P B T EUROMET- Project * Traceability for developing Traceability for EU-wide comparable Measurement...
-
Upload
charleen-allison -
Category
Documents
-
view
224 -
download
0
Transcript of P B T EUROMET- Project * Traceability for developing Traceability for EU-wide comparable Measurement...
P BP BTT
EUROMET- Project *for developing TraceabilityTraceability for EU-wide comparable
Measurement Results in Water Monitoring
Organized by
Physikalisch-Technische Bundesanstalt (PTB), GermanyBundesanstalt für Materialforschung- und prüfung (BAM), Germany
Laboratoire National de Metrologie et d‘Essais (LNE), FranceInstitute 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.
Detlef Schiel, PTB, Germany
P BP BTT
ComparabilityComparability
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
Reference point
Calibration materialCertified Reference materialComparison measurement
P BP BTT
ComparabilityComparability
Motivation: - Requirement of comparable measurement results for monitoring and assessment of the water quality (Annex V, 1.3.6)
Consensus value
Confined 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)
P BP BTT
ComparabilityComparability
Measurement results of the monitoring laboratories
SI (Mol) Internationally accepted traceability basis
Traceability and Dissemination chains
Motivation: Metrological demand due to the requirement of comparable measurement results for monitoring and assessments of the water quality (Annex V, 1.3.6)
P BP BTT
Euromet-Project 924Euromet-Project 924
Objective: - Development of a traceability and dissemination system
Subject: - Inorganic elements of the list of priority substancesNi, Cd, Pb, Hg
Deliverables: - Sustainability- Link with all monitoring laboratories- Europe-wide comparable measurement results - global acceptance (key comparison of CCQM)
P BP BTT
Intended Dissemination StructureIntended Dissemination Structure
Step 2: Validation of the measurement procedure of the PRLs supported by NMIs
Step 3: Link of field laboratories and PRLs in the framework of a PT scheme
NMIs
Monitoring Laboratories
Potential Reference Laboratories
Step 1: Link of NMIs and PRLs by means of a comparison measurement
PRL: Potential Reference Laboratories
P BP BTT
Time scheduleTime schedule
2007 May Step 1: Comparison of NMIs and PRLs
2007 Nov. Meeting of the participants in the PTB
2008 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
P BP BTT
ParticipantsParticipants
NMIs: PTB (Ge), BAM (Ge), LNE (Fr), IRMM (EU), SP (Se), INM (Ro), NCM (Bg), LGC (UK)
PRLs: Ge 8Fr 4Se 2Il 2Pt 2Hu 1It 1At 1
Registered so far:Registered so far: 8 NMIs and 21 PRLs from 13 EU countries 8 NMIs and 21 PRLs from 13 EU countries
P BP BTT
Thanks Thanks
for your attentionfor your attention
P BP BTT
List of participants (preliminary)List of participants (preliminary)
- 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
PTB + BAM
LNE - Cemagref - INERIS - BRGM - IFREMER
IRMM
NPL (Israel) - National Public Health Laboratory - National Water Monitoring Laboratory
LGC - ?
SP - NIVA- Analytica- ITM (Uni Stockholm)
Σ 7 NMIs and 17 PCLs
NMIs PCLs
National authorities +PT scheme providers
National authorities
National authorities
Analytical service provider
P BP BTT
CCQM pilot studiesCCQM pilot studies
CCQM-P100.1 CCQM-P100.2
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
Pure water
Prepared by BAM
Gravimetrically spiked
Gravimetrical reference value
Concentration 0,02 - 0,1 μg/l
Natural water
Prepared by LNE
Water will be filtered
Spiked, but no gravimetrical reference value
Concentration 0,2 - 1,0 μg/l
P BP BTT
Setup of the comparison (step1)Setup of the comparison (step1)
Separation in two partsIn order to come to unambiguous results
Part 1: Synthetic water (BAM)Distribution in April/Mai
Sample a: Cd 0,1 - 0,3 μg/l, Pb 5 - 10 μg/lNi 10 - 30 μg/l
Sample b: Hg 0,04 - 0,06 μg/l
Part 2: Natural water (LNE)Distribution in July
Sample a+c: Cd, Pb, Ni in PFA- bottles 100ml, acidified with HNO3
Sample b+d: Hg in glass bottles 500ml, stabilized in BrCl
- 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 c: Cd 0,3 - 0,5 μg/l, Pb 15 - 25 μg/lNi 30 - 50 μg/l
Sample d: Hg 0,3 - 0,5 μg/l
P BP BTT
Additional remarksAdditional 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 year avtivities: EMRP
Participation: First step towards the proposed dissemination structure Therefore: Also open to countries without any QC system so far
P BP BTT
List of pList of priority substancesriority substances
Good water quality is defined by „Environmental quality standards“ (EQS)
33 Substances has 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 psCd 0,08-0,2 phs Hg
0,05 phs Ni20 ps
(tributyltin 0,0002 phs)
ps priority substancephs: priority hazardous substance
P BP BTT
Precision method (PTB)
Traceability and dissemination chainTraceability and dissemination chain
Method of the routine laboratory
Certification method (Merck)
Purity determination (BAM)
Gravimetrical preparation (PTB)
Sample X
Sample solution wX(E)
Secondary standard Y
Commercial sol., Urel= 0,3% wY(E)
Transfer standard T
Transfer sol., Urel= 0,1% wT(E)
SI
kg and mol NA
Primary standard
Primary sol. S, Urel= 0,05% wS(E)
Pure material, Urel= 0,01% wpur
Dis
sem
inat
ion
Values of materials assigned bymethods of measurement
Traceability
P BP BTT
registered participated
METABOLITES & SUBSTRATES Total Cholesterol 9 9Total Glycerol 2 2Creatinine 5 3Uric Acid 6 5Urea 3 3Glucose 4 3Total Bilirubine 2 2
ELECTROLYTES Sodium 8 6Potassium 7 4Chloride 4 3Calcium 4 1Lithium 5 2Magnesium 4 1
ENZYMES ALT 12 10AST 8 4CK 9 4LDH 9 4GGT 9 5Amylase 6 2
PROTEINS Total Protein 3 2Albumin 4 3
HORMONES Aldosterone 1 1Cortisol 3 3Progesterone 3 3Testosterone 1 1Estradiol-17ß 1 1Estriol (non-conjugates) 1 1Total Thyroxine (TT4) 1 1Total Tri-iodothyronine (TT3)17-Hydroxyprogesterone 1 1
THERAP.DRUGS Digoxin 1 1Digitoxin 3 3Theophyllin
Glyc. Proteins HbA1c 4 3
SUM 143 97
LaboratoriesMeasurand
Reference Laboratories in Laboratory Medicine
RELA 2003
registered participated
METABOLITES & SUBSTRATES Total Cholesterol 9 8Total Glycerol 2 2Creatinine 12 10Uric Acid 6 6Urea 3 2Glucose 5 4Total Bilirubine 2 2
ELECTROLYTES Sodium 5 5Potassium 12 11Chloride 3 3Calcium 3 3Lithium 4 4Magnesium 3 3
ENZYMES ALT 7 5AST 7 5CK 5 4LDH 18 16GGT 9 7Amylase 7 4
PROTEINS Total Protein 7 7Albumin
HORMONES Aldosterone 1 1Cortisol 8 7Progesterone 2 2Testosterone 1 1Estradiol-17ß 1 1Estriol (non-conjugates) 1 1Total Thyroxine (TT4) 1 1Total Tri-iodothyronine (TT3) 1 117-Hydroxyprogesterone 1 1
THERAP.DRUGS Digoxin 5 5Digitoxin 2 2Theophyllin
SUM 153 134
LaboratoriesMeasurand
Reference Laboratories in Laboratory Medicine
RELA 2004