共查询到20条相似文献,搜索用时 31 毫秒
1.
Seeley SK Bandurski SV Brown RG McCurry JD Seeley JV 《Journal of chromatographic science》2007,45(10):657-663
A flow-switching two-dimensional gas chromatography (GCxGC) apparatus has been constructed that can operate at temperatures as high as 340 degrees C. This system is employed to analyze complex hydrocarbon mixtures such as diesel fuel, gas-oil, motor oil, and petroleum contaminated environmental samples. The GCxGC system generates two-dimensional chromatograms with minimal overlap between the aliphatic and aromatic regions This allows these compound classes to be independently quantitated without prior fractionation. The GCxGC system is used to analyze extracts of spiked water samples, wastewater, and soil. The accuracy of the method is compared to that of the Massachusetts Extractable Petroleum Hydrocarbons (MA EPH) method. The GCxGC system generates a quantitative accuracy similar to the MA EPH method for the analysis of spiked water samples. The GCxGC method and the MA EPH method generate comparable levels of total hydrocarbons when wastewater is analyzed, but the GCxGC method detects a significantly higher aromatic content and lower aliphatic content. Both the GCxGC method and MA EPH method measure comparable levels of aromatics in the soil samples. 相似文献
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Jan Blomberg Peter J. Schoenmakers Jan Beens Robert Tijssen 《Journal of separation science》1997,20(10):539-544
In general, petrochemical products contain only a limited number of chemical classes of compounds (sample dimensionality). The enormous number of individual components within these classes, however, soon puts limitations upon a single chromatographic technique when it comes to adequate characterization of these products. Comprehensive two-dimensional gas chromatography (GC×GC) clearly opens the possibility of estimating the composition of hydrocarbon mixtures in a far more detailed fashion than hitherto possible. Although the emphasis of papers of GCxGC thus far almost exclusively applies to the unsurpassed peak-capacity, in the oil industry there is a need for characterization, rather than for analyzing all the individual compounds. In principle a GCxGC system can provide an almost perfect match between its intrinsic properties and the dimensionality of oil samples. To establish the applicability of GCxGC towards petrochemical analytical challenges, a commercially aavailable prototype instrument was subjected to an exhaustive characterization of a typical hydrocarbon precess stream and a fast characterization of a light gas oil. Although there are no fundamental limitations towards the quantitative aspects of a GCxGC system, this paper confines itself to qualitative results only. Quantitative aspects of GCxGC will be published in a forthcoming paper. 相似文献
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Adam F Bertoncini F Thiébaut D Esnault S Espinat D Hennion MC 《Journal of chromatographic science》2007,45(10):643-649
The detailed characterization of middle distillates is essential for a better understanding of reactions involved in refining processes. Owing to a higher resolution power and an enhanced sensitivity, but especially to a group-type ordering in the chromatographic plane, comprehensive two-dimensional gas chromatography (GCxGC) offers unsurpassed characterization possibilities for petroleum samples. However, GCxGC fails to totally discriminate naphthenes from unsaturates occurring in hydrotreated diesel samples. This article aims at promoting the implementation of LC-GCxGC for the quantitative determination of hydrocarbon distribution in middle distillates, including naphthenes. In this configuration, liquid chromatography (LC) enables the separation of hydrocarbons into two fractions (viz., saturated and unsaturated) before the subsequent analysis of each fraction by GCxGC. In this paper, the choice of GCxGC conditions in order to achieve the separation and identification of hydrocarbons by chemical class is discussed; under these conditions, naphthenes are separated according to the number of saturated rings. For the first time, the presence of di-, tri-, and tetra-naphthenes resulting from the hydroconversion of aromatics can clearly be evidenced. A quantitative procedure for the determination of the distribution of hydrocarbons, including the distribution of naphthenes according to the number of saturated rings, is also proposed and discussed in detail. LC-GCxGC is found to provide an unequalled degree of information that will widely contribute to a better understanding of hydroconversion processes. 相似文献
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Mao D Lookman R Van De Weghe H Vanermen G De Brucker N Diels L 《Journal of chromatography. A》2009,1216(14):2873-2880
