Bureau International des Poids et Mesures
Key Comparisons, the MRA and CMCs:
An International Measurement Infrastructure
Robert Wielgosz
Bureau International des Poids et Mesures
Bureau International des Poids et Mesures
Bureau International des Poids et Mesures
The task of the BIPM is to ensure world-wide uniformity of measurements and their traceability to the International System of Units (SI).
Bureau International des Poids et Mesures
Bureau International des Poids et Mesures
International Trade Requires Traceability and Comparability
NMI: National Measurement Institute
Seller Buyer
Specifications Requirements
Measurements Measurements
NMIbNMIacomparability
trac
eabi
lity
trade
Bureau International des Poids et Mesures
Bureau International des Poids et Mesures
Objectives of the MRA are to:
establish the degree of equivalence of measurementstandards maintained by NMIs;
provide for the mutual recognition of calibration andmeasurement certificates issued by NMIs; thereby to
provide governments and other parties with a securetechnical foundation for wider agreements related tointernational trade, commerce and regulatory affairs
Bureau International des Poids et Mesures
Mutual recognition of national measurement standards and of calibration and measurement certificates issued by national
metrology institutes
Statements of the measurement capabilities of each NMI in the BIPM key comparisons and calibration database publicly available on the web; included are:
the results of the key comparisons
lists of calibration and measurement capabilities of each participating NMI ( some ten thousand lines of data now on the web)
www.bipm.org
Bureau International des Poids et MesuresFebruary 2001
Bureau International des Poids et Mesures
CCQM-P28 Ozone, ambient level
SRP0,2SRP0,2
SRP12,16SRP12,16
SRP25SRP25SRP21SRP21
SRP24SRP24SRP20SRP20
SRP17SRP17SRP29SRP29
SRP14,18SRP14,18
SRP15,23SRP15,23
SRP22SRP22
SRP1SRP1--1010
+ BIPM : SRP27,28, 31, 32 and 33+ BIPM : SRP27,28, 31, 32 and 33
SRP11SRP11
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SRP facilities at the BIPM
Triad ofTriad of SRPsSRPs maintained at the BIPM maintained at the BIPM
Measurement range: to 500 nmol/mol
Instruments: SRP27, SRP28, SRP31, SRP32, SRP33, SRP19 (PTB, UBA)
Reference instrument: SRP27
Bureau International des Poids et Mesures
Consultative CommitteesRMOsBIPM
Key comparison database
MRA appendix C
Mutual Recognition Arrangement
National Metrology Institutes
national key calibration quality supplementarymeasurement comparisons measurement systems comparisons to
standards capabilities support calibrations
results submissions
degrees of calibrationequivalence measurement
capabilities
Regional MetrologyOrganizations
(RMOs)
Consultative Committees
MRA appendix B
J C R B(Joint Committee of the RMOs
and the BIPM)
Bureau International des Poids et Mesures
Bureau International des Poids et Mesures
Regional Metrology Organizations
COOMET
APMP
EUROMETSIM
SADCMET
Bureau International des Poids et Mesures
Consultative Committee for Amount of Substance –CCQM - Metrology in Chemistry
Aim• Establishing worldwide comparability• Traceability to SI, or if not (yet) possible to other internationally
agreed references• Development of primary methods and databases
Thus• Scientific component• Interlaboratory comparisons and proficiency testing component
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CCQM
CCQM Working Groups
Key Comparisons and CMC Quality NRC-INMSOrganic Analysis NISTInorganic Analysis LGCGas Analysis NMiElectro-chemical Analysis SMUSurface Analysis NPLBio-Analysis LGC/NIST
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CCQM WG on Organic Analysis
• P,p’DDT in fish oil• LSD in human urine• Cholesterol in human serum• Glucose and creatinine in human serum• PCB’s in sediment• Organic purity assessment series• Ethanol in aqueous matrix (forensic level)• Organic calibration solutions (PCB, PAH, pesticides, etc.)• Drugs of abuse in urine
Bureau International des Poids et Mesures
CCQM WG on Inorganic Analysis
• Mono-elemental solutions• Pb and Cd in sediment• Zn and Cd in rice ; Pb in wine• Ca in serum• As in fish or shellfish• Metals in food digest• S in fuel• Minor elements in steel• Boron in Si• Purity of HCl
