Comparison of Two Extraction Methods for the Determination of Polycyclic Aromatic Hydrocarbons in Surface Soils Using Headspace SPME with GC-FID (original) (raw)
Related papers
Solid-phase extraction of polycyclic aromatic hydrocarbons from soil samples
Journal of Chromatography A, 1995
ABSTRACT A new solid-phase extraction (SPE) method was developed for the analysis of 16 polyaromatic hydrocarbons (PAHs) on the US Environmental Protection Agency priority list, in soil samples. Different types of SPE columns were tested and conditioning and elution steps were optimised. In the final procedure, soil samples are extracted with acetone and, after dilution with HPLC-grade water, loaded on a C8 SPE column. After washing, all PAHs are eluted with tetrahydrofuran (THF). The final THF extract is analysed on an HPLC system for PAHs.Recoveries of the volatile PAHs, naphthalene, acephthylene and acenaphthalene were 80–90%. All other recoveries are comparable with standard liquid-liquid extraction (LLE) and range from 75 to 90%.The method is compared with the conventional LLE method for different types of real soil samples of a Dutch monitoring programme. Results indicate that SPE is a good method for the sample preparation for the analysis of PAHs in soil samples. Compared with LLE, correlation coefficients are better than 0.9 with relative standard deviations for SPE between 0.8 and 9.1%. LLE standard deviations ranged from 1.1 to 15.1%.
African Journal of Environmental Science and Technology, 2011
The development of a fast, efficient and quantitative technique for the extraction, clean-up, and preconcentration of the 16 United States Environmental Protection Agency (USEPA) priority polycyclic aromatic hydrocarbons (PAHs) was carried out on contaminated soils. The effect of Soxhlet, ultrasonication and mechanical shaking used in the extraction of a low-level PAH soil certified reference material (CRM131-100) was investigated. Six different extraction solvents: acetone, cyclohexane, 2-propanol, methanol, acetonitrile and dichloromethane, were tested to select the most suitable solvent for the extraction of the 16 PAHs from the certified soil reference material. The results were compared to determine the method with the highest extraction efficiency. The clean up and preconcentration procedures for the PAHs were optimised using the solid phase extraction (SPE). Acetonitrile, dichloromethane and tetrahydrofuran were tested as eluants for the optimisation of SPE clean up. Chromatographic conditions for the separation of PAHs using High Performance Liquid Chromatography (HPLC) using UV-DAD and fluorimetric detection with programmed excitation and emission wavelengths were also optimised. The optimised ultrasonic extraction procedure and SPE clean-up extracted the PAHs from the certified reference material with recoveries ranging from 63.6 % to over 100%.
Extraction techniques for polycyclic aromatic hydrocarbons in soils
2010
This paper aims to provide a review of the analytical extraction techniques for polycyclic aromatic hydrocarbons (PAHs) in soils. The extraction technologies described here include Soxhlet extraction, ultrasonic and mechanical agitation, accelerated solvent extraction, supercritical and subcritical fluid extraction, microwave-assisted extraction, solid phase extraction and microextraction, thermal desorption and flash pyrolysis, as well as fluidised-bed extraction. The influencing factors in the extraction of PAHs from soil such as temperature, type of solvent, soil moisture, and other soil characteristics are also discussed. The paper concludes with a review of the models used to describe the kinetics of PAH desorption from soils during solvent extraction.
Determination of trace amounts of polycylic aromatic hydrocarbons in soil
Fresenius' Zeitschrift f�r Analytische Chemie, 1987
Summary. A method is described for the determination of polycyclic aromatic hydrocarbons in natural soil. The soil is dried and extracted by ultrasonic agitation with dichloromethane. The extract is purified by liquid-liquid partitioning with dimethylformamide, water and hexane followed by high performance liquid chromatography on a silica column. Quantitative analysis of the purifred extract is carried out by combined gas chromatography/mass spectrometry. The method yields reliable results at the ng/g level. naphthalene, biphenyl, acenaphthene, fluorene, phenanthrene, fl uoranthene, pyrene, chrysene/triphenylene and benzo-a-pyrene. Three additional PAHs were used as internal standards; d1s-biphenyl, 3,6-dimethylphenanthrene and 1,1-binaphthyl.
