A Screening Method for Polycyclic Aromatic Hydrocarbons Determination in Water by Headspace SPME with GC-FID

A simple method for determination of polycyclic aromatic hydrocarbons (PAHs) in water using headspace solid-phase microextraction (HS-SPME) with gas chromatography-flame ionisation detector (GC-FID) was developed. In order to obtain the convenient experimental conditions for HS-SPME extraction an experimental design with two steps was accomplished. A 2^6-2 fractional factorial design and central composite design (CCD) considering three significant factors were used. Naphthalene, anthracene and fluoranthene were chosen as representatives of two, three and four aromatic rings, and the global response of three PAHs was used for the results, evaluation. The chosen extraction conditions were: 85 μm polyacrylate fibre; 50 °C temperature; 60 min time; 20 mL-dissolution volume (in 40 mL glass vial); without salt addition; and 2 min desorption time. The procedure was extended to other seven PAHs (acenaphthylene, acenaphthene, fluorene, phenanthrene, pyrene, chrysene and benzo(a)anthracene) and the analytical characteristics were checked. The limit of detection (LOD) was from 0.08 (anthracene) to 0.20 μg L^?1 (naphthalene). The precision expressed as relative standard deviation (RSD in %) using 50 μg L^?1 of each analyte ranged from 6.8 to 17 %. The method was applied to the analysis of the surface waters and leaching waters of contaminated soils from Gipuzkoa (North Spain). The PAHs were not detected in surface water samples. Most of the PAHs were found in the leachates from contaminated soils showing a maximum global value of 75.5 μg L^?1.     

A Screening Method for Polycyclic Aromatic Hydrocarbons Determination in Sediments by Headspace SPME with GC–FID

A screening method for polycyclic aromatic hydrocarbons (PAHs) determination in sediment using headspace solid phase microextraction (HS-SPME) with gas chromatography–flame ionization detection was developed. In order to obtain the convenient experimental conditions for HS-SPME extraction an experimental design with two steps was done. 0.2 g of sediment and 85 µm polyacrylate fibre, 80 °C and 120 min were the chosen extractions conditions. The limit of detection (LOD) was from 0.8 ng g⁻¹ (fluoranthene) to 8 ng g⁻¹ (chrysene). The relative standard deviation (RSD) was less than 7.0%. Determination of PAHs in NRC–CNRC–HS–3B reference marine sediment showed good agreement with the certified values. The method was applied in the analysis of ten river and estuary surface sediments from Gipuzkoa (North Spain). PAHs total concentration ranged from 400 to 5,500 ng g⁻¹.