CCQM-K102 Polybrominated diphenyl ethers in sediment

The key comparison CCQM-K102: Polybrominated diphenyl ethers in sediment was coordinated by the JRC, Directorate F – Health, Consumers & Reference Materials, Geel (Belgium) under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM). Thirtheen National Metrology institutes or Designated Institutes and the JRC participated. Participants were requested to report the mass fraction (on a dry mass basis) of BDE 47, 99 and 153 in the freshwater sediment study material. The sediment originated from a river in Belgium and contained PBDEs (and other pollutants) at levels commonly found in environmental samples. The comparison was designed to demonstrate participants' capability of analysing non-polar organic molecules in abiotic dried matrices (approximate range of molecular weights: 100 to 800 g/mol, polarity corresponding to pKow < -2, range of mass fraction: 1-1000 µg/kg). All participants (except one using ultrasonic extraction) applied Pressurised Liquid Extraction or Soxhlet, while the instrumental analysis was performed with GC-MS/MS, GC-MS or GC-HRMS. Isotope Dilution Mass Spectrometry approach was used for quantification (except in one case). The assigned Key Comparison Reference Values (KCRVs) were the medians of thirteen results for BDE 47 and eleven results for BDE 99 and 153, respectively. BDE 47 was assigned a KCRV of 15.60 µg/kg with a combined standard uncertainty of 0.41 µg/kg, BDE 99 was assigned a KCRV of 33.69 µg/kg with a combined standard uncertainty of 0.81 µg/kg and BDE 153 was assigned a KCRV of 6.28 µg/kg with a combined standard uncertainty of 0.28 µg/kg. The k-factor for the estimation of the expanded uncertainty of the KCRVs was chosen as k = 2. The degree of equivalence (with the KCRV) and its uncertainty were calculated for each result. Most of the participants to CCQM-K102 were able to demonstrate or confirm their capabilities in the analysis of non-polar organic molecules in abiotic dried matrices. Throughout the study it became clear that matrix interferences can influence the accurate quantification of the PBDEs, if the analytical methodology applied is not appropriately adapted and optimised. This comparison shows that quantification of PBDEs at the µg/kg low-middle range in a challenging environmental abiotic dried matrix can be achieved with relative expanded uncertainties below 15 % (more than 70 % of participating laboratories), well in line with the best measurement performances in the environmental analysis field.JRC.F.6-Reference Material