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Foreword by the Chairman: CITAC Strategy for 2007-2010

thanks for their contributions over the years and at CITAC and for the trip, and not CITAC itself? their involvement in CITAC activity. I wish them Why is CITAC necessary at all? Even if such the best for their future endeavors! questions are natural, they were unexpected for me before the meeting where I planned to start I would also like to thank my predecessor, Dr. my CITAC Chairmanship (I rather expected to Vera Ponçano (2004-2007), Instituto de Pesquisas hear compliments - but life is life). Tecnologicas, Brazil, for her warm, heartfelt attitude towards every CITAC member during My answers were: her term as chairperson, especially at the IV - Really, CITAC is a voluntary organization Metrochem, and Dr. Laurie Besley, the National active in the field of scientific and applied, not Metrology Institute of Australia, past CITAC legal metrology. However, participation in the Honorary Secretary, for his humor, optimism and Metre Convention and in the International help in discussing and overcoming problems. It Organization for Standardization, for example, is a subject of pride for CITAC that Vera was able is also voluntary. Decisions and documents I am honored to have been elected the CITAC to prepare at this time her Ph.D. thesis “Network of such organizations are not obligatory, but Chairman and grateful to my colleagues for their Organization in Chemical Metrology” and to they are helpful, as a rule. In particular, guides confidence. These were the first CITAC elections defend it successfully on 1 November 2007 at the for analytical (testing) laboratories developed when voting was organized electronically by e- University of São Paulo, Brazil. Congratulations, with CITAC participation are useful for the mail. In spite of the virtual system of elections, I Vera! laboratories and their accreditation bodies, as am entirely approachable, and anybody who was well as for users of the laboratory measurement interested in testing this could shake hands with It is my pleasure as well to congratulate the (analytical/test) results. me after the adoption of the voting results at the first CITAC award winners, authors of the most - Of course, website graphics depend on the 22nd CITAC Members Meeting, July 17, 2007, São interesting/important papers on metrology in money invested, but the value of the CITAC Paulo, Brazil, at the IV International Congress on chemistry by CITAC version 2007: Dr. David website is to be assessed by its scientific, Chemical Measurement Traceability and Quality L. Deuwer, National Institute of Standards professional chemical/ metrological content. Assurance (IV Metrochem). and Technology, USA, Dr. Bertil Magnusson, - The CITAC budget is based on membership Swedish National Testing and Research Institute, payments only. I am pleased that the following officers were and his co-authors from NORDTEST, and Prof. - I am proud that the CITAC members are my elected at the same time: Venkatesh Iyengar, Tufts University, USA. More friends. However, it should be taken into account - Dr. Wynand Louw, the National Metrology details can be found in the message from Dr. that CITAC members were elected as leading Institute of South Africa, as Vice-Chairman and Wynand Louw, the Award Coordinator, and in specialists in metrology in chemistry, and their CITAC Award Coordinator; the papers of the award winners. contributions are known internationally. - Dr. Philippe Charlet, the Laboratoire National de Metrologie et d'Essais, France, as Secretary As a government employee, I cannot attend any I also explained the CITAC’s aims. In the end, the and CITAC News Editor; and meeting abroad without permission from a special trip was approved. - Prof. Dr. Wolfhard Wegscheider, the Leoben committee for business trips at the Ministry I returned to these questions after the trip to University, Austria, as Treasurer and CITAC guiding the National Physical Laboratory of Israel formulate with CITAC members our strategy for Website Administrator. (INPL). Discussing my request to take part in the 2007-2010. The draft strategy prepared using What more could any chairman dream of than 22nd CITAC Members Meeting in conjunction email communication is available at the website working with so qualified and capable a team? with the IV Metrochem, one of the members of www.citac.cc (page "About CITAC") and in the the committee for trips said that in his opinion present CITAC News issue, p. 37. This draft will Dr. Koichi Chiba, National Metrology Institute of CITAC is not such an important organization: be further discussed at the 23rd CITAC Members Japan, Prof. Venkatesh Iyengar, Tufts University, 1) he can also establish an “international forum” Meeting (in conjunction with the CCQM USA, and Dr. Chainarong Cherdchu from the with his friend from USA by internet whenever meetings in Paris, 3o March 2008). Therefore, National Metrology Institute of Thailand were he wants; 2) his “international forum” website at this time I would like to invite CITAC News elected as new CITAC members. This favorable decorated with graphic art and a video (with readers to contribute to improving the strategy addition comes after the resignations of Mr. pretty girls) will be richer than the CITAC and to the realization of CITAC’s goals. John Hammond, Optiglass Ltd., UK, because of a website; and 3) decisions of his “international change in his field of activity, and by Dr. Kensaku forum” will not be obligatory for laboratories Dr. Ilya Kuselman Okamoto, National Metrology Institute of Japan, and institutions as the CITAC decisions are. Why CITAC Chairman due to his retirement from the Institute. Many should the Ministry pay for activity of its employee INPL, Israel

