Quantitative determination of polycyclic aromatic hydrocarbons, polychlorinated biphenyls and organochlorine pesticides in sewage sludges using supercritical fluid extraction and mass spectrometric detection

• Published in: Journal of Chromatography A Vol. 852; no. 2; pp. 545 - 558
• Main Authors: Berset, J.D., Holzer, R.
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 13.08.1999; Elsevier
• Subjects: Analysis methods; Analytical chemistry; Applied sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography - methods; Exact sciences and technology; Gas chromatographic methods; Insecticides - analysis; Mass Spectrometry; Organochlorine compounds; Pesticides; Pollution; Polychlorinated biphenyls; Polychlorinated Biphenyls - analysis; Polycyclic Compounds - analysis; Polynuclear aromatic hydrocarbons; Reference Standards; Sewage - chemistry; Supercritical fluid extraction; Wastes; Polynuclear aromatic hydrocarbons; Organochlorine compounds; Pesticides; Polychlorinated biphenyls; Environmental analysis; Sewage sludge; Supercritical fluid extraction; Electron impact; Chemical analysis; Hydrocarbon; Coupled method; Polycyclic aromatic compound; Polychlorobiphenyl; Certified reference material; Gas chromatography; Sample preparation; Mass spectrometry; Quantitative analysis
• ISSN: 0021-9673
• DOI: 10.1016/S0021-9673(99)00641-X

Supercritical CO 2 extraction (SFE) proved to be a valuable, fast, quantitative and partly selective extraction technique for determining polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and chlorinated pesticides (OCPs) in sewage sludges of different catchment areas based on a comparison study with certified reference materials (CRMs) and on recovery data. Most PCB extracts could be measured directly after SFE whereas for PAHs a short clean-up improved the final separation by high-resolution capillary gas chromatography. Due to the amount of coextracted compounds and the low levels of OCPs, extracts obtained by SFE had to be submitted to a multistep clean-up for final measurement. Average concentrations of 6.9 mg/kg dry mass (dm) for the sum of the 16 Environmental Protection Agency PAHs, 0.1 mg/kg dm for the sum of the seven PCB congeners and 0.002–0.072 mg/kg dm for the OCPs were found in the sewage sludges. Compared to studies performed earlier in our laboratory PAHs are still present in similar concentrations whereas PCB levels have decreased significantly. OCPs could be detected in only low amounts. A correlation between sludge type and degree of contamination could only be found for PAHs.