An assessment of aqueous solubility (leaching potential) of soil contaminations with petroleum hydrocarbons (TPH) is important in the context of the evaluation of (migration) risks and soil/groundwater remediation. Field measurements using monitoring wells often overestimate real TPH concentrations in case of presence of pure oil in the screened interval of the well. This paper presents a method to calculate TPH equilibrium concentrations in groundwater using soil analysis by high-performance liquid chromatography followed by comprehensive two-dimensional gas chromatography (HPLC-GCXGC). The oil in the soil sample is divided into 79 defined hydrocarbon fractions on two GCXGC color plots. To each of these fractions a representative water solubility is assigned. Overall equilibrium water solubility of the non-aqueous phase liquid (NAPL) present in the sample and the water phase's chemical composition (in terms of the 79 fractions defined) are then calculated using Raoult's law. The calculation method was validated using soil spiked with 13 different TPH mixtures and 1 field-contaminated soil. Measured water solubilities using a column recirculation equilibration experiment agreed well to calculated equilibrium concentrations and water phase TPH composition. 相似文献
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A. Liberti P. Ciccioli A. Cecinato E. Brancaleoni C. Di Palo 《Journal of separation science》1984,7(7):389-397
An analytical procedure is described for the fractionation of organic compounds present in environmental samples and the determination of nitro polyaromatic hydrocarbons (nitro-PAHs). Both low and high resolution liquid chromatography are employed for the prefractionation of the soluble organic fraction (SOF) extracted from particulate matter or gaseous pollutants collected on adsorption traps. High resolution gas chromatography is used to analyze four fractions containing alkanes, PAHs, nitro-PAHs, and other polar PAHs. Nitrogen-containing species are separated by GC and detected specifically using an alkali flame (NPD) detector. Flame ionization (FID) detection, GC-MS of positive ions, and negative ion chemical ionization MS of the whole fraction is used for the identification and quantitation of the various components. The composition of SOF extracted from particulate matter emitted from diesel exhausts is elucidated and a large number of nitro-PAHs identified by the combination of the various techniques. 相似文献
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The use of gas chromatography (GC)-mass spectrometry (MS), GC-time-of-flight MS (TOFMS), comprehensive two-dimensional GC (GCxGC)-flame ionization detection (FID), and GCxGC-TOFMS is discussed for the characterization of the eight important representative components, including Z-alpha-santalol, epi-alpha-bisabolol, Z-alpha-trans-bergamotol, epi-beta-santalol, Z-beta-santalol, E,E-farnesol, Z-nuciferol, and Z-lanceol, in the oil of west Australian sandalwood (Santalum spicatum). Single-column GC-MS lacks the resolving power to separate all of the listed components as pure peaks and allow precise analytical measurement of individual component abundances. With enhanced peak resolution capabilities in GCxGC, these components are sufficiently well resolved to be quantitated using flame ionization detection, following initial characterization of components by using GCxGC-TOFMS. 相似文献
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The present investigation was aimed at identifying the compound(s) responsible for the carcinogenic activity of a variety of jute batching oil (known as non-FDA variety, pre-FDA variety, or JBO-P), a crude petroleum distillate substantially used in jute industries. This was initially performed by isolating from JBO-P a polyaromatic hydrocarbon (PAH) fraction containing compounds of more than three rings. This fraction was then analysed for its PAH profile by gas chromatography and individual components identified by comparing its flame ionisation detector (FID) signal with those obtained from reference PAHs. The results revealed that PAHs of more than three rings, reported to be a recognised class of chemical carcinogens, were present in the JBO-P sample at the level of 3300 mg/kg of oil (0.33%, w/w); benzo(a)pyrene and dibenz(a,h)anthracene, known to be highly potent carcinogens, constituted 129 mg/kg (0.0129%, w/w) and 29 mg/kg (0.0029%, w/w) of the total oil, respectively; and except for a few signals, the PAH profile of JBO-P was found to be somewhat similar to that reported for a sample of carcinogenic used engine oil. 相似文献
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Qian K Diehl JW Dechert GJ DiSanzo FP 《European journal of mass spectrometry (Chichester, England)》2004,10(2):187-196
We report the first coupling of supercritical fluid chromatography (SFC) with field ionization time-of-flight high-resolution mass spectrometry (FI-ToF HRMS), in parallel with ultraviolet (UV) detection and flame ionization detection (FID), for rapid and quantitative analysis of petroleum middle distillates. SFC separates petroleum middle distillates into saturates and 1- to 3-ring aromatics. FI generates molecular ions for hydrocarbon species eluted from the SFC. The high resolution and exact mass measurements by ToF mass spectrometry provide elemental compositions of the molecules in the petroleum product. The amounts of saturates and aromatic ring types were quantified using the parallel SFC-FID assisted by SFC-UV. With a proper carbon-number calibration, the detailed composition of the petroleum middle distillate was rapidly determined. 相似文献
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Debin Mao Richard Lookman Hendrik Van De Weghe Dirk Van Look Guido Vanermen Nicole De Brucker Ludo Diels 《Journal of chromatography. A》2009,1216(9):1524-1527