CITAC NEWS ● FEBRUARY 2008 TTableable ooff ContentsContents CCITACITAC NNewsews

Foreword by the Chairman: CITAC Strategy for 2007-2010 / I. Kuselman ...... 1

Editorial: The 22nd CITAC Members’ Meeting in São Paulo, July 17, 2007 / P. Charlet ...... 3 CITAC News published by: Laboratoire National de Métrologie et d'Essais / W. Louw ...... Message from the Vice Chair 4 (LNE) Message from the Past Chair / V. Ponçano ...... 4 29, avenue Roger Hennequin 78197 TRAPPES Cedex Reports of International Organizations France ● An Update on the CCQM Activity in 2007 / R. Kaarls ...... 5 Tel +33 1 30 69 21 95 ● ILAC Update for CITAC News 2008 / A. Squirrell ...... 7 ● IMEKO Technical Committee [TC-23] on Food and Nutritional Metrology / V. Iyengar ...... 9 Fax +33 1 30 69 12 34 ● EURAMET METCHEM Activity in Metrology in Chemistry / P. Charlet ...... 10 E-mail [email protected] ● Bayesian Statistics to Improve Reference Values in Metrology in Chemistry: ...... 12 an ERANET-Plus Project / S. Demeyer, P. Charlet ● APMP Activity Report 2007 / L. Samuel ...... 14 Internet: http://www.citac.cc ● SADCMET Amount of Substance Annual Report to CITAC 2007 / W. Louw ...... 15 ● Report from SIM / Y. Mitani ...... 18 Internet administrator: ● Sampling – Validation, Quality Control and Uncertainty Estimation / C. Grøn ...... 19 ● Measurement Uncertainty Revisited: Alternative approaches to uncertainty evaluation ...... 22 Wolfhard Wegscheider, / B. Magnusson University of Leoben, Austria ● Information from the EuCheMS Division of Analytical Chemistry / J.E.T. Andersen ...... 23 Award Winners 2007 Newsletter Editor: ● CITAC Most Interesting/Important Papers on Metrology in Chemistry 2007 / W. Louw ...... 24 Dr Philippe Charlet, France ● How to Combine Results Having Stated Uncertainties: to MU or not to MU? / D.L. Duewer.. 25 ● Nordtest Handbook for Calculation of Measurement Uncertainty based on Quality Control ... 27 and Method Validation / B. Magnusson, H. Howind, M. Krysell, T. Naykki Newsletter designed and produced by: ● Metrological Concepts for Enhancing the Reliability of Food and Nutritional Measurements .. 30 Aryeh Lewis / V. Iyengar ISAS International Seminars Meeting Reports P.O. Box 34001, Jerusalem 91340 ● IV International Brazilian Congress on Chemical Measurements, Traceability and ...... 31 Israel Quality Assurance / V. Ponçano Tel: +972 2 6520574 ● Workshop on Sampling Validation, Quality Control and Uncertainty Estimation / C. Grøn .... 32 ● The 1st International Proficiency Testing Conference, Romania 2007 / G. Guslicov ...... 33 Fax: +972 2 6520558 ● BERM 11 – 11th International Symposium on Biological and Environmental Reference ...... 33 e-mail: [email protected] Materials / K. Okamoto Announcements ● The Revised VIM is Out / P. De Bièvre ...... 35 No liability is accepted for the ● Symposium: Advances in Understanding-Chemical Measurement Quality / B. Magnusson .. 35 accuracy of the information ● The 17th International Conference of the Israel Society for Quality / I. Kuselman ...... 35 ● 6th Workshop on Proficiency Testing in Analytical Chemistry, Microbiology ...... 36 and the views expressed are not and Laboratory Medicine / B. Brookman necessarily the official policy of the CITAC Working Group CITAC Strategy for 2007-2010 (draft) ...... 37 members’ institutes or national Messages from New Members governments. ● Venkatesh Iyengar ...... 38 ● Chainarong Cherdchu ...... 38 For additional copies of the ● Koichi Chiba ...... 38 CITAC News, please contact the CITAC Members’ List ...... 39 newsletter editor.

