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EUROMET- Project * for developing Traceability for EU-wide comparable

EUROMET- Project * for developing Traceability for EU-wide comparable Measurement Results in Water Monitoring. Detlef Schiel, PTB, Germany. Organized by Physikalisch-Technische Bundesanstalt (PTB), Germany Bundesanstalt für Materialforschung- und prüfung (BAM), Germany

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EUROMET- Project * for developing Traceability for EU-wide comparable

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  1. EUROMET- Project * for developing Traceability for EU-wide comparable Measurement Results in Water Monitoring Detlef Schiel, PTB, Germany Organized by Physikalisch-Technische Bundesanstalt (PTB), Germany Bundesanstalt für Materialforschung- und prüfung (BAM), Germany Laboratoire National de Metrologie et d‘Essais (LNE), France Institute for Reference Materials and Measurements (IRMM), EU • *) EUROMET is a cooperative voluntary organisation between national metrology institutes in the EU and EFTA, including the European Commission.

  2. Measurement results of the monitoring laboratories Reference point Comparability • Motivation: Metrological demand due to the requirement of comparable measurement results for monitoring and assessments of the water quality (Annex V, 1.3.6) Calibration material Certified Reference material Comparison measurement

  3. Comparability • Motivation: Metrological demand due to the requirement of comparable measurement results for monitoring and assessments of the water quality (Annex V, 1.3.6) • Motivation: - Requirement of comparable measurement results for monitoring and assessment of the water quality (Annex V, 1.3.6) Confined comparability Consensus value

  4. Traceability and Dissemination chains Comparability • Motivation: Metrological demand due to the requirement of comparable measurement results for monitoring and assessments of the water quality (Annex V, 1.3.6) Measurement results of the monitoring laboratories Internationally accepted traceability basis SI (Mol)

  5. Euromet-Project 924 Objective: - Development of a traceability and dissemination system Subject: - Inorganic elements of the list of priority substances Ni, Cd, Pb, Hg Deliverables:- Sustainability - Link with all monitoring laboratories - Europe-wide comparable measurement results - global acceptance (key comparison of CCQM)

  6. Monitoring Laboratories • Step 3: Link of field laboratories and PRLs in the framework of a PT scheme • Step 2: Validation of the measurement procedure of the PRLs supported by NMIs • Step 1: Link of NMIs and PRLs by means of a comparison measurement NMIs PRL: Potential Reference Laboratories Intended Dissemination Structure Potential Reference Laboratories

  7. Time schedule • 2007 May Step 1: Comparison of NMIs and PRLs • 2007 Nov. Meeting of the participants in the PTB • Step 2: Validation of procedures of the PRLs and • Step 3: Comparison measurement organised by the PRLs for the monitoring laboratories • 2009 Feb. Report for Euromet

  8. Participants NMIs: PTB (Ge), BAM (Ge), LNE (Fr), IRMM (EU), SP (Se), INM (Ro), NCM (Bg), LGC (UK) PRLs: Ge 8 Fr 4 Se 2 Il 2 Pt 2 Hu 1 It 1 At 1 Registered so far: 8 NMIs and 21 PRLs from 13 EU countries

  9. Thanks • for your attention

  10. List of participants (preliminary) NMIs PCLs PTB + BAM - Rheinisch-Westfälisches Institut für Wasserwirtschaft - Bayerisches Landesamt für Umwelt - Institut für Hygiene und Umwelt, Hamburg - Landeslabor Schleswig-Holstein - Hessisches Landesamt für Umwelt und Geologie - Thüringer Landesanstalt für Umwelt und Geologie - Inst. f. Siedlungswasserbau, Wassergüte- und Abfallwirtschaft, Stuttgart - Landesumweltamt NRW National authorities +PT scheme providers LNE • - Cemagref • INERIS • BRGM- IFREMER National authorities NPL (Israel) • National Public Health Laboratory • National Water Monitoring Laboratory National authorities SP • - NIVA • Analytica • ITM (Uni Stockholm) Analytical service provider LGC - ? IRMM Σ7 NMIs and 17 PCLs

  11. CCQM pilot studies CCQM-P100.1 CCQM-P100.2 • Natural water • Prepared by LNE • Water will be filtered • Spiked, but no gravimetrical reference value • Concentration 0,2 - 1,0μg/l • Pure water • Prepared by BAM • Gravimetrically spiked • Gravimetrical reference value • Concentration 0,02 - 0,1 μg/l • Samples provided in glass bottles 500ml and stabilized in BrCl • Methods of measurement: e.g. ICP MS, AFS combined with cold with cold vapor technique and Au-preconcentration EPA method description 1631: http://www.epa.gov/waterscience/methods/1631method.html EN 13506 • CRMs e.g. BCR-579 or NRC

  12. Setup of the comparison (step1) Separation in two parts In order to come to unambiguous results Part 2: Natural water (LNE) Distribution in July Part 1: Synthetic water (BAM) Distribution in April/Mai • - Gravimetrically spiked • Gravimetrical reference value - Concentrations on the EQS level - Water will be filtered- Spiked, but no gravimetrical reference values- Slightly higher concentrations than in part 1 Sample a: Cd 0,1 - 0,3μg/l, Pb 5 - 10 μg/lNi 10 - 30 μg/l Sample b: Hg 0,04 - 0,06 μg/l Sample c: Cd 0,3 - 0,5μg/l, Pb 15 - 25 μg/lNi 30 - 50 μg/l Sample d: Hg 0,3 - 0,5 μg/l Sample a+c: Cd, Pb, Ni in PFA- bottles 100ml, acidified with HNO3Sample b+d: Hg in glass bottles 500ml, stabilized in BrCl

  13. Additional remarks • Methods of e.g.ICPMS,AAS,AFS probably combined measurement: with cold vapour technique or Au-preconcentration for Hg. • Traceability: e.g. NIST, PTB/BAM/Merck • CRM: e.g. Pb, Cd: BCR- 609; Hg: BCR-579, NRC • Costs: about 150-200 Euro for the comparison step1 • Status: Supplementary comparison of EUROMET • Planned CCQM Key at least for Hg in the next yearavtivities: EMRP • Participation: First step towards the proposed dissemination structure Therefore: Also open to countries without any QC system so far

  14. List of priority substances • Good water quality is defined by „Environmental quality standards“ (EQS) • 33 Substanceshas been identified to be in particular critical • 29 organic compounds and • 4 inorganic elements and their compounds • Main selection criteria: Persistence, Bioaccumulation, Toxicity substance c in μg/l priority Pb 7,2 ps Cd 0,08-0,2 phs Hg 0,05 phs Ni 20 ps (tributyltin 0,0002 phs) ps priority substance phs: priority hazardous substance

  15. Sample X wX(E) Sample solution Method of the routine laboratory Secondary standard Y Commercial sol., Urel= 0,3% wY(E) Certification method (Merck) Dissemination Traceability Transfer standard T Transfer sol., Urel= 0,1% wT(E) Precision method (PTB) Primary sol. S, Urel= 0,05% wS(E) Primary standard Pure material, Urel= 0,01% wpur Gravimetrical preparation (PTB) Purity determination (BAM) SI kg and mol NA Traceability and dissemination chain assigned bymethods of measurement Values of materials

  16. SUM 160 SUM 160

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