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CCQMCCQM--K8: Elemental Calibration Solution Standards K8: Elemental Calibration Solution Standards [Al, Cu, Fe, Mg [Al, Cu, Fe, Mg -- each at nominal value of 1 g/kg] each at nominal value of 1 g/kg] Dates of Study: 1999Dates of Study: 1999--20002000
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Fill CellI with HClat mHCl = 0,01 mol kg-1
measure E0Ag/AgCl
Fill CellI with samplemeasure pa
for at least 3 molalitiesof added chloride
Determine pa0 bylinear extrapolation
to mCl→0
Calculate γClat ionic strength
of sample
Calculate pHpH = pa0 + γCl
Literaturevalue forγ ± HCl
Bates-GuggenheimConvention
Result forsample (2)
Result forsample (1)
Harned Cell pH measurements
Measurement of pH. Definition, standards, and procedures (IUPAC Recommendations 2002)
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CCQM-K9: pH measurement comparison
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Calibration and Measurement Capabilities (CMCs)
Appendix C Search Form
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Cholesterol in human serum
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Automotive Emission Gases: CO in N2
Bureau International des Poids et Mesures
CCQM Pilot Study CCQM-P15, Pb and Cd in Sediment
Bureau International des Poids et Mesures
CCQM Pilot Study CCQM-P15, Pb and Cd in Sediment
Bureau International des Poids et Mesures
CCQM-P12 Pb in Wine
0.066
0.088
0.110
0.132
0.154
0.176
0.198
c
1
0-9
mol
·g-1
CCQM-P12 : Pb in wine
IRMM certified value(corresponds to IMEP-16 certified value)
Results from BAM, Germany; CENAM, Mexico; CSIR-NML, South-Africa; EMPA, Switzerland; IRMM, European Commission; KRISS, Korea; LGC, United Kingdom; LNE, France; NARL, Australia; NIMC, Japan; NIST, United States of America; NRCCRM, China; PTB, Germany; VNIIM, Russian Federation
±50%
Bureau International des Poids et Mesures
Assessing the quality of results of measurements : IMEP-16
13.59
16.31
19.03
21.74
24.46
27.18
29.90
32.62
35.33
38.05
40.77
-50
-40
-30
-20
-10
0
10
20
30
40
50
Use of an official method
No use of an official method
No information
Pb
Results from all participants in relation to the use of an official analytical method
IMEP- 16: Pb in wineCertified value : 27.18 ± 0.25 µg·L-1 [U=k·u c (k=2)]
Use of an official method 3No use of an official method 7No info 1
Values below -50%
No use of an official method 5 'Less than' value
Values above 50%Use of an official method 6No use of an official method 20No info 1
official method 2676/90
11
Bureau International des Poids et Mesures
Reference value, demonstrated to be equivalent at global level
13.6
16.3
19.0
21.7
24.5
27.2
29.9
32.6
35.3
38.1
40.8
Pb amount content
5 'less than' values11 values
below -50%
28 valuesabove 50%
IMEP-160.066
0.088
0.110
0.132
0.154
0.176
0.198
-50
-40
-30
-20
-10
0
10
20
30
40
50
CCQM-P12
Bureau International des Poids et Mesures
JOINT COMMITTEE on TRACEABILITYin LABORATORY MEDICINE (JCTLM)
Declaration of co-operation
establishing
A framework for the international recognition of available higher-order reference materials, measurement procedures and
reference measurement laboratories
Bureau International des Poids et Mesures
“The aim of the Joint Committee is to support world-widecomparability, reliability and equivalence of measurement results in Laboratory Medicine, for the purpose of improving health care, by:
• promoting the concept of traceability of measurement results to the Système International d’Unités (SI) or, where necessary, to other internationally agreed references;
• promoting close links between Reference Laboratories in Laboratory Medicine and National Metrology Institutes;
• co-ordinating and giving guidance in the establishment of Reference Measurement Systems with respect to medical
needs;
Mission Statement
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JCTLM
Implementation of • EC-IVD Directive (98/79/EC)
EC-IVD Directive, Annex I, Essential requirements A.3'...The traceability of values assigned to calibrators
and/or control materials must be assured throughavailable reference measurement procedures and/oravailable reference materials of a higher order.'
