Interaction of 15 priority substances for water monitoring at ng L-1 levels with glass-, aluminium- and fluorinated polyethylene bottles for the containment of water reference materials

Certified water reference materials (CRMs) are currently not available for most of the hydrophobic organic pollutants listed in the EU Water Framework Directive (WFD). To find the most suitable container type for subsequent reference material productions, feasibility studies for the preparation of waters with polycyclic aromatic hydrocarbons (PAHs), polybrominated diphenyl ethers (PBDEs) and tributyltin (TBT) close to Environmental Quality Standards (EQS) in water have been performed. Due to the hydrophobic nature of these compounds and their tendency to adsorb onto container-walls, an adequate selection of the most appropriate material for containment, storage and transport of water reference materials is crucial. Three different materials (aluminium, amber glass and fluorinated polyethylene, FPE) and three volume ranges (500/600 mL, 1000/1200 mL and 2000/3000 mL) were tested at ng L-1 level of the target compounds. FPE shows by far the highest loss of analytes due to adsorption onto the container walls for all compounds studied. Aluminium and glass are equally suited for PAHs and PBDEs, but aluminium is unsuitable as container material for TBT due to acid cleaning requirements. The volume of the containers had no dramatic effect on the adsorption behaviour of target compounds for the different volumes tested.JRC.D.2-Standards for Innovation and sustainable Developmen

Joint Research Project env08 “Traceable measurements for monitoring critical pollutants under the European Water Framework Directive (WFD) 2000/60/EC”

The Joint Research Project ENV08 “Traceable measurements for monitoring critical pollutants under the European Water Framework Directive (WFD) 2000/60/EC” is a multi-partner trans-national project within the targeted call “Environment” of the European Metrology Research Programme (EMRP). The EMRP represents a metrology-focused European programme of coordinated research and development that facilitates closer integration of national research programmes. ENV08 deals with the grand challenges for multidisciplinary metrology in environment meeting “the most urgent industrial and societal needs” as stated in the EMRP Outline 2008. The project aims to provide reference methods capable of analysing priority hazardous substances specified in the WFD at the proposed low environmental quality standard concentrations in the body of ground, surface and coastal waters. In addition, ENV08 will answer the need for accuracy and comparability of measurements for the end users capabilities assessment by developing concepts for reference materials. ENV08 is coordinated by BAM (Germany) and involves 14 European institutes. Five institutes work on the development of a validated measurement procedure for Polycyclic Aromatic Hydrocarbons (PAH) in whole water samples at a concentration level required by the EU Water Framework Directive (WFD)

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