● 2 / / CITAC CITAC NEWS NEWS ●FEBRUARY FEBRUARY 2008 2008 EEditoriald i t o r i a l The 22nd CITAC Members’ Meeting in São Paulo, July 17, 2007

were adopted. It was decided to include in the CITAC is also continuing to present its activities Agenda of the 23rd CITAC Members' Meeting worldwide with involvement planned for April oral reports of the liaison officers, taking into 2008 in Berlin (Workshop on Uncertainty in account the importance of the information Sampling and in Compliance Assessment) and conveyed by the officers. in Paris (the CITAC 23rd Member’s Meeting in conjunction with the CCQM meetings), in May The Terms of Reference of CITAC have been in Athens (EURACHEM GA and Workshop revised and the updated version was accepted on Education and Training), in October in during the meeting. These Terms of Reference Rome (Workshop on Proficiency Testing), will be the base for the development of the and in November in South Africa (Test and CITAC Strategy Plan 2007-2010 presented in this Measurement Conference). CITAC also CITAC News issue by Dr. Ilya Kuselman. plans to take part at the Joint Committee on Traceability in Laboratory Medicine (JCTLM) Reporting on CITAC activities, Dr. Kuselman in Fortaleza, Brazil. The policy paper related to In July, only eight members assembled in Hotel informed members about the recently the procedure for CITAC to highlight important Feller, near the most famous avenue of São published EURACHEM/CITAC guides “Use of papers in metrology in chemistry was adopted. Paulo,Brazil to conduct the 22nd CITAC Members’ uncertainty in the assessment of compliance” Finally, Dr. Ilya Kuselman, the new Chairman, Meeting and enjoyed the pleasant Brazilian and “Estimation of measurement uncertainty expressed gratitude to Mrs. Vera Ponçano for wintertime. Members came from very different arising from sampling”. He asked members to her contribution by enlightening the vision of parts of the world, from Finland, USA, Russia, be more active in development of the guides CITAC’s Mission during the past three years and Israel, South Africa, France, Czech Republic “Assessing performance in qualitative analysis”; the hope that Vera will continue her activity as and, of course Brazil. We were very honored “The fitness for purpose of analytical methods: the CITAC Past-Chair. to also have Dr. Alejandro Herrero, Director of a laboratory guide to method validation and IRMM (EU, Belgium), as observer. The meeting related topics” (revision); and “Selection and Functioning also as the CITAC News Editor preceded the IV International Congress on use of proficiency testing schemes for a limited I would like to draw your attention to the Chemical Measurement, Traceability and Quality number of participants”. These guides, currently contents of this issue. As usual, the reports Assurance (IV Metrochem) on July 18th- 20th in being developed, demonstrate the strong of international organizations and regional São Paulo. emphasis of CITAC on the dissemination of the metrology organizations are presented but you concepts of metrology in chemistry throughout will also find the full text of the awarded “most After the welcome words from the Chair, Mrs. industry and society. interesting papers on metrology in chemistry in Vera Ponçano, the agenda was