass microfiber filter (Whatman GF/A, porosity 0.45 µm). Warm heptane was used to drain out the precipitate coating the flask wall, and to thoroughly rinse the solid collected on the filter. The solid was dissolved with dichloromethane; the solution was then concentrated in a rotary evaporator and dried under nitrogen flow up to complete solvent elimination. In the case of BAL 150 crude oil, this technique yielded an asphaltene fraction of about 3%. ...

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“…The other two parameters used in the present pattern recognition study, IBP and API gravity (=141.5/specific gravity at [11][12][13][14][15][16][17][18][19] "The minus sign means that the two parameters involved are inversely correlated. 'The asterisk indicates that a correlation exists between the two parameters involved (with a 5% probability that such correlation occurs by chance).…”

Section: Other Parametersmentioning

confidence: 99%

Pattern recognition for screening of crude oils using multivariate circular profiles

Lai¹,

Giroux²,

Nai-lin³

et al. 1993

Can. J. Chem.

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. Can. J. Chem. 71, 968 (1993). An appropriate pattern recognition method has been designed to visually discriminate between crude oils belonging to different geographic origins. Each oil is represented by a circular profile that consists of parameter axes that radiate from the centre like spokes on a wheel. One objective of this approach is to provide an optimum set of axes that will best differentiate one circular profile from another. Several parameters were considered for evaluating the oils: photoacoustic spectroscopy (PAS), carbon-13 nuclear magnetic resonance (13c NMR, for %C, = aromatic carbon content), high-performance liquid chromatography (HPLC, for unsaturated, aromatic, and polar compounds), initial boiling point (IBP), American Petroleum Institute (API) gravity, and ultraviolet-visible spectrophotometry (for A, , , = maximum absorption wavelength and E,,,, = maximum molar absorptivity). By computerized statistical evaluation, the selected parameters are PAS and HPLC for unsaturated, aromatic, and polar compounds.EDWARD P.C. LAI, REGI D. GIROUX, NAILIN CHEN et RUNDE GUO. Can. J. Chern. 71,968 (1993). On a mis au point une mCthode approprike de reconnaissance des formes qui permet de distinguer visuellement entre des huiles brutes d'origines diffkrentes. Chaque huile est reprCsentCe par une profil circulaire comportant des parametres axiaux qui s'Ccartent du centre comme les rayons d'une roue. L'objectif de cette approche est de fournir un ensemble optimal de parametres axiaux qui permettra de distinguer un profil circulaire d'un autre. On a considCrC plusieurs parametres pour Cvaluer les huiles : la spectroscopie photoacoustique (SPA), la rCsonance magnetique nuclCaire du carbone-13 (RMN du I3C, pour le %C, = concentration de carbone arornatique), la chrornatographie liquide i haute performance (CLHP, pour les composes insaturks, aromatiques et polaires), le point d'kbullition initial (PEI), la densitk de 1'Institut ArnCricain des PCtroles (API) et la spectrophotomCtrie ultraviolette-visible (pour le A, , , = longueur d'onde d'absorption rnaximale et le E,,,, = absorbance molaire maximale). Sur la base d'une evaluation statistique par ordinateur, les parametres choisis sont la SPA et la CLHP pour les composCs insatures, aromatiques et polaires.[Traduit par la rkdaction]

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Quantitative carbon-13 and proton nuclear magnetic resonance spectroscopy of crude oil and petroleum products. I. Some rules for obtaining a set of reliable structural parameters

Cited by 112 publications

References 21 publications

Investigation of the mechanism of sediment formation in residual oil hydrocracking process through characterization of sediment deposits

Investigation of the mechanism of sediment formation in residual oil hydrocracking process through characterization of sediment deposits

A fraction to fraction study of photo-oxidation of BAL 150 crude oil asphaltenes

Pattern recognition for screening of crude oils using multivariate circular profiles

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