Validation of Procedures to Quantify Nonextractable Polycyclic Aromatic Hydrocarbon Residues in Soil
Journal of Environment Quality, 2003
plished by solvent extraction methods. These include batch solvent shaking extraction, continuous soxhlet ex-This study was conducted to optimize butanol solvent shake extractraction, and improved versions such as the soxtec extion, dichloromethane soxtec extraction, and methanolic saponification extraction for the selective extraction of aged polycyclic aromatic tractor and accelerated solvent extraction (Northcott hydrocarbons from soil. Extraction kinetics for these methods was and Jones, 2000c). Differences in the ability of specific established to determine the optimal time necessary to achieve exhausaqueous and organic solvents to extract compounds tive compound extraction. This resulted in times of 12, 6, and 5 h, from environmental solids can provide information rerespectively, for butanol, dichloromethane, and saponification, to exgarding compound retention mechanisms (Cheng, 1990; tract polycyclic aromatic hydrocarbons from previously spiked, then Kubiak et al., 1990). It aged soil. Increasing the soil mass to butanol volume ratio reduced the is generally accepted that solvents extract the available proportion of polycyclic aromatic hydrocarbon extracted by butanol, compound fraction of contaminant and not the bound highlighting the importance of determining and maintaining a constant or sequestered residues. Various studies have used soil to solvent ratio for comparative purposes. Drying soil samples before dichloromethane soxtec extraction reduced by 30 to 76% the n-butanol (BuOH) as a "mild" solvent for extracting amount of polycyclic aromatic hydrocarbons extracted. The effect of the bioavailable, or labile, fraction of polycyclic arosample drying is discussed with relevance to enhancing the formation matic hydrocarbons (PAHs) in soil, and dichloromethof nonextractable compounds in soil and compound losses previously ane (DCM) as a "vigorous" solvent for the quantitative assumed by volatilization. The optimized extraction procedures proextraction of total extractable PAHs (Hatzinger and vided low variability with relative standard deviations Յ 5.2% for Alexander, 1995; Kelsey and Alexander, 1997; White et analysis of multiple replicates. The results obtained by the optimized al., 1997). procedures provided equivalent or improved reproducibility to those Conventional and enhanced solvent extraction techobtained by other methods reported in the literature.
Pressurised liquid extraction of polycyclic aromatic hydrocarbons from contaminated soils
Journal of Chromatography A, 2000
Pressurised liquid extraction (PLE) was applied to determine the atmospheric levels of 16 polycyclic aromatic hydrocarbons (PAHs) in the gas and particulate phases. The method involved high-volume air sampling with quartz fibre filters (QFFs) and polyurethane foam (PUF) plugs and analytes were subsequently extracted from the samples by PLE, and determined with GC-MS. We optimised the PLE conditions for the solvent, the number of cycles and extraction temperature. Recoveries were higher than 90% for most compounds. Method LODs and LOQs were between 0.001 and 0.02 ng/m 3 and between 0.01 and 0.05 ng/m 3. Air samples were taken from a site in the region of Tarragona in Catalonia, Spain, where one of the largest petrochemical complexes in southern Europe is located. The total concentration of PAHs were from 6.7 to 27.66 ng/m 3 , with predominant levels of PAHs appearing in the gas phase (48-81%), and an average level of benzo[a]pyrene, the most carcinogenic PAH, of 0.86 ng/m 3 .
2010
An HPLC-Florescence Detection (FLD) method was developed and validated for the determination of sixteen polycyclic aromatic hydrocarbons (PAHs) in soil. The analyzed PAHs include naphthalene (Nap), acenaphthylene (Acy), acenaphthene (Ace), fluorene (Flu), phenanthrene (Phe), anthracene (Ant), fluoranthene (Fln), pyrene (Pyr), 1,2-benza[a]anthracene (BaA), chrysene (Chr), benzo[e]pyrene (BeP), benzo[e]acenaphthylene (BeA), benzo[k]fluoranthene (BkF), dibenzo[a,h]anthracene (DahA), benzo[g,h,i]perylene (Bghi)P and indeno[1,2,3-cd]pyrene (InP). The method employs a quick, easy, cheap, effective, rugged and safe (QuEChERS) multiresidue sample preparation procedure adopted from the Association of Analytical Communities (AOAC) Official method 2007.01 for extraction and cleanup. The analytes were separated on an Agilent ZORBAX Eclipse PAH column (4.6 mm × 50 mm, 1.8 μm) by gradient elution with a binary system of acetonitrile water with subsequent fluorescence detection set at appropriate ...
