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PubMed2006

Forensic fingerprinting of diamondoids for correlation and differentiation of spilled oil and petroleum products.

Diamondoids (adamantanes and diamantanes) are rigid, three-dimensionallyfused cyclohexyl-ring alkane compounds that can be found in almost all crude oils and in most petroleum products. Forforensic environmental investigations, the most commonly used biomarkers are high molecular weight (MW) tri- to pentacyclic terpanes and steranes. Most of these high MW biomarkers, however, are removed from the original crude oil feedstocks during the refining processes, while smaller biomarkers including diamondoids are concentrated in petroleum products. Fingerprinting diamondoids could thus provide another diagnostic means for correlation and differentiation of spilled oils and be particularly valuable for light to midrange distillates, such as jet and diesel fuels, the source of which may be difficult to identify using routine biomarker techniques. In this work, a reliable GC-MS analytical method has been developed for characterization and quantitation of diamondoids. The method detection limits for five target diamondoids were determined to be in the range of 0.06-0.14 microg/g oil. Distributions of diamondoids in over 100 different oils and refined products were quantitatively compared. The concentrations of four groups of target biomarkers were found, in general, to decrease in the order of sesquiterpanes > terpanes and steranes > adamantanes > diamantanes in both crude oils and refined products. A number of indices of admantanes and diamantanes have been developed and assessed as source indicators using their diagnostic powers (DP). The effects of evaporative weathering and biodegradation on alteration of diamondoid distributions have been quantitatively investigated. Finally, a spill case study by statistical evaluation of diagnostic ratios using the "two-tailed" Student's tapproach is presented to illustrate the unique utility of diamondoids for correlation and differentiation of unknown spilled diesels.

Adamantane↗
PubMed2005

Characterization, weathering, and application of sesquiterpanes to source identification of spilled lighter petroleum products.

Biomarkers have become increasingly important for identifying the source of spilled oil, due to their specificity and high resistance to biodegradation. The biomarkers most commonly used in forensic investigations are the high molecular weight (MW) tri- and pentacyclic terpanes and steranes. For lighter petroleum products such as jet fuels and diesels, the refining processes remove most high MW biomarkers from the original crude oil feedstock. The smaller bicyclic sesquiterpanes, however, are concentrated in these products. Sesquiterpanes are ubiquitous components of crude oils and ancient sediments. Examination of GC-MS chromatograms of these bicyclic biomarkers using their characteristic fragment ions (m/z 123, 179, 193, and 207) provides a highly diagnostic means for identifying spilled oil, particularly for lighter refined product samples that are difficult to identify by current techniques. In this work, sesquiterpanes in crude oils and petroleum products are identified and characterized, distributions of sesquiterpanes in oils and refined products are compared, the effects of evaporative weathering on sesquiterpane distributions are examined, and a methodology using diagnostic indices of sesquiterpanes is developed for oil correlation and differentiation. Finally, two case studies are presented to illustrate the unique utility of sesquiterpanes for fingerprinting and identifying unknown diesel spills.

Chromatography, Gas↗
PubMed2003

Application of laser-based ion mobility (IM) spectrometry for the analysis of polycyclic aromatic compounds (PAC) and petroleum products in soils.

The capability of laser-based IM spectrometry to detect PAC and petroleum products (oils) in model matrices, laboratory reference (LR) materials and in real-world contaminated soil samples was demonstrated. Quantitative IM investigations of PAC-doped PVC films yielded detection limits in the ppm range for single PAC. The potential of IM spectrometry for in situ analysis was demonstrated by the analysis of PAC-containing certified reference (CR) material, and of petroleum product-containing LR materials and real-world soil samples. The calibration of IM signals obtained from oil-doped LR materials was also possible, and detection of oils with concentrations below 100 mg kg(-1) was achieved. The in situ analysis of real-world contaminated soils with the IM and LIF techniques was in good accordance with ex situ reference investigations.

Lasers↗
PubMedDate not supplied

[Effect of photosynthetic bacteria and compost on degradation of petroleum products in soil].

Addition of diesel fuel and waste engine oil to soil was found to cause biostimulation of hydrocarbon-oxidizing microorganisms. Corynebacteria constitute a large group of hydrocarbon-oxidizing microorganisms. Addition of a liquid culture of photosynthetic bacteria to soil not only facilitates degradation of petroleum products, but also stimulates growth of hydrocarbon-oxidizing microorganisms. Combined addition of photosynthetic bacteria and compost to soil polluted with petroleum products causes even a more significant increase in the count of hydrocarbon-oxidizing bacteria and substantially increases the rate of pollutant degradation.

Biodegradation, Environmental↗
PubMed2005

Isotope dilution ICP-MS with laser-assisted sample introduction for direct determination of sulfur in petroleum products.

Inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with direct laser-assisted introduction of isotope-diluted samples into the plasma, using a laser ablation system with high ablation rates, was developed for accurate sulfur determinations in different petroleum products such as 'sulfur-free' premium gasoline, diesel fuel, and heating oil. Two certified gas oil reference materials were analyzed for method validation. Two different 34S-enriched spike compounds, namely, elementary sulfur dissolved in xylene and dibenzothiophene in hexane, were synthesized and tested for their usefulness in this isotope dilution technique. The isotope-diluted sample was adsorbed on a filter-paper-like material, which was fixed in a special holder for irradiation by the laser beam. Under these conditions no time-dependent spike/analyte fractionation was only observed for the dibenzothiophene spike during the laser ablation process, which means that the measured 34S/32S isotope ratio of the isotope-diluted sample remained constant-a necessary precondition for accurate results with the isotope dilution technique. A comparison of LA-ICP-IDMS results with the certified values of the gas oil reference materials and with results obtained from ICP-IDMS analyses with wet sample digestion demonstrated the accuracy of the new LA-ICP-IDMS method in the concentration range of 9.2 microg g(-1) ('sulfur-free' premium gasoline) to 10.4 mg g(-1) (gas oil reference material BCR 107). The detection limit for sulfur by LA-ICP-IDMS is 0.04 microg g(-1) and the analysis time is only about 10 min, which therefore also qualifies this method for accurate determinations of low sulfur contents in petroleum products on a routine level.

Lasers↗
PubMed2001

Forensic analysis of commercial petroleum products using selective fluorescence quenching.

A novel method for the forensic analysis of commercial petroleum products is presented. In this approach, the petroleum sample is extracted with nitromethane and then separated by capillary liquid chromatography with laser-induced fluorescence detection. The addition of selective fluorescence quenching agents allows the sample to be profiled by the distribution of alternant and nonalternant polycyclic aromatic hydrocarbons (PAHs). In preliminary studies, the quenching behavior of nitromethane and diisopropylamine was established by using a standard mixture of sixteen PAHs ranging in size from two to six aromatic rings. Subsequent examination of new and used motor oil demonstrated that characteristic differences arise in the PAH content, which may allow for the unique identification of oil from a particular engine or vehicle. In addition, three brands of petrolatum jelly were successfully distinguished. Although a number of alternant alkylated and heterocyclic PAHs were found in all petrolatum samples, there were significant differences in the relative concentrations of alternant as well as nonalternant PAHs. This allowed for clear differentiation of the samples through qualitative inspection of their chromatograms as well as quantitative statistical correlation techniques.

Journal Article↗
PubMed2002

Studies on the effect of inoculation of activated sludge with bacteria actively degrading hydrocarbons on the biodegradation of petroleum products.

Eighteen strains of bacteria were isolated from activated sludge purifying petroleum-refining wastewaters. These strains were plated on solidified mineral medium supplemented with oil fraction in concentration 1000 mg/l. Four of the strains that grew best in the presence of oil were selected for further studies. The strains were identified based on Bonde's scheme and microscopic observations. Three of them belonged to the genus Arthrobacter and one to the genus Micrococcus. Stationary cultures of single strains and their mixtures were set up in mineral medium containing oil (sterile and non-sterile) as sole carbon source in concentration 1000 mg/l. The oils were found to be removed the most efficiently by a mixture of the strains. After 14 days of culture the amount of oil was utilized by from 63 to 95%. In the next stage of the studies the bacteria were used to inoculate activated sludge. Stationary cultures of the activated sludge were set up in mineral medium with oil. The utilisation of petroleum products by non-inoculated activated sludge (control), activated sludge inoculated with a single strain or a mixture of all four strains was examined. In both inoculated activated sludge cultures approximately 80% of the oils were removed, compared to 60% in the control activated sludge. Therefore, inoculated activated sludge showed 20% higher effectiveness of removal of petroleum derivatives.

Arthrobacter↗
PubMed2006

Remediation of saturated soil contaminated with petroleum products using air sparging with thermal enhancement.

Pollutants in the form of non-aqueous phase liquids (NAPLs), such as petroleum products, pose a serious threat to the soil and groundwater. A mathematical model was derived to study the unsteady pollutant concentrations through water saturated contaminated soil under air sparging conditions for different NAPLs and soil properties. The comparison between the numerical model results and the published experimental results showed acceptable agreement. Furthermore, an experimental study was conducted to remove NAPLs from the contaminated soil using the sparging air technique, considering the sparging air velocity, air temperature, soil grain size and different contaminant properties. This study showed that sparging air at ambient temperature through the contaminated soil can remove NAPLs, however, employing hot air sparging can provide higher contaminant removal efficiency, by about 9%. An empirical correlation for the volatilization mass transfer coefficient was developed from the experimental results. The dimensionless numbers used were Sherwood number (Sh), Peclet number (Pe), Schmidt number (Sc) and several physical-chemical properties of VOCs and porous media. Finally, the estimated volatilization mass transfer coefficient was used for calculation of the influence of heated sparging air on the spreading of the NAPL plume through the contaminated soil.

Air↗
PubMed1978

[Health conditions of workers chronically exposed to ethyl gasoline and other petroleum products].

Results of 5-year periodic examinations and SDH, LAP and GGTP activity in blood serum of 207 workers chronically exposed to ethyl gasoline and other petroleum products were analysed. In addition, in the selected groups, the levels of IgA, IgG and IgM immunoglobulins, complement C3 fraction and alpha2 macroglobulins were determined. Results of objective and enzymatic examinations indicate a slight toxic liver lesion. No significant changes in albuminous fractions were found, except a significant reduction in alpha2 macroglobulins.