Enhanced bioremediation of petroleum hydrocarbons in two biopiles was quantified by high-performance liquid chromatography (HPLC) followed by comprehensive two-dimensional gas chromatography (GCXGC). The attenuation of 34 defined hydrocarbon classes was calculated by HPLC–GCXGC analysis of representative biopile samples at start-up and after 18 weeks of biopile operation. In general, a-cyclic alkanes were most efficiently removed from the biopiles, followed by monoaromatic hydrocarbons. Cycloalkanes and polycyclic aromatic hydrocarbons (PAHs) were more resistant to degradation. A-cyclic biomarkers farnesane, trimethyl-C13, norpristane, pristane and phytane dropped to only about 10% of their initial concentrations. On the other hand, C29–C31 hopane concentrations remained almost unaltered after 18 weeks of biopile operation, confirming their resistance to biodegradation. They are thus reliable indicators to estimate attenuation potential of petroleum hydrocarbons in biopile processed soils. 相似文献
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测定了不同来源的渣油、不同改性工艺沥青的薄层色谱图,提取了谱图特征变量,以偏最小二乘方法为数学工具,通过经典柱色谱法取得基础数据,建立渣油沥青的薄层色谱(TLC)-族组成模型。采用该模型预测待测样品的族组成,并与经典柱色谱法的测定结果相比,饱和烃质量分数、芳烃质量分数和胶质质量分数的相关系数分别为0.9765,0.9901和0.9937。测定结果与经典柱色谱法的测定结果相一致。 相似文献
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Comprehensive two-dimensional gas chromatography (GCxGC) is used to analyze petroleum diesel, biodiesel, and biodiesel/petroleum diesel blends. The GCxGC instrument is assembled from a conventional gas chromatograph fitted with a simple, in-line fluidic modulator. A 5% phenyl polydimethylsiloxane primary column is coupled to a polyethylene glycol secondary column. This column combination generates chromatograms where the fatty acid methyl esters (FAMEs) found in biodiesel occupy a region that is also populated by numerous cyclic alkanes and monoaromatics found in petroleum. Fortunately, the intensities of the petroleum hydrocarbon peaks are far lower than the intensities of the FAME peaks, even for blends with low biodiesel content. This allows the FAMEs to be accurately quantitated by direct integration. The method is calibrated by analyzing standard mixtures of soybean biodiesel in petroleum diesel with concentrations ranging from 1 to 20% v/v. The resulting calibration curve displays excellent linearity. This curve is used to determine the concentration of a B20 biodiesel/petroleum diesel blend obtained from a local retailer. Excellent precision and accuracy are obtained. 相似文献
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Sun K Winniford W Griffith J Colura K Green S Pursch M Luong J 《Journal of chromatographic science》2003,41(10):506-518
Fast screening of wash oils is demonstrated using comprehensive two-dimensional gas chromatography (GCxGC). Wash oils are used in ethylene production plants to minimize compressor fouling. The composition of a wash oil determines its effectiveness in solubilizing heavy hydrocarbons. In particular, the relative amount of 1- and 2-ring aromatics is important. The presence of oxygenates is undesirable because of adverse effects to the process. It is shown that GCxGC is well suited for this application. Species in wash oils are separated and grouped into three bands: a nonpolar aliphatics band, 1- and 2-ring aromatics band, and polyaromatics band. For a given polar secondary column, the spacing between bands in the second dimension can be adjusted in a broad range by selecting a primary column and an oven-temperature-programming rate. Integration of GCxGC peaks is evaluated using a standard GC integration program and a new GCxGC integration program. Consistent results are obtained using both programs for well-separated GCxGC peaks with relative differences for individual peak ranging from 0.04% to 1.6%. Peak responses are integrated by the GCxGC software, and the relative amounts of aromatics content and aliphatics content are estimated by peak response percent with relative standard deviations ranging from 0.15% to 2.8% (n = 3). 相似文献
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Summary The representative refined mineral oil samples, crude petroleum straightrun distillates, potentially used in the manufacture of crop protection products were analysed by isocratic and gradient high performance liquid chromatography (HPLC) to investigate their trace polycyclic aromatic hydrocarbon (PAH) content. Liquid-liquid extraction followed by size-exclusion column chromatography was employed to isolate the fraction containing PAHs with more than two fused rings. The identity of individual PAHs was confirmed by comparing their UV and fluorimetric detector signals with those recorded from reference standards. The level of extracted PAHs in the oil samples are discussed with respect to their physical and chemical properties. 相似文献
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Freitas LS Von Mühlen C Bortoluzzi JH Zini CA Fortuny M Dariva C Coutinho RC Santos AF Caramão EB 《Journal of chromatography. A》2009,1216(14):2860-2865
In this work the higher peak capacity and resolution of comprehensive two-dimensional gas chromatography (GCxGC) has been successfully applied, for the first time, to tentatively identify several polar organic compounds of organic extracts of aqueous phases resulting from microwave demulsification process of water-in-crude oil emulsions. Results have shown that higher temperatures and longer exposure time to microwave irradiation produced water phases with a wider variety of polar organic compounds. The microwave process showed to be suitable for the extraction of several polar compounds classes of petroleum. The proposed microwave extraction method and GCxGC identification of polar compounds of petroleum samples are of practical interest for the petrochemical industry due to corrosion and related problems associated with these polar compounds in refinery equipments. The GCxGC/time-of-flight MS technique shows to be very important in the total separation of different classes of compounds and allows the identification of many compounds in these classes. 相似文献
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The most commonly used military fog oil is characterized by comprehensive two-dimensional gas chromatography (GC×GC) coupled to either Flame Ionization Detection (FID) or Time-of-Flight Mass Spectrometric Detection (TOFMS) to advance the knowledge regarding the complete chemical makeup of this complex matrix. Two different GC×GC column sets were investigated, one employing a non-polar column combined with a shape selective column and the other an inverse column set (medium-polar/non-polar). The inverse set maximizes the use of the two-dimensional separation space and segregates aliphatic from aromatic fractions. The shape selective column best separates individual polycyclic aromatic hydrocarbons (PAHs) from the bulk oil. The results reveal that fog oil (FO) is composed mainly of aliphatic compounds ranging from C10 to C30, where naphthenes comprise the major fraction. Although many different species of aromatics are present, they constitute only a minor fraction in this oil, and no conjugated PAHs are found. The composition of chemically similar aliphatic constituents limits the analytical power of silica gel fractionation and GC–MS analysis to characterize FO. Among the aliphatic compounds identified are alkanes, cyclohexanes, hexahydroindanes, decalins, adamantanes, and bicyclohexane. The aromatic fraction is composed of alkylbenzene compounds, indanes, tetrahydronaphthalenes, partially hydrogenated PAHs, biphenyls, dibenzofurans and dibenzothiophenes. This work represents the best characterization of military fog oil to date. As the characterization process shows, information on such complex samples can only be parsed using a combination of sample preprocessing steps, multiple detection schemes, and an intelligent selection of column chemistries. 相似文献
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Summary Diaromatics are geochemically significant constituents of crude oils. Their determination is usually achieved by elaborate prefractionation methods, such as medium pressure liquid chromatography and HPLC, prior to capillary gas chromatography. The present contribution describes the quantitative analysis of methylnaphthalenes, ethylnaphthalenes, and dimethylnaphthalenes in selected crude oils by two-dimensional capillary GC. Since the method does not comprise any work-up procedure the determination of geochemical parameters (alkylnaphthalene concentration ratios) is performed on the original, untreated crude oil samples. Accordingly, the analytical results reflect the original composition. The influence by evaporational losses in the laboratory is minimized. 相似文献
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Schoenmaker PJ Oomen JL Blomberg J Genuit W van Velzen G 《Journal of chromatography. A》2000,892(1-2):29-46
In this paper, we compare the current separation power of comprehensive two-dimensional gas chromatography (GCxGC) with the potential separation power of GC-mass spectrometry (GC-MS) systems. Using simulated data, we may envisage a GC-MS contour plot, that can be compared with a GCxGC chromatogram. Real examples are used to demonstrate the current potential of the two techniques in the field of hydrocarbon analysis. As a separation technique for complex hydrocarbon mixtures, GCxGC is currently about as powerful as GC-MS is potentially powerful. GC-MS has not reached its potential separation power in this area, because a universal, soft ionization method does not exist. The greatest advantage of GCxGC is, however, its potential for quantitative analysis. Because flame-ionisation detection can be used, quantitative analysis by GCxGC is much more robust, reliable and reproducible. 相似文献
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Accurate quantitative analysis for selected polycyclic aromatic hydrocarbons present on urban dust can be obtained by using a simple procedure consisting of sonic-probe extraction with cyclohexane; clean-up with Florisil((R))-XAD-4((R)), and measurement by high-resolution gas chromatography with flame-ionization detection (HRGC/FID). The analysis can be further simplified by eliminating the clean-up step if HRGC/electron-impact mass-spectrometry (MS) is available. Both the FID and MS methods give results consistent with those obtained by standard procedures. The direct HRGC/MS procedure, combined with chemical ionization, can also be applied to the determination of polycyclic organic materials present in solvent-refined coal, shale oil and crude oil. 相似文献