Evaluation of Soil Contamination by Polycyclic Aromatic Hydrocarbons in Gipuzkoa (Northern Spain)
Http Dx Doi Org 10 1080 15320383 2011 587042, 2011
Representative polycyclic aromatic hydrocarbons (PAHs) of low-medium molecular weight were determined using headspace solid-phase microextraction and gas chromatography with a flame ionization detector (HS-SPME-GC-FID) in ten surface soil samples from Gipuzkoa (Northern Spain). The sum of the PAHs ranged from 0.21 to 136.26 mg kg −1. Pyrene and chrysene were the most abundant detected PAHs with an average concentration around 3.1 mg kg −1. Pearson's correlation and PAH isomer ratios were applied to study the different origins of contamination. The results indicated that the PAH contamination in the studied area was a mixed pattern of pyrolytic and petrogenic inputs. Multivariate exploratory techniques, principal component analysis (PCA), and cluster analysis (CA) were also applied corroborating the PAH compounds patterns in the soils.
Journal of The Chilean Chemical Society, 2019
Background: Polycyclic aromatic hydrocarbons (PAHs) are a class of chemicals which have 2 to 7 fused aromatic rings. It is demonstrated that even trace amounts of PAHs are carcinogens, mutagens, and teratogens which can lead to serious risk to the health of humans. According to these facts, determination of PAHs in environmental samples is essential. Methods: In this study, ultrasonic in combination with salt-assisted liquid-liquid extraction was used efficiently for the extraction of PAHs from soil and water samples. In order to evaluate the performance of the proposed method three PAHs, naphthalene, anthracene and pyrene were selected as model analytes. Influential parameters on the extraction efficiency of analytes such as extraction solvent and its volume, salting-out agent and its concentration, ultrasonic time, ultrasonic amplitude and pulse were investigated and optimized. Results: The optimum conditions were as follow; extracting solvent; tetrahydofuran, extracting solvent volume; 3 mL, salting-out agent; sodium acetate, salting-out agent concentration; 20 %w/v, ultrasonic time; 10 s, ultrasonic amplitude; 60% and ultrasonic pulse; 0.5 s. The limits of quantitation for pyrene, naphthalene and anthracene were 1.0, 1.0 and 0.7 ng g-1 , respectively. Under the optimum conditions, obtained recoveries in different matrices were in the range of 80.0 to 100.0% with a relative standard deviation better than 7.5%. Conclusions: In the proposed method, after the UAE, sample was exposed to SALLE without need of solid residue removal from the sample. Therefore, extraction steps such as filtration and centrifuge were removed which lead to time saving.
Journal of Chromatography A
A method for the rapid determination of 18 polycyclic aromatic hydrocarbons (PAHs) in soil has been established based on a simplified solvent extraction and GC/MS/MS operated in pseudo multiple reaction monitoring mode (PMRM), a technique where the two quadrupoles mass monitor the same m/z. The PMRM approach proved superior to the classic single quadrupole technique, with enhanced sensitivity, specificity, and significant reduction in time consuming sample clean-up procedures. Trace level PAHs could be readily confirmed by their retention times and characteristic ions. The limit of quantitation in soil was observed to be 20 ng/g for 16 EPA-priority PAHs and 2 additional PAHs specific to Environment Canada. The developed method was linear over the calibration range 20-4000 ng/g in soil, with observed coefficients of determination of >0.996. Individual PAH recoveries from fortified soil were in the range 58.1 to 110.1%, with a precision between 0.3 and 4.9% RSD. The ruggedness of the method was demonstrated by the success of an inter-lab proficiency test study organized by the Canadian Association for Laboratory Accreditation. The present method was found to be applicable as a rapid, routine screening for PAH contamination in soil, with significant savings in terms of preparation time and solvent usage.