Female↗
PubMed2004

[Distribution of sulfur-containing compounds in the gasoline range petroleum products].

A capillary gas chromatography coupled with sulfur chemiluminescence detection (GC-SCD) method has been developed for detailed analysis and group-type characterization of sulfur compounds in gasoline range petroleum products. Chemical treatment of the samples was carried out using selective reactions for group-type classification of compounds. A total of 107 sulfur compounds were tentatively classified and identified based on standard substances and retention rule. The relative standard deviations (RSDs) of retention times were no more than 0.25%. The quantitative analysis on major sulfur compounds and total sulfur was carried out based on the linear response of sulfur chemiluminescence detector and the internal standard method. The recoveries were in the range of 96% - 115%. For the sulfur-containing compounds whose concentration exceeded 7 mg/kg, the RSDs of the determination were less than 8.9%. Various types of gasoline were analyzed and their sulfur distributions were investigated using the developed method. The results show that the method can be used to separate, identify and quantitate sulfur-containing compounds.

Chromatography, Gas↗
PubMedDate not supplied

[Study of the integral toxicity of aqueous media, polluted by petroleum and petroleum products using bacterial tests].

A biotest kit was used to assess the integral toxicity level of aquatic medium contamination with petroleum and petroleum-based products. The integral toxicity dynamics was also monitored during biodegradation of petroleum and petroleum-based products by an association of petroleum-degrading strains including Acinetobacter sp., Mycobacterium flavescens, and Rhodococcus sp. The following bacterial tests were used: the bioluminescence (BL) test based on Photobacterium leiognathi; electro-orientation (EO), optoosmotic (OO), and growth test; as well as the reducing activity (RA) test based on the Agrobacterium radiobacter culture. No significant increase in the integral toxicity level of aquatic medium was observed when diesel fuel and kerosene contamination had been subjected to biodegradation. Although express biotests (EO, OO, RA, and BL) detected a pronounced increase in the integral toxicity of aquatic medium, long-term growth biotest revealed no statistically significant increase in the toxicity level.

Acinetobacter↗
PubMed2002

Total synchronous fluorescence scan spectra of petroleum products.

Extending the two-dimensional synchronous fluorescence scan to a three-dimensional total synchronous fluorescence scan (TSFS) spectral measurement gives the total synchronous fluorescence characteristics of a multifluorophoric sample at various possible wavelength intervals (Deltalambda), which could help to characterize multifluorophoric systems better. TSFS spectra of petroleum products such as diesel, kerosene, petrol, engine oil etc., available in the Indian market, are reported. Fluorescence in these samples is due to the presence of polycyclic aromatic hydrocarbons (PAHs) of various ring sizes. The TSFS contour plot profiles of the neat samples measured at right-angle geometry is a result of various energy-degrading photophysical processes such as inner filter effect, light attenuation, resonance energy transfer, collisional quenching etc. TSFS plots make it easy to obtain the optimized Deltalambda of an unknown sample of analytical interest. TSFS and the excitation-emission matrix (EEM) techniques are similar, but the contour profiles generated are different. The response of the TSFS contour profiles to dilution is different from that in the EEM contour profiles. Thus, TSFS can provide an alternative way of presenting the fluorescence response of concentrated multifluorophoric samples.

Fuel Oils↗
PubMed2006

Spectral range optimization for the near-infrared quantitative analysis of petrochemical and petroleum products: naphtha and gasoline.

The proper selection of the spectral range in partial least squares (PLS) calibration is critical when highly overlapping spectra from compositionally complex samples are used, such as naphtha and gasoline. In particular, the relevant spectral information related to a given property is frequently localized in a narrow range, and the most selective region may be difficult to locate. We have presented the importance of range optimization in near-infrared (NIR) spectroscopy for the analyses of petrochemical and petroleum products that are generally highly complex in composition. For this purpose, the determination of a detailed compositional analysis (so called PIONA) and the distillation temperature of naphtha were evaluated. In the same fashion, the research octane number (RON) and Reid vapor pressure (RVP) were selected for gasoline. By optimizing the range using moving window (MW) PLS, the overall calibration performance was improved by finding the optimal spectral range for each property. In particular, for a detailed compositional analysis of naphtha, it was effective to search for localized spectral information in a relatively narrow range with fewer factors.

Journal Article↗
PubMed1980

Polycyclic aromatic hydrocarbons in petroleum products for medicinal and cosmetic uses--analytical procedure.

Two methods for extraction and determination of benzo[a]pyrene and other PAH in liquid and white soft paraffins, widely used for medicinal and cosmetic purposes, are compared. A method based on extraction by frontal elution chromatography, column and thin-layer chromatography and final spectrophotofluorometric determination gave the best results in the determination of the very low levels (ng/g) of PAH present in these fully refined samples. The complete analytical procedure showed an acceptable percentage of recoveries and good applicability to routine analysis of the PAH content in these petroleum products for the proper evaluation of their potential hazards to human health.

Benzopyrenes↗