Validation of European horizontal methods for the analysis of PAH, PCB and dioxins in sludge, treated biowaste and soil

Abstract

Background: Draft standards for the determination of organic pollutants in the solid matter of environmental matrices such as sludge, treated biowaste and soil have been basically developed in the framework of the European standardisation project HORIZONTAL. A research project financed by the German Federal Environment Agency was initiated to finalise some of these CEN standard drafts, since fully validated standard procedures are crucial for the evaluation of their reliability in the context of implementation in legislation on environmental health. Approach: Appropriate test materials (< 2 mm particle size) were prepared and homogenised from contaminated soils, sludge and treated biowaste containing polycyclic aromatic hydrocarbons (PAH), polychlorinated biphenyls (PCB), dioxins, furans and dioxin-like-PCB and served, along with reference solutions, as the basis for international interlaboratory comparisons. Performance data of three analytical standard procedures were obtained by the statistical evaluation of results received from 11 to 29 participants per test material. Results: The overall variation coefficients of reproducibility (between-lab standard deviations) for the sum parameters were roughly between 10 and 35%. The variation coefficients of repeatability (within-lab standard deviations) range between 3 and 8% and show no trend considering the substance groups or matrices. The highest coefficients of reproducibility were found for the analysis of PAH, which were between 26 and 35%, depending on the matrix, whereas 7-17% reproducibility was observed for toxicity equivalents (TEQ) comprising dioxins, furans and dl-PCB. Conclusions: Overall, the results confirm that the procedures described in the Technical Specifications are fit for purpose for all three matrices and that the feasibility of the HORIZONTAL approach, to cover several matrices with one standard per analyte, was thereby proven.

Developing an Improved Strategy for the Analysis of Polychlorinated Dibenzo-p-Dioxins/Furans and Dioxin-like Polychlorinated Biphenyls in Contaminated Soils Using a Combination of a One-Step Cleanup Method and Gas Chromatography with Triple Quadrupole Mass Spectrometry

“…The average recoveries of the labeled standards are in the range of 54.2%-90.0% with an RSD of 15% for 12 13 C-dl-PCBs and 46.1%-69.9% with an RSD of 20% for 15 13 C-PCDDs/Fs. These results satisfy the QC criteria of the EN 16190:2018 method (50%-130% for tetrachlorinated to hexachlorinated congeners and 40%-130% for heptachlorinated and octachlorinated congeners) [50][51][52].…”

Case Study on Secondary Building Materials for a Greener Economy

“…Different soil-like material types containing PAHs were investigated (see Section 2.2). A major challenge in sample acquisition was the relatively narrow target range of the PAH content, which was between 3 and 6 mg/kg of dry matter (concentration between precautionary limit value and its double value)-considering a high measurement uncertainty at this concentration level mainly caused by the laborious sample preparation steps before analysis [28]. Finally, twelve of the twenty-three investigated materials had a total PAH content in the desired range (see Table 1 and Figure 4).…”

PAHs, PCBs and Environmental Contamination in Char Products

“…The addition of biochar containing POPs would increase the concentration. The main barrier to analysis of POP in soil is the variability of the soil and a methodology is complex and there is no specified guidelines and corresponding legislation [2]. Consequently, there is no incentive to analyze for organic contamination and the main analysis reports metal levels.…”