TY - CONF A1 - Lehnik-Habrink, Petra A1 - Mülow-Stollin, Ulrike A1 - Kluge, Stephanie A1 - Bremser, Wolfram A1 - Piechotta, Christian T1 - Evaluation of suitability of PLE, soxhlet, and shaking for extraction of POPs from soil N2 - The occurrence of persistent organic pollutants like polychlorinated biphenyls (PCB) and organochlorine pesticides (OCP) in the environment is still a matter of concern, even years after their use was abolished. Hence, threshold values are regulated by law which reference a number of national and international standards for determination of said contaminants. In this context, soil is an especially difficult matrix, because several defining parameters can vary in a wide range. Organic matter content in particular has a crucial influence on extractability of contaminants because it largely governs formation of non-extractable or bound residues. For this study, four soils of different total organic carbon (TOC) content were generated from uncontaminated reference soil (RefeSol 01-A) and compost which were spiked to contaminant levels representative of the Bundes-Bodenschutz-Verordnung (BBodSchV). These test materials were extracted using accelerated solvent extraction (ASE), Soxhlet extraction, and liquid-liquid extraction. For the latter method, samples were initially extracted for 15 minutes employing acetone. The follow-up extraction step was carried out using cyclohexane and the extraction time varied between 15 minutes and 16 hours. After clean-up, extracts were analysed via gas chromatography-mass spectrometry (GC MS) and with a gas chromatograph equipped with an electron capture detector (GC ECD). Statistical analysis of the experimental values showed that recovery was not dependent on matrix TOC content. Also, no clear preference for a single method could be detected. Concerning liquid-liquid-extraction, it is merely observed that prolonged extraction time results in slightly higher recoveries, while moderate extraction times appear to yield the most robust results. Although Soxhlet and ASE show high recoveries, they also lead to larger standard deviations and are not suitable for determination of thermolabile pesticides. In addition to recovery by different extraction methods, the agreement of values obtained by ECD and MS was evaluated. For ECD, standard deviations are generally higher but overall the values obtained by MS and ECD are comparable. T2 - International network of environmental forensics CY - Oerebro, Sweden DA - 27.06.2016 KW - Pesticides KW - PCB KW - Organic matter KW - Comparison extraction methods PY - 2016 AN - OPUS4-38605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lehnik-Habrink, Petra A1 - Mülow-Stollin, Ulrike T1 - Comparison of extraction methods for analysis of OCP and PCB in soils N2 - The determination of organochlorine pesticides (OCP) and polychlorinated biphenyls is challenging because they are strongly physical and chemical bound to soil organic matter. There are various valid standards for the determination of these analytes in soil that differ especially in the extraction method and extraction time. In order to make profound assessments concerning the extraction efficiency seven extraction procedures namely pressurized liquid extraction (PLE), soxhlet and shaking with different extraction times 0.5 h, 1 h, 3 h, 6 h and 16 h were compared. For the study four soils of different total organic carbon (TOC) content were generated from uncontaminated reference soil and compost which were spiked to contaminant levels representative of the Bundes-Bodenschutz-Verordnung. Clean-up and measurement conditions using gas chromatography with mass spectrometry (GC-MS) were kept constant. Statistically analysis of the experimental values showed that recovery rates were not dependent on matrix TOC content. In consideration of measurement uncertainties of 10% - 20% for the determination of OCP and PCB in soil no differences in the efficiency between the tested extraction procedures could be observed. T2 - ISO Meeting CY - Paris, France DA - 24.10.2016 KW - Standardization KW - PCB KW - OCP KW - Extraction methods PY - 2016 AN - OPUS4-38611 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lehnik-Habrink, Petra A1 - Aichner, Bernhard A1 - Bussian, B. A1 - Hein, Sebastian T1 - Human influences on forest soil - pollution with PAH, PCB and OCP in Germany N2 - While organic pollutants have been extensively studied in urban and agricultural areas, data from forested regions are relatively rare. Within the framework of a forest soil inventory in Germany polycyclic aromatic hydrocarbons (PAH), polychlorinated biphenyls (PCB) and organochlorine pesticides (OCP) were analyzed in 1500 soil samples taken from 3 soil horizons at 447 sites. An analytical protocol was developed and validated for the simultaneous extraction and measurement of all analytes in humic rich soil at trace level range. It included pressurized liquid extraction (PLE) and a two step cleanup procedure consisting of gel permeation chromatography (GPC) followed by solid phase extraction (SPE). Quantification was carried out using gas chromatography combined with mass spectrometry (GC-MS). In line with the monitoring campaign a comprehensive quality assurance concept was implemented to guarantee constant analytical measurement conditions for two years. The protocol is applicable for field laboratories with a high level of automation and for analyzing high sample amounts. At most sampling sites pollutant concentrations gradually decrease with depth. Only few spots showed highest concentrations in the upper mineral soil. In the O-horizon the sum concentrations of 16 PAHs range from 104 to 14.000 µg/kg, of 6 PCBs from <1 to 106 µg/kg and the sum of DDT and metabolites range from <1 to ca. 4.000 µg/kg. The observed concentration of PAH, PCB and OCP reflect an ubiquitous background contamination at most sites. Relatively high concentrations of PAH and PCB are related to industrial areas and peak concentrations only of PAH are associated with open cast mining of brown coal areas. The spatial distribution of the contents of DDT and metabolites in German forest soils can clearly be attributed to historic application. A contribution of ubiquitous background pollution derived from long-range atmospheric transport is likely for some compounds in the studied area, e.g., DDT in the western part of Germany. The results generally reflect the distribution of POPs in densely populated and industrialized countries located in temperate regions]. T2 - International network of environmental forensics CY - Oerebro, Sweden DA - 27.06.2016 KW - Forest soil KW - Organic pollution KW - Spatial distribution PY - 2016 AN - OPUS4-38598 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -