Routine analysis of hydrocarbons, PCB and PAH in marine sediments using supercritical CO2 extraction

Berg, B. E.; Lund, Hanne; Kringstad, Alfhild; Kvernheim, Arne Lund

doi:10.1016/s0045-6535(98)00213-6

Cited by 35 publications

(25 citation statements)

References 15 publications

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“…Extraction, online cleanup, concentration and analysis by GC-ECD (GC-MS) took only 90 min. Another methodology for the determination of PCBs [72] [20] octane from C 18 -modified silica provided the best results. A comparison of the evaluated recoveries obtained with this method and the results from Soxhlet extraction and inter-laboratory studies showed that no significant differences were found.…”

Section: Biological Matricesmentioning

confidence: 99%

“…Berg et al [20] studied PCBs along with PAHs and hydrocarbons in marine sediments using automated SFE for routine analysis. Analytes were collected in n-hexane, then diluted and divided into three aliquots to determine each family of compounds.…”

Section: Marine Sedimentsmentioning

confidence: 99%

“…During the SFE step, many interfering components, such as large amounts of elemental sulphur, are coextracted from sediment samples together with the target analytes; so a clean-up procedure is generally required before the final chromatographic determination [25]. The simplest treatment that can be used on the sample to eliminate sulphur consists of a mixture of copper powder directly activated in the extraction cell [20,66,76]. Among the different extraction methods used for the certification of 14 PCB congeners and 4 OCPs in the new reference materials certified (NMIJ CRM 7304-a and NMIJ CRM 7305-a) [66], SFE stands out from the other procedures owing to its simplicity and high specificity.…”

Section: Elimination Of Sulphur From the Sedimentsmentioning

confidence: 99%

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Supercritical fluid extraction of polyhalogenated pollutants from aquaculture and marine environmental samples: A review

García-Rodríguez

Carro-Díaz

Lorenzo-Ferreira³

2008

J of Separation Science

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ReviewSupercritical fluid extraction of polyhalogenated pollutants from aquaculture and marine environmental samples: A review This article focuses on the state-of-the-art in sample preparation using supercritical fluid extraction (SFE), to monitor the content of polyhalogenated pollutants in aquaculture and marine environmental samples. Marine sediments and biological applications, including several types of samples matrices (fish, shellfish, seaweed and fish feed) and analyte groups (polychlorinated biphenyls (PCBs), polybrominated biphenyls (PBBs), polybrominated diphenylethers (PBDEs), polychlorinated dibenzop-dioxin (PCDD)/Fs and organochlorinated pesticide (OCPs)) are discussed with respect to SFE use and optimisation of conditions. We also discuss the great analytical potential of SFE, the integration of the extraction and clean-up steps for rapid sample processing justifying its use for routine work. The most recent SFE applications to the determination of these pollutants in marine environmental (biota and sediment) samples, published in the last 15 years, are reviewed.

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Section: Biological Matricesmentioning

confidence: 99%

Section: Marine Sedimentsmentioning

confidence: 99%

Section: Elimination Of Sulphur From the Sedimentsmentioning

confidence: 99%

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Supercritical fluid extraction of polyhalogenated pollutants from aquaculture and marine environmental samples: A review

García-Rodríguez

Carro-Díaz

Lorenzo-Ferreira³

2008

J of Separation Science

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“…The apparatus had to meet several constraints: (1) Only small (ie., max of a gram or two) quantities of pure PCB congeners could be used, both from a safety and a cost standpoint; (2) the solubility of PCB congener in the aqueous phase had to be determined in situ, so that no sampling (and no consumption of or exposure to PCBs) would be required; (3) the in situ method of solubility analysis had to be sensitive enough to obtain good accuracies for systems containing as little as a few ppm of PCB congener in water; (4) the apparatus had to operate from ambient to 200-250 "C. A schematic of the apparatus that was designed and constructed is shown in Figure 1 1. The apparatus, which is of the static recirculating type, consists of a view cell for contacting the PCB liquid (bottom) phase and the aqueous (top) phase, and for establishing equilibrium between these phases. Continuous flow of the aqueous phase through the PCB phase in the cell and through the optical flow cell is accomplished with a magnetic pump that was constructed at Clemson (see Figure 12).…”

