TY - JOUR A1 - Sturgeon, R. E. A1 - Wahlen, R. A1 - Brandsch, T. A1 - Fairman, B. A1 - Wolf-Briche, C. A1 - Alonso, J. I. G. A1 - González, P. R. A1 - Encinar, J. R. A1 - Sanz-Medel, A. A1 - Inagaki, K. A1 - Takatsu, A. A1 - Lalere, B. A1 - Monperrus, M. A1 - Zuloaga, O. A1 - Krupp, E. A1 - Amouroux, D. A1 - Donard, O. F. X. A1 - Schimmel, H. A1 - Sejeroe-Olsen, B. A1 - Konieczka, P. A1 - Schultze, P. A1 - Taylor, P. A1 - Hearn, R. A1 - Mackay, L. A1 - Myors, R. A1 - Win, Tin A1 - Liebich, Almuth A1 - Philipp, Rosemarie A1 - Yang, L. A1 - Willie, S. T1 - Determination of tributyltin in marine sediment: Comité Consultatif pour la Quantité de Matière (CCQM) pilot study P-18 international intercomparison N2 - The capabilities of National Metrology Institutes (NMIs—those which are members of the Comité Consultatif pour la Quantité de Matière (CCQM)of the CIPM) and selected outside "expert" laboratories to quantitate (C4H9)3Sn+ (TBT) in a prepared marine sediment were assessed. This exercise was sanctioned by the 7th CCQM meeting, April 4–6, 2001, as an activity of the Inorganic Analysis Working Group and was jointly piloted by the Institute for National Measurement Standards of the National Research Council of Canada (NRC) and the Laboratory of the Government Chemist (LGC), UK. A total of 11 laboratories submitted results (7 NMIs, and 4 external labs). Two external laboratories utilized a standard calibration approach based on a natural abundance TBT standard, whereas all NMIs relied upon isotope dilution mass spectrometry for quantitation. For this purpose, a species specific 117Sn-enriched TBT standard was supplied by the LGC. No sample preparation methodology was prescribed by the piloting laboratories and, by consequence, a variety of approaches was adopted by the participants, including mechanical shaking, sonication, accelerated solvent extraction, microwave assisted extraction and heating in combination with Grignard derivatization, ethylation and direct sampling. Detection techniques included ICP–MS (with GC and HPLC sample introduction), GC–MS, GC–AED and GC–FPD. Recovery of TBT from a control standard (NRCC CRM PACS-2 marine sediment) averaged 93.5±2.4% (n=14). Results for the pilot material averaged 0.680±0.015 µmol kg–1 (n=14; 80.7±1.8 µg kg–1) with a median value of 0.676 µmol kg–1. Overall, performance was substantially better than state-of-the-art expectations and the satisfactory agreement amongst participants permitted scheduling of a follow-up Key comparison for TBT (K-28), a Pilot intercomparison for DBT (P-43), and certification of the test sediment for TBT content and its release as a new Certified Reference Material (HIPA-1) with a TBT content of 0.679±0.089 µmol kg–1 (expanded uncertainty, k=2, as Sn) (80.5±10.6 µg kg–1). Electronic Supplementary Material Supplementary material is available in the online version of this article at http://dx.doi.org/10.1007/s00216-003-2016-9. KW - Tributyltin KW - Marine sediment KW - International intercomparison PY - 2003 U6 - https://doi.org/10.1007/s00216-003-2016-9 SN - 1618-2642 SN - 1618-2650 VL - 376 IS - 6 SP - 780 EP - 787 PB - Springer CY - Berlin AN - OPUS4-10905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nxumalo, T. A1 - Akhdhar, A. A1 - Mueller, V. A1 - Simon, Fabian A1 - von der Au, Marcus A1 - Cossmer, Antje A1 - Pfeifer, Jens A1 - Krupp, E. A1 - Meermann, Björn A1 - Kindness, A. A1 - Feldmann, J. T1 - EOF and target PFAS analysis in surface waters affected by sewage treatment effluents in Berlin, Germany N2 - Per- and polyfuoroalkyl substances (PFAS) are emerging organic pollutants and can occur in surface and groundwater. To identify the degree of pollution in surface water with PFAS, often targeted HPLC–ESI–MS/MS has been employed in which commonly 30–40 compounds are analyzed. However, other PFAS and organofuorines remain undetected. We sampled surface water of the river Spree and the Teltow Canal in Berlin, Germany, which are afected by the efuent discharge of wastewater treatment plants. Here, we employed high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) for measuring extractable organofuorines (EOF) and compared in a mass balance approach the total fuorine to the identifed and quantifed PFAS from the targeted analysis. The analysis highlights that the EOF are in the range expected for an urban river system (Winchell et al. in Sci Total Environ 774, 2021). However, downstream of an efuent discharge, the EOF increased by one order of magnitude, e.g., 40.3 to 574 ng F L−1, along the Teltow Canal. From our target analytes, mostly short-chained perfuorinated carboxylic acids and sulfonates occur in the water, which however makes up less than 10% of the EOF. The increase in EOF in the Teltow Canal correlates well with the increase of perfuorohexanoic acid (PFHxA), indicating that PFHxA is characteristic for the discharged EOF but not responsible for the increase. Hence, it points to PFHxA precursor discharge. The study highlights that EOF screening using HR-CS-GFMAS is necessary to identify the full scale of pollution with regard to PFAS and other organofuorines such as pharmaceutical compounds from the efuent of WWTPs. KW - PFAS KW - WWTP KW - GF-MAS PY - 2023 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-580341 VL - 415 SP - 1195 EP - 1204 PB - Springer AN - OPUS4-58034 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -