World Structure for Metrology in Chemistry (CCQM) · PDF file15/01/04 NMi - the Art of Measurement 1 World Structure for Metrology in Chemistry (CCQM) Ed W.B. de Leer, Robert Kaarls

15/01/04 NM i - the Art of M easurement

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World Structure forMetrology in Chemistry (CCQM)

Ed W.B. de Leer, Robert KaarlsNMi Van Swinden Laboratorium

INMETRO, 17 November 2003


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• Metre Convention and Metrology Infrastructure• Ten years of CCQM• CCQM and the NMIs• CCQM and CCQM Working Groups• CCQM activities• Certified Reference Materials• Cooperation with other intergovernmental and international

organizations• Joint Committee on Traceability in Laboratory Medicine• Material properties• Designated institutes• BIPM programme

Contents


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M etre Convention

• The Convention of the Metre is a diplomatic treaty which givesauthority to the General Conference on Weights and Measures(Conférence Générale des Poids et Mesures, CGPM), theInternational Committee for Weights and Measures (ComitéInternational des Poids et Mesures, CIPM) and the InternationalBureau of Weights and Measures (Bureau International desPoids et Mesures, BIPM) to act in matters of world metrology,particularly concerning the demand for measurement standardsof ever increasing accuracy, range and diversity, and the needto demonstrate equivalence between national measurementstandards


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M etre Convention (II)

The Convention was signed in Paris in 1875 by representatives ofseventeen nations. As well as founding the BIPM and laying downthe way in which the activities of the BIPM should be financed andmanaged, the Metre Convention established a permanentorganizational structure for member governments to act in commonaccord on all matters relating to units of measurement.

The Convention remains the basis of international agreement onunits of measurement. There are now fifty-one Member States,including all the major industrialized countries.


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Metre Convention1875

General Conference onWeights and Measures (CGPM)

International Committee forWeights and Measures (CIPM)

Bureau Internationaldes Poids et Mesures (BIPM)

ConsultativeCommittees (CCs) National Metrology

Institutes (NMIs)

CIPMMRA

Organization Structure


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• Comité Consultatif pour la Quantité de la Matière(CCQM) established by the CIPM in 1993

• Hypothesis: Traceability of measurement results inchemistry is feasible

• Many chemists were at least rather sceptical• Clear need for comparable measurements in trade,

industry and society, traceable to common, long-term stable, references• However, traceability to SI was already claimed implicitly, but mostly not justified• Lack of measurement uncertainty statement

Ten years CCQM


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The CCQM in 1996


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• Now, after 10 years, we can state that comparability and traceability can be realized with uncertainties sufficient for intended purpose• Enormous amount of work still to be done• Still developments considerably behind compared

to the development of “classical” physical metrology• Need for setting priorities• And in cooperation with many other organizations, like WMO, WHO, IAEA, IFCC, ISO, ISO REMCO, ILAC, IUPAC and CITAC

Ten years CCQM


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• CCQM (~60 persons, 25 countries)• CCQM WG’s (~140 persons, many institutes)

• Organic analysis NIST (USA)• Inorganic analysis LGC (UK)• Gas analysis NMi-VSL (Netherlands)• Electrochemical analysis SMU (Slowakia)• Bio-analysis LGC/NIST (UK/USA)• Surface analysis NPL (UK)• Key Comparisons and CMC Quality NRC (Canada)

CCQM and its Working Groups


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• Areas covered:• Health• Food• Environment• Advanced materials• Commodities• Forensics• Pharmaceuticals• Bio-technology• Surface analysis• General analytical applications

CCQM and its Working Groups


11• Studies (~60 studies on development, try-outs, etc.)• Key Comparisons (~50 Key Comparisons)• Underpinning claimed Calibration and Measurement Capabilities – CMC’s of the NMI’s and other designated institutes• Harmonization (methods, measurement uncertainty)• Certified Reference Materials• Know-how transfer

CCQM activities


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• Cholesterol, glucose, and creatinine in serum• Organic contaminants in tissue• pp’-DDE in corn oil and fish oil• PCB’s in sediment• Ethanol in aqueous water• LSD in urine• Drugs of abuse in urine• Purity studies• NMR studies• Organic solutions of PAH’s, PCB’s and pesticides

