Determination of Aroclor 1260 in soil samples by gas chromatography with mass spectrometry and solid-phase microextraction

An expedited field analysis method was developed for the determination of polychlorinated biphenyls (PCBs) in soil matrices using a portable gas chromatography-mass spectrometry (GC-MS) instrument. Soil samples of approximately 0.5 g were measured with a portable scale and PCBs were extracted by headspace solid-phase microextraction (SPME) with a 100 µm polydimethylsiloxane (PDMS) fiber. Two milliliters of 0.2 M potassium permanganate and 0.5 mL of 6 M sulfuric acid solution were added to the soil matrices to facilitate the extraction of PCBs. The extraction was performed for 30 min at 100 ℃ in a portable heating block that was powered by a portable generator. The portable GC-MS instrument took less than 6 min per analysis and ran off an internal battery and helium cylinder. Six commercial PCB mixtures, Aroclor 1016, 1221, 1232, 1242, 1248, 1254, and 1260, could be classified based on the GC chromatograms and mass spectra. The detection limit of this method for Aroclor 1260 in soil matrices is approximately 10 ppm, which is sufficient for guiding remediation efforts in contaminated sites. This method was applicable to the on-site analysis of PCBs with a total analysis time of 37 min per sample. However, the total analysis time could be improved to less than 7 min per sample by conducting the rate-limiting extraction step for different samples in parallel.

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“…In this study, as elsewhere, 100 µm PDMS fibers were found to be the most suitable for PCB analyses. 29,30,34…”

Section: Experimental Methodsmentioning

confidence: 99%

Field Analysis of Polychlorinated Biphenyls (PCBs) in Soil Using Solid-Phase Microextraction (SPME) and a Portable Gas Chromatography–Mass Spectrometry System

et al. 2016

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“…Polychlorinated biphenyls (PCBs), a group of chlorinated aromatic hydrocarbons with 209 congeners, have been applied in a wide range of areas including heat transfer fluids and dielectric fluids . However, they are a typical class of the persistent organic pollutants that cause great harm to the environment as well as human health, due to their toxicity, lipophilicity, high stability, and biomagnification through the food chain . It is very urgent to develop a simple, rapid, and efficient method for the determination of PCB residues in water.…”

Section: Introductionmentioning

confidence: 99%

Separation and enrichment of six indicator polychlorinated biphenyls from real waters using a novel magnetic multiwalled carbon nanotube composite absorbent

Zhang

Gan

Pan

et al. 2015

J of Separation Science

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A novel and effective magnetic multiwalled carbon nanotube composite for the separation and enrichment of polychlorinated biphenyls was developed. Fe3 O4 @SiO2 core-shell structured nanoparticles were first synthesized, then the poly(sodium 4-styrenesulfonate) was laid on its surface to prepare the polyanionic magnetic nanoparticles. The above materials were then grafted with polycationic multiwalled carbon nanotubes, which were modified by polydiallyl dimethyl ammonium chloride through the layer-by-layer self-assembly approach. Its performance was tested by magnetic solid-phase extraction and gas chromatography with mass spectrometry for the determination of six kinds of indicator polychlorinated biphenyls in water samples. Under optimal conditions, the spiked recoveries of several real samples for six kinds of polychlorinated biphenyls (PCB28, PCB52, PCB101, PCB138, PCB153, PCB180) were in the range of 73.4-99.5% with relative standard deviations varying from 1.5 to 8.4%. All target compounds showed good linearities in the tested range with correlation coefficients higher than 0.9993. The limits of quantification for six kinds of indicator polychlorinated biphenyls were between 0.018 and 0.039 ng/mL. The proposed method was successfully applied to analyze polychlorinated biphenyls in real water samples. Satisfactory results were obtained using the effective magnetic absorbent.

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“…The optimization of the SPME-GC/MS method was discussed in another publication (Zhang et al, 2014). Aroclor 1260 standard was used to evaluate the optimization of the SPME and instrument conditions.…”

Section: Resultsmentioning

confidence: 99%

“…Extraction of PCBs from soil samples under optimized conditions were conducted using headspace SPME with 2 mL of saturated potassium dichromate solution and a 100 µm PDMS fiber at 100 °C for 30 min (Zhang et al, 2014). An aliquot of 0.5 g of soil sample was placed in a 20-mL SPME vial with the addition of 20 µL of internal standard solution.…”

Section: Sample Preparationmentioning

confidence: 99%

Simultaneous quantification of Aroclor mixtures in soil samples by gas chromatography/mass spectrometry with solid phase microextraction using partial least-squares regression

Zhang

Harrington

2015

Chemosphere

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Multivariate partial least-squares (PLS) method was applied to the quantification of two complex polychlorinated biphenyls (PCBs) commercial mixtures, Aroclor 1254 and 1260, in a soil matrix. PCBs in soil samples were extracted by headspace solid phase microextraction (SPME) and determined by gas chromatography/mass spectrometry (GC/MS). Decachlorinated biphenyl (deca-CB) was used as internal standard. After the baseline correction was applied, four data representations including extracted ion chromatograms (EIC) for Aroclor 1254, EIC for Aroclor 1260, EIC for both Aroclors and two-way data sets were constructed for PLS-1 and PLS-2 calibrations and evaluated with respect to quantitative prediction accuracy. The PLS model was optimized with respect to the number of latent variables using cross validation of the calibration data set. The validation of the method was performed with certified soil samples and real field soil samples and the predicted concentrations for both Aroclors using EIC data sets agreed with the certified values. The linear range of the method was from 10μgkg(-1) to 1000μgkg(-1) for both Aroclor 1254 and 1260 in soil matrices and the detection limit was 4μgkg(-1) for Aroclor 1254 and 6μgkg(-1) for Aroclor 1260. This holistic approach for the determination of mixtures of complex samples has broad application to environmental forensics and modeling.

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Determination of Aroclor 1260 in soil samples by gas chromatography with mass spectrometry and solid-phase microextraction

Cited by 8 publications

References 27 publications

Field Analysis of Polychlorinated Biphenyls (PCBs) in Soil Using Solid-Phase Microextraction (SPME) and a Portable Gas Chromatography–Mass Spectrometry System

Field Analysis of Polychlorinated Biphenyls (PCBs) in Soil Using Solid-Phase Microextraction (SPME) and a Portable Gas Chromatography–Mass Spectrometry System

Separation and enrichment of six indicator polychlorinated biphenyls from real waters using a novel magnetic multiwalled carbon nanotube composite absorbent

Simultaneous quantification of Aroclor mixtures in soil samples by gas chromatography/mass spectrometry with solid phase microextraction using partial least-squares regression

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