Section: I?mentioning

confidence: 99%

Basic Engineering Research for D and D of R Reactor Storage Pond Sludge: Electrokinetics, Carbon Dioxide Extraction, and Supercritical Water Oxidation

Matthews¹,

Bruce²,

Davis³

et al. 2002

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“…[5][6][7][8][9] However, the recovery yields of PCBs by SFE were significantly affected by various operating parameters, including the extraction temperature, [6][7][8][9][10][11][12][13] extraction pressure 8,9,12-14 and modifier addition. 8,9,[14][15][16][17] Therefore, optimization of the SFE conditions is very important for the accurate quantification of PCBs in sediments.Isotope dilution mass spectrometry (IDMS) has potential to be operated as a primary method of measurement. 18 Accurate quantification of PCBs may be expected when the IDMS technique is applied with GC-MS.…”

mentioning

confidence: 99%

Evaluation of Supercritical Fluid Extraction for Isotope Dilution Gas Chromatography-Mass Spectrometric Quantification of Polychlorinated Biphenyls in Sediment

et al. 2006

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Polychlorinated biphenyls (PCBs) are representative persistent organic pollutants and suspected to be endocrine disrupters. Although PCBs have been removed from production and use in Japan since the early 1970s, they still remain in the environment. One of the major environmental sinks for PCBs is the sediment matrix, and thus the accurate quantification of trace PCBs in this matrix is important for evaluating their risk.In general, the quantification of PCBs in the sediment includes three analytical processes: the extraction of PCBs from the sediment, cleanup of the extracts, and analysis by gas chromatography (GC) with either mass spectrometry (MS) or electron-capture detection. The classical extraction methods, such as Soxhlet extraction 1,2 and saponification, followed by solvent extraction, 3 are usually applied as extraction techniques, but these methods are time-consuming and require a large amount of organic solvents. Supercritical fluid extraction (SFE) can possibly overcome these disadvantages. 4 A number of articles have appeared on the SFE of PCBs from sediments. Compared with Soxhlet extraction, SFE can provide a comparable or higher extraction efficiency. [5][6][7][8][9] However, the recovery yields of PCBs by SFE were significantly affected by various operating parameters, including the extraction temperature, [6][7][8][9][10][11][12][13] extraction pressure 8,9,12-14 and modifier addition. 8,9,[14][15][16][17] Therefore, optimization of the SFE conditions is very important for the accurate quantification of PCBs in sediments.Isotope dilution mass spectrometry (IDMS) has potential to be operated as a primary method of measurement. 18 Accurate quantification of PCBs may be expected when the IDMS technique is applied with GC-MS. However, equilibration between isotope-labeled compounds added as internal standards and native analytes in the sample is a prerequisite in the IDMS technique. The results from ID-GC-MS would show an incorrectly low amount of PCBs if equilibration is not achieved, as would occur if the quantitative extraction of analytes from a solid matrix is not achieved. 19Therefore, highly efficient extraction is required for the accurate quantification of PCBs in sediments, even if isotope-labeled PCB congeners are used as internal standards.The National Metrology Institute of Japan (NMIJ) has developed two kinds of marine sediment certified reference materials (CRMs) to be used for the validation of PCB quantification. [20][21][22] In the certification process, five kinds of independent extraction methods were applied for IDMS quantification to avoid any possible procedural bias. For that purpose, we developed four accurate extraction methods for PCBs in sediments in advance. We developed pressurized liquid extraction 23,24 and microwave-assisted extraction 25 as extraction techniques for the IDMS quantification. A method of saponification, followed by solvent extraction, was also optimized to give higher recovery yields of PCB congeners. 26SFE is another extraction technique we have d...

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Routine analysis of hydrocarbons, PCB and PAH in marine sediments using supercritical CO2 extraction

Cited by 35 publications

References 15 publications

Supercritical fluid extraction of polyhalogenated pollutants from aquaculture and marine environmental samples: A review

Supercritical fluid extraction of polyhalogenated pollutants from aquaculture and marine environmental samples: A review

Basic Engineering Research for D and D of R Reactor Storage Pond Sludge: Electrokinetics, Carbon Dioxide Extraction, and Supercritical Water Oxidation

Evaluation of Supercritical Fluid Extraction for Isotope Dilution Gas Chromatography-Mass Spectrometric Quantification of Polychlorinated Biphenyls in Sediment

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