CCQM WG on Organic Analysis


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• Calcium in serum• Arsenic in shellfish• Lead, copper, cadmium, zinc in wine• Cadmium and zinc in rice• Metals in synthetic food digest• Lead and cadmium in natural water and sediments• Minor elements in steel• Constituents in aluminium alloy• Di- and tributyltin in sediment• Sulphur in fuels• Elemental solutions

CCQM WG on Inorganic Analysis


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• CO, CO2, NO, SO2 in nitrogen• Automotive gases (CO, CO2 and C3H8 in nitrogen)• Natural gas (C1 – C6, He, N2, CO2)• Benzene, toluene, xylene in nitrogen and air• VOC’s in air• Greenhouse gases at ambient levels• Ozone at ambient levels• Ethanol in air• Reactive gases at ambient levels• SF6 and CFC’s in nitrogen• Measurement uncertainty < 1%, approaching 0.001%

CCQM WG on Gas Analysis


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• Addressing metrological issues in biotechnology and molecular biology• Work distinguishes between nucleic acid/gene, protein and cell measurements• Quantitative DNA analysis important in food testing, clinical and therapeutic measurements and forensics (DNA fingerprinting)• Instrument manufacturers and users require traceability and calibration• Internationally comparable and traceable measurements required by EU IVD directive

CCQM WG on Bio-Analysis


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• DNA profiling• DNA primary quantification• Peptide/protein quantification in proteomics• PCR quantitation study• Fluorescent dyes spectral correction studies• Bio-molecular gene, protein and cell measurements

CCQM WG on Bio-Analysis


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• Developments in nanotechnology, semiconductorindustry and industries producing and working withthin layer technologies are highly dependent on

proper surface measurements• These industries include polymers, coatings and paint, and measurements dealing with corrosion for

aerospace, protein adhesion and toxicity for bodyimplants

• The industries have asked NMI’s to address the metrological problems in surface analysis

CCQM WG on Surface Analysis


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CCQM WG on Surface Analysis

• Dopant distribution in silicium• Fe-Ni and Co-Pt alloy thin-film composition• Coatings• Surface layers, contaminants• Polymer surfaces• Thin-film multilayer systems


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Key Comparisons and CMC Quality

• Composed of representatives/experts of the Regional Metrology Organizations (RMO’s) and of experts from all CCQM Working Groups• Coordination of Key Comparisons• Defining gaps between the CMC’s of the NMI’s,

as claimed under the CIPM MRA, and the demonstration of competence and capability by the results of Key Comparisons and Studies• Discussion on unsolved questions concerning CMC’s• Defining criteria for claimed CRM’s


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CCQM and Certified Reference Materials

• NMI’s deliver traceability to customers through their calibration/chemical analysis facilities and through sales of Certified Reference Materials• Appendix C of the CIPM MRA lists these possibilities• CRM’s are widely used by customers for calibration

and method validation• Quality of claimed CRM’s to be based on NMI’s

own competence and capabilities to characterize (stability, homogeneity, etc.) and to assign a value tothe CRM in compliance with ISO Guide 34


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• Need for special CRM’s, in particular matrix materials, is almost infinite• NMI’s to develop calibration/chemical analysis capabilities• NMI’s to certify and deliver very pure materials• Commercially available CRM’s often lack traceability and measurement uncertainty statement• Great difficulties for laboratories seeking accreditation according to ISO 17025 or ISO 15189

in the field of clinical laboratories• Cooperation with ISO REMCO, IAGRM

CCQM and Certified Reference Materials


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• Accurate measurements traceable to SI, being long-term stable, fixed anchor points are essential for

several fields• WMO programmes require highest achievable levels• Comparability and traceability high on the agenda

of the clinical and in-vitro diagnostics community• If traceability to SI is not (yet) possible, then traceability to other internationally agreed references

(for example WHO units for biological activity)

Cooperation with inter-governmentaland international organizations


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CCQM has established cooperation with:

• WMO World Meteorological Organization• WHO World Health Organization• IFCC International Federation of Clinical Chemistry• IAEA International Atomic Energy Agency• IRMM EU Institute for Reference Materials & Meas.• ISO REMCO ISO Reference Materials Committee• CITAC Internatl.Coop. on Traceability A. Chemistry• IUPAC Internatl. Union Pure and Applied Chemistry

Cooperation with inter-governmental and international organizations


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• Established by BIPM, IFCC and ILAC• In cooperation with all stakeholders• Regulators, industry associations, quality assurance

and proficiency testing providers, documentary standards organizations, WHO and WHO laboratories• Aim of JCTLM is to realize and support worldwide

reliable comparability and traceability of measurement results in laboratory medicine

Joint Committee on Traceability inLaboratory Medicine - JCTLM


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• EU Directive on In Vitro Diagnostic medical devices requires traceability of calibrators to standards of “higher order”• Traceability to SI, but if not (yet) possible to

other internationally agreed references (e.g.WHO units for biological activity)

• World market for IVD products ~20 billion €per year

• Potential savings in health care > 20 billion US $per year



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• JCTLM Working Group 1 on Reference Materials is reviewing reference materials nominated as being of “higher order”• JCTLM Working Group 2 on Reference Laboratories is developing criteria for referencelaboratories• JCTLM WG 1 will work in close cooperation

with the CCQM



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• JCTLM Working Group 1 has eight sub-groups:• Electrolytes (calcium, chloride, potassium, etc.)• Enzymes (AST, amylase, CK, GGT, etc.)• Metabolites, substrates (cholesterol, urea, etc.)• Proteins (albumin, troponin-1, PSA)• Nucleic acids (DNA, RNA)• Drugs (digoxin, lithium, etc.)• Hormones (cortisol, estriol, testosterone, etc.)• Coagulation factors

JCTLM Working Group 1


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JCTLM Working Group 1 new sub-groups:

• Blood grouping and typing• Blood gases• Infectious diseases• Non-electrolyte metals• Vitamins

A database of reference materials of higher orderwill be published by the BIPM and the IFCC

JCTLM Working Group 1


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CCQM will liaise also with:

• Codex Alimentarius Commission of the FAOand the WHO

• World Anti-Doping Agency – WADA• Pharmacopeia• And others where relevant

New networks


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Good knowledge of material properties isindispensable in to-day’s industry and society

• CRM’s• Optical filters• Heat transfer coefficients• Viscosity

Ad Hoc Working Group on Viscosity has carried outcomparison, organized by PTB and CannonInstrument Company, demonstrating good agreementwithin 1% to 0.1% uncertainty

Material properties


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CCQM General issues

• Joint CCQM working group meetings contribute tocross-fertilization, know-how transfer,

harmonization, avoiding duplication, right experts doing the right things• CCQM workshops and thinkshops have been and

will be held on:“Primary methods” and on “how far does thelight shine?”Measurement uncertaintyTraceability in general and special fields

(clinical)Traceability in food analysis (November 2003)


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Many NMI’s do currently not have broad expertisein metrology in chemistry

• Trade, industry and society need to be served in an effective and efficient at short notice

• Designate other national institutes and laboratories with special expertise as an NMI for certain quantities and measurement ranges, so they can participate in the CIPM MRA

Designated institutes


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• Guarantee a level economic playing field andtreat customers on an equal footing in the casethat a commercial organization is being

designated to act as an NMI in a certain field• Most NMI’s do not have expensive facilities

like a reactor for instrumental neutron activation analysis (INAA)• If INAA is needed it is recommended to make

use of available reactors in the country concerned

Designated institutes


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BIPM wants to be able to assist the chemicalcommunity in the development of traceability andcomparability concepts:• BIPM started with a small group on Gas Analysis, focusing on ozone measurements• In 2003 the CCQM advised unanimously that the chemistry section of the BIPM should add a small activity on purity analysis in the field oforganic and clinical chemistry• This programme has been and will be tuned with the IFCC and the NMI’s

BIPM and Metrology in Chemistry


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Good progress has been made; still several issueshave to be addressed:• Education on metrology in chemistry, including

the understanding of traceability and measurement uncertainty• Definition of the measurand• Method-dependent measurement results• Matrix problems• Commutability in clinical and therapeutic measurements• Non-SI traceable measurement results• Traceability chain via CRM’s

Conclusions


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The CCQM in 2002

Documents

World Structure for Metrology in Chemistry (CCQM) · PDF file15/01/04 NMi - the Art of Measurement 1 World Structure for Metrology in Chemistry (CCQM) Ed W.B. de Leer, Robert Kaarls