Bureau International des Poids et Mesures
JCTLM Executive• Priority setting• Decision on projects• Identification of appropriate organizations
2002-2004: Chairman - IFCC : Prof J H H ThijssenSecretariat - BIPMExecutive Secretary: Dr R I Wielgosz
IFCC, ILAC, BIPM and JCTLM WG Chairmen
Working Groups:WG 1: Reference Materials and Reference ProceduresWG 2: Reference Measurement Laboratories
Organization Structure
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JCTLM Working Group on Reference Materials and Reference Measurement Procedures
Charge:
• establishing a process for identifying, and reviewing against agreed upon criteria
• publishing a List of “higher order” Certified Reference Materials and Reference Measurement Procedures required for IVD industry compliance with the EC IVD Directive regarding in vitro diagnostic medical devices.
Co-Chairs: Willie E. May (NIST) Heinz Schimmel (EU Institute for Reference Materials & Measurements)
Bureau International des Poids et Mesures
JCTLM Working Group on Reference Laboratory Networks
Charge:
• Collecting information on existing and candidate reference measurement laboratories (RMLs)
• Encouraging and facilitating the formation of networks of RMLs for different groups of measurable quantities (concerning electrolytes, substrates/metabolites, enzymes, HbA1c, low molecular hormones, etc.)
• Developing comparisons to demonstrate the competence of RMLs
Co-Chairs: Professor Dr. Lothar Siekmann, University of Bonn (Germany)Professor Dr. Linda Thienpont, University of Gent (Belgium)
Bureau International des Poids et Mesures
Relevant ISO Standards
ISO 17511 In vitro diagnostic medical devices - Measurement of quantities in biological samples - Metrological traceability of values assigned to calibrators and control materials
ISO 15193 Presentation of reference measurement procedures
ISO 15194 Description of reference materials
ISO 15195 Reference Measurement Laboratories
ISO 18153 Metrological traceability of values for catalytic concentration of enzymes assigned to calibrators and control materials
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Primary Calibrators (ISO 17511)
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Initial Provisional List of Higher Order Reference Materials andReference Measurement Procedures -Two categories:
I. Certified Reference Materials and Reference Measurement Procedures for well-defined chemical entities or internationally recognized reference method-defined measurands, such as enzymes. Reference Materials included in this category are those that aretraceable to the SI units. [Electrolytes, Enzymes, Drugs, Metabolites and Substrates, Non-Peptide Hormones, Proteins (some)]
II. International Conventional Reference Materials, i.e., where the measurand(s) is/are not completely defined and/or no internationally recognized reference measurement procedure is available [e.g., WHO reference materials for Coagulation Factors, Nucleic Acids, someProteins]
Bureau International des Poids et Mesures
Joint Committee on Traceability in Laboratory MedicineJoint Committee on Traceability in Laboratory MedicineJCTLM
Review Teams for Highest Priority Analyte Areas
Worldwide representation from Lab Accreditation Organizations, NMIs, Professional Societies , and IVD Industry
Electrolytes Enzymes
Metabolites and Substrates Proteins
Nucleic Acids Drugs
Hormones Coagulation Factors
Bureau International des Poids et Mesures
CRM comparability studies