adopted and the 2007”. European NMIs have been fully involved in minutes of the previous meeting were accepted. Furthermore, in order to arouse attention 2007 in the elaboration of joint research projects The results of the election of CITAC officers and input of the CITAC members regarding in the framework of iMERA (Implementation and new members, as well as resignations are the development of the guides, it was decided of Metrology in the European Research Area). described in the Foreword by Dr. Ilya Kuselman, to include in the agenda of the next CITAC A paper related to a selected project, in the the new Chairman. Members' Meeting oral reports of the CITAC Targeted Program “Health”, on the new approach representatives who are involved in the Working of Bayesian statistics to improve reference values The financial report indicated that a limited Groups developing the guides. in metrology in chemistry is also presented in number of members are currently paying their this issue. annual fees. Therefore, there is a clear need to The CITAC procedure for nomination and explain, particularly to less motivated members, awarding the most interesting/important papers Meeting reports and announcements of why CITAC is unique as a facilitator of contacts by on metrology in chemistry was adopted. Dr. upcoming meetings on metrology in chemistry disseminating traceability information. In order Wynand Louw, the new CITAC Vice-Chairman are also included. May I draw your attention on to get more flexibility, a proposal from the Chair and Award Coordinator, was asked to initiate the MEFNM 2008, The International Conference was adopted to establish a new membership the first round of the procedure already in the payment, a collective one for organization, current year. on Metrology of Environment, Food and institution or company. The “collective” member Nutrition Measurements, to be held in Budapest could appoint his representative having a specific Dr. Kuselman stressed that it is important next year. This conference will join the activities expertise. On the whole CITAC is financially sound. for CITAC, as an international organization of three IMEKO technical committees and two active in the field of metrology in chemistry, to of them, Food and Nutrition, and Chemical The liaison reports by Dr. Laly Samuel (APMP), support the journal "Accreditation and Quality Measurements are chaired by CITAC members Dr. Robert Kaarls (CCQM), Dr. Wynand Louw Assurance. Journal for Quality, Comparability (Venkatesh Iyengar and myself). (SADCMET), Dr. Yoshito Mitani (SIM), Mr. Alan and Reliability in Chemical Measurement" The updated list of CITAC members is available Squirrell (ILAC) and Dr. Willie May (JCTLM) have (ACQUAL), in the same way that a number of at the end of this issue. been received electronically by the members. chemical societies support the “Analytical and The reports and the draft guidelines for CITAC Bioanalytical Chemistry” journal. This will be liaison officers which were circulated before the of particular major importance when ACQUAL Dr. Philippe Charlet meeting and discussed by e-mail and included changes its sub-title to "Journal for Metrology CITAC Secretary the updated list of the CITAC liaison officers, and Quality in Chemistry" or similar. LNE, France

● CITACCITAC NEWS NEWS ● FEBRUARY FEBRUARY 2008 2008 / / 3 MMessageessage ffromrom tthehe VViceice ChairChair

Since its official inception a little more than a Being the Vice-Chair of CITAC not only creates decade ago, metrology in chemistry spread its the opportunity to make a contribution to the wings over the entire world; huge strides were international goals of CITAC, but also paves the way made in bringing the concept of metrology to further the activities of CITAC in Africa. This is to each country especially in the developing especially important in the next year or two with the countries. More importantly, documents and recent establishment of the Intra-Africa Metrology traceability solutions must reach each and every System (AFRIMETS) where CITAC can play a role accredited (and other) analytical and testing to distribute metrology related documents in an laboratory. I believe that it is in this important easily accessible location and form. May I also, in final frontier of analytical chemistry that CITAC my capacity as the AFRIMETS Chairperson (on can play a vitally important role to disseminate, behalf of my NMI and African colleagues), wish interpret and assist to implement the advances in CITAC a fruitful and productive 2008. traceability in metrology in chemistry being made at the NMI level. Dr. Wynand Louw Vice-Chair, CITAC NMI, South Africa MMessageessage ffromrom tthehe PPastast CChairhair Metrochem IV, a high level congress supported national institutions has a relevant role. With this by CITAC and BNCM members. During my in mind, I decided to develop a study for my PhD professional career it became more evident at the University of Sao Paulo, concluded in 2007, how important it was to work in a partnership with a focus on the Organization and Management mode where one could get together results of of Laboratory Networks. common interest and act in a complimentary way which increases knowledge through interacting This research focused on identifying the benefits with each colleague and institution involved in the and increasing the amount of understanding work being developed. It has been a great way to associated with operation and performance of a advance in providing relevant technological tools for network system focusing on chemical metrology. the community and country. Particularly in chemical Its development comprised the identification metrology, it provides relevant metrological tools of factors of influence and dimensions of for laboratories to get quality results and generate improvement. The experimental research was confidence and safety for society. conducted through a multiple case study that Usually a compass identifies directions and included national and international experiences ensures that one knows his/her location and/or Having clearly developed these concepts and developed through interviews and questionnaires stays on a pre-defined course. It is important in using the opportunity of this environment, it with 33 senior researchers from the Brazilian life to have a compass in order to know where became a challenge to study in depth subjects Network for Chemical Measurements (formerly you are going, to set your priorities and goals and related to management and relationships between the Brazilian Program on Metrology in Chemistry) to be totally focused on a cause while trying to institutions with focus on common interest, in and 58 managers of chemical metrology area function in the middle of a myriad of situations an academic way. I remember a dear friend who from 54 institutions in 46 countries that were that appear daily. These perturbations demand insisted that I go ahead with my PhD; he said it mainly signatories to the Metre Convention. our attention, while many times taking us off the would be like flying in another dimension where I The conclusion was that cooperative actuation “North” course that was originally set. So, to exist could see the whole thing, having the relationship like networks are especially beneficial because in this life routine one needs a compass that will of each part better defined... and that was what of the diversity of current demands for chemical hold the preset direction or priorities intact. To happened. metrology. In a network, these demands can set these priorities we need to know what matters be resolved with less investment, in a timely most in life, our personal values. One needs to So, three and half years ago it became another manner, using national specialists and equipment, reconfirm the direction and be sure about the priority, developed in conjunction with all the and following global standards. However, goals that were set. In this way I tried to define my other activities in my life. Even with a harmonic management of such a network system requires day by spending time on issues that would provide compass, melody and faith it was not easy to carry careful monitoring of all factors that effect its intense personal and professional pleasure. But this on all issues under my responsibility and become performance and maintenance, including those was possible only now, at this time in my life, since a student again after such a long time. There were factors needed for its improvement. Future my four children have grown up and are going their no weekends, a mixture of day and night, notes researchers are needed to validate these results, own individual ways. and observations were constant companions. But applying them to other network systems. In the primary direction to travel, the North, was addition, complimentary studies should be done My initial course of direction was my work at always there and I was fixed on reaching this point to identify the “weight” of the influencing factors IPT as Director for Metrology in Chemistry without deviating or stopping. The participation to networks and their relation using mathematical and Coordinator for International Affairs. of friends and colleagues was fundamental in models such as modeling techniques. Also Simultaneously I was coordinating a Brazilian stimulating and providing the best information practical experiences like the ones presented in Network for Chemical Measurement Laboratories for this work. this study can be applied in the development of (BNCM) which today is comprised of colleagues theories like the Actor Network Theory. from 47 technology institutions and universities The dissemination of chemical measurement from 12 Brazilian states; this was in addition traceability at the national level is a concern and Dr. Vera Ponçano to CITAC activities that brought a stimulating an important task for managers with this kind of CITAC Past Chair input for the development of activities like the responsibility. In this context cooperation among IPT, Brazil

● 4 / / CITAC CITAC NEWS NEWS ●FEBRUARY FEBRUARY 2008 2008 RReportseports ooff InternationalInternational OOrganizationsrganizations An Update on the CCQM Activity in 2007

The interest of NMIs and other (potential) should be handled. The CCQM concluded that It has resulted in the creation of two ad hoc Designated Institutes to participate in the a careful approach will be needed that would CCQM Working Groups: activities of the CCQM and its working groups has lead to a considered opinion. The CCQM agreed ● the KCRV and Its Uncertainty, chaired continued to increase. Inasmuch as metrology on Recommendation CCQM 1 (2007) “On by Prof. M. Cox, NPL; in chemistry is increasingly recognized to be of the possible redefinition of the mole and the ● Efficient Testing of Claimed CMCs, chaired by high importance for the quality of life and the kilogram”. Dr. G. Turk, NIST. economy (export) of countries we still expect The ad hoc working groups will report back a further increase of the activities in the field of Further the CCQM established a working group in April 2008 to the CCQM. In the meantime metrology in chemistry. on the redefinition of the mole chaired by Dr. M. interesting and creative discussions within the Milton. Other members are Dr. L. Besley, Prof. CCQM Working Groups concerned are taking The CCQM has met on 19-20 April 2007 de Bièvre, Dr. Marc Salit and Dr. R. Wielgosz. place. at the BIPM. As usual the meeting was The CCQM will cooperate with the IUPAC attended by more than 70 persons of about Commission on Isotope Abundance and Atomic The CCQM Working Group on Organic 45 organizations, not only representing NMIs Weights (CIAAW) and the International Avogadro Analysis reported results of key comparisons and other Designated Institutes, but also Coordination (IAC). The issue will be discussed and pilot study comparisons on: representing intergovernmental organizations again at the next meeting of the CCQM in 2008. ● volatile organic compounds (VOCs) in a and international bodies, like the IAEA, WMO, solution of methanol Codex Alimentarius Commission, IFCC, ILAC, CCQM Working Groups ● ethanol in aqueous matrix JCTLM, WADA, AOAC International, CITAC, All CCQM working groups reported about the ● cortisol and progesterone in human serum IUPAC, ISO, ENGL (European Network of GMO work carried out over the period 2006-2007. ● nutrients in infant formula testing Laboratories) and CropLife International At this very moment about 108 Pilot Study (association of multi-national GMO producers). comparisons and 67 Key Comparisons have been The excellent results obtained in a pilot study on Due to illness a contribution by the representative carried out, are in progress or are planned for 19 - norandrosterone, carried out in cooperation of the ENFSI (European Network of Forensic the near future. This is an increase of about 15% with the WADA was published. This drug belongs Science Institutes) had to be cancelled. compared to a year ago. This again demonstrates to the group of second most abused anabolic the rapidly growing interest in reliable, steroids. A next comparison in cooperation with All seven CCQM Working Groups met during comparable and traceable measurements in WADA is being prepared. the days before the meeting of the CCQM. The chemistry by a growing community representing meetings of the CCQM and its working groups all areas of trade, industry and society. In Work in progress includes VOCs in solution and were also attended by representatives from addition, several Key Comparisons are followed PCBs in mussel tissue. Future work will include the NIBSC (WHO) and the US pharmacopoeia up by a subsequent Key Comparison under the study comparisons on theophylline and digoxin, (USP). Both organizations contributed actively same code number, or are repeated by a RMO as malachite green in fish, residues of veterinary to the work in the BAWG and the OAWG. a RMO Key Comparison. Also, the RMOs are now drugs, apple juice spiked with pyrethroids, The CCQM Working Groups on Organic Analysis, organizing more supplementary comparisons. acrylamide in potato chips and organic Inorganic Analysis, Gas Analysis Electrochemical components in alcoholic drinks. The work by the Analysis and Bio Analysis also met during the In order to limit the number of Key Comparisons BIPM in taking a leading role on purity analysis second half year of 2007. as much as possible and to work in the most (theophylline) has been well received. efficient and effective way, the CCQM and its The following are the points discussed and working groups have started a study on how The CCQM Working Group on Inorganic activities carried out. use can be made of the results of pilot study Analysis reported results of key comparisons Redefinition of the Mole comparisons and how we can best test the and pilot studies comparisons on: The CCQM is of the opinion that there are no capabilities and competences of the NMIs ● Pb, Fe, Cu and Cd in wine fundamental objections with regard to a re- and other designated institutes by testing ● Toxic elements in bovine liver definition of the mole based on a fixed value for more generally the competences and available ● stable isotope delta values the Avogadro constant. Such a change would capabilities (techniques and procedures) in the ● As, Hg, Se and methyl-mercury content in not yet have any effect at the practical level of institutes. marine fish chemical measurements and measurement ● Assay of chloride content of KCl uncertainty. However, it should be ensured CCQM Workshop ● Total Se and Se-speciation analysis of Se- that any possible modifications to widely-used A CCQM workshop on calculating the KCRV rich wheat flour. equations was communicated clearly, so that and its uncertainty and new approaches to a Other comparisons are in progress: the large number of scientists who depend on more efficient and effective way of testing the ● analysis of copper alloy (key comparison) measurement results expressed in amount of capabilities and competences of NMIs and other ● trace elements in phosphogypsum substance units are clear as to how any change DIs has been held on 18 April 2007 at the BIPM. ● Sr isotopic ratio measurements

● CITACCITAC NEWS NEWS ● FEBRUARY FEBRUARY 2008 2008 / / 5 RReportseports ooff InternationalInternational OOrganizationsrganizations

● Cd, Cr, Hg, Pb in poly propylene (plastics) Work on measuring the salinity of ocean water purity analysis of theophylline was successful. for the EU RoHS Directive is being prepared in order to improve the Work is now underway on digoxin and steroid ● Purity of zinc metrological traceability of these measurements. hormones. In close cooperation with the This is also a EURAMET project lead by the PTB OAWG the BIPM will coordinate a series of key A workshop on Neutron Activation Analysis Presentations have been made on the potential comparisons covering a wider field based on as a primary method has taken place. NAA has for stripping voltammetry to perform as a a model on “molecular weight versus polarit been added to the short list of potential primary primary method and activity measurements in space”. methods in metrology in chemistry. complex mixtures. The BIPM QM-K1 is an on-going key comparison The CCQM Working Group on Gas Analysis The CCQM Working Group on Surface of ozone. Standard reference photometers have reported results of key comparisons and pilot Analysis reported results on: been upgraded with kits from NIST. study comparisons on, carbon dioxide in air, ● silicon dioxide on silicon (key comparison) Comparisons of NO in nitrogen carried out by oxygen in nitrogen and hexane in methane. ● C and N concentrations in coatings on steel the BIPM have delivered very good results with Proposed comparisons include: ● C in bulk steel noticeably improved uncertainties for analytical ● Purity of methane ● Nitrogen concentration in a “diamond-like” values. ● Mercaptans in methane (odourisation of carbon film natural gas) ● Fe-Ni concentration in alloy films on silicon JCTLM ● In carrying out the key comparison different Stack emission gases (NO, SO2, CO, CO2, Work in the scope of the JCTLM was reported by propane in nitrogen) technologies have been applied, delivering Dr. W. May, chair of the JCTLM Working Group ● Species at trace levels typical of different results. Investigations have identified 1 on Reference Materials and Methods of Higher environmental measurements the existence of an effect in some results due to Order, and Prof. L. Siekmann, chair of the JCTLM ● Reactive species. the existence of hydrocarbon and water layers on Working Group 2 on Reference Measurement the samples (ultra-thin surface contamination). Laboratory Services and inter-laboratory Further, the collaboration with the WMO Global The work of the SAWG group will be extended to comparisons. WG 2 is organizing series of Atmospheric Watch programme (WMO GAW) encompass work on organic layers on surfaces. regular inter-laboratory comparisons. The has been reported. The WMO GAW has now also results of laboratories listed with their services in requested that the CCQM Working Group on The CCQM Working Group on Bio Analysis the JCTLM database are of clearly good quality. Gas Analysis takes responsibility for maintaining reported results of comparisons on quantitative Results of the inter-comparisons are available at a “scale” for atmospheric VOCs on their behalf in polymerase chain react ion (PCR) (key the web-site of the DGKL. support of the WMO VOC global network. comparison), protein structural measurements by circular dichroism, protein quantification, Up-dated lists of CRMs and measurement The CCQM GAWG has participated together quantification of DNA methylation and assay by procedures “of higher order” as well as available with the WMO GAW’s VOC group in a workshop ELISA. reference measurement laboratory services are in Garmisch-Partenkirchen, Germany. Proposed work includes: now regularly published in the JCTLM database. ● glycan species measurement in digested (www.bimp.org) The organization of a BIPM – WMO symposium glycoprotein mixture “On Metrology and Climate Change” in the ● quantification of cells with specific A discussion with the EU is continuing with spring of 2009, among others addressing green phenotypic characteristics respect to the formal recognition of the JCTLM house gases, ocean salinity and irradiation issues, ● multiplexed RNA gene-expression bio-markers database by the EU. will be very welcome. ● genomic DNA quantification The NIBSC (WHO) and the Pharmacopoeia Codex Alimentarius Commission The CCQM Working Group on (USP) are actively cooperating and participating The cooperation with the Codex Alimentarius Electrochemical Analysis reported results on in the activities of the BAWG. Commission and the Inter Agency Meeting is carbonate buffer, phosphate buffer and nitrate developing satisfactorily. Dr. Doyran from the and nitrite in calibration solutions and natural The CCQM Working Group on Key Codex Alimentarius Commission outlined the water. Comparisons and CMC Quality reported that background of the Commission and described Proposed comparisons include: now 3736 CMCs published in the KCDB database the remit of the Commission on Methods of ● electrolytic conductivity of the BIPM are related to the work under the Analysis and Sampling. The Codex Alimentarius ● pH of carbonate and oxalate buffers CCQM (www.bimp.org/kcdb). Commission is considering the application of ● assay of potassium chloride measurement uncertainty including allowance It has been proposed to also consider pH in BIPM Programme of Work for sampling uncertainty. The Codex Commission organic solutions such as bio-fuels. The BIPM programme of work has been is also assessing the safety and labelling of presented by Dr. Wielgosz. The comparison on biotechnology products.

● 6 / / CITAC CITAC NEWS NEWS ●FEBRUARY FEBRUARY 2008 2008 RReportseports ooff InternationalInternational OOrganizationsrganizations

Working Group 7 the ENGL. The ENGL laboratories operate within industry in reliable, comparable and traceable Mr. Finidori, secretary of Working Group 7 the EU Framework Directive on GMOs. This measurements. He gave an example of the (GMOs and derived products) of ISO TC 34 includes harmonization and standardization disruption of trade due to independent adoption (food products) gave an overview of work on of measurement methods and quality systems. of measurement methods and materials. DNA-based methods, protein-based methods, Sampling strategies are a hot topic. IHCP is He mentioned the importance of applying deﬁnitions and sampling strategies. also an EU Reference laboratory for GMO standardised PCR methods and the need for measurements that is also involved in method adequate CRMs. Further discussions should take ENGL validation. place in order to identify the role for the NMIs Dr. Moens from the Institute of Health and in this area. Consumer Protection (IHCP) at the EU JRC in Ispra, in his function as deputy chair of the CropLife International Dr. Robert Kaarls European Network of GMO Testing Laboratories Mr. Dana from CropLife International described President CCQM (ENGL), gave an overview of the Activities under the interest of the multi-national GMO The Netherlands

ILAC Update for CITAC News 2008

CITAC The first ILAC Executive Committee and This year, the developing country seminar ILAC has maintained its close cooperation Arrangement Committee (ARC) meetings for was held jointly in Sydney on 31st October 07, with CITAC and thus has enabled us to 2007 were hosted by COFRAC in Paris, France between ILAC, IAF and the Asia-Pacific Metrology continue our efforts in strengthening the during the first week of March. As is usual for Programme (APMP). The three organisations links between accreditation and metrology the first Executive meeting of the year, planning took advantage of the proximity and overlap (particularly in chemistry) – an essential link of the work program for 2007 was high on the between both sets of annual meetings to conduct to assist accreditation bodies and accredited agenda, with the updated work programs of this joint seminar on the topic of “Interactions laboratories in delivering traceable and reliable the Committees also being reviewed. Another between National Metrology Institutes measurement results which are fit for their standard activity for the first meeting of the year and Accreditation Bodies for Laboratories, intended use. Issues of common interest include is the review of the General Assembly Resolutions Inspection Bodies and Certification Bodies - metrological traceability, proficiency testing, and the status of those requiring action. with particular focus on issues for Developing reference materials and further applications of Economies”. UNIDO was a co-sponsor of the measurement uncertainty (including qualitative The June meetings in 2007 were hosted by CNAS seminar, as one of the partner organisations analysis) and CITAC’s input on these issues, in Beijing, China. Meetings of the ILAC and of the Joint Committee on Coordination of through their membership of ILAC’s Laboratory IAF Executive Committees, the ILAC/IAF Joint Technical Assistance to Developing Countries Committee (which is currently chaired by Committee for Closer Cooperation (JCCC), the in Metrology, Accreditation and Standardisation Dr Máire Walsh, a CITAC member) is much ILAC Arrangement Management Committee (JCDCMAS). appreciated. A general update on recent activities (AMC), the IAF MLA Management Committee within ILAC follows: (MC) and a joint session of the ILAC AMC and The ILAC Arrangement IAF MLA MC were held during this period. As of 19 June 2007, there were fifty- Terms of Reference for the operation of the joint eight Signatories (Full Members) to the sessions of the ILAC AMC and IAF MLA MC were Arrangement, representing forty-six economies. ILAC Meetings approved by each organization at the ILAC-IAF The 2006 Annual Meetings for ILAC and IAF, Joint General Assembly in Cancun in November The Inter American Accreditation Cooperation were hosted by the Entidad Mexicana de 2006. (IAAC) received formal recognition of their Acreditación A.C. (EMA) in Cancun, Mexico, Multilateral Arrangement (MLA) during from 6-14 November 2006. Representatives The 2007 Annual Meetings (ILAC and IAF) were the meetings in Cancun. This recognition of several international liaison organizations co-hosted by NATA and JAS-ANZ in Sydney, was granted following an extensive peer attended and the meetings were both productive Australia, on 19–31 October. Please visit the ILAC evaluation process that culminated in a and informative. Delegates participated in a very website for a list of the Adopted Resolutions at ballot amongst ILAC Arrangement Council full meeting schedule but were also fortunate to the ILAC General Assembly. The 2008 meeting members. The IAAC recognition is for Testing experience some very enjoyable cultural events will be held in Stockholm, Sweden, during the & Calibration and signatories to the IAAC arranged by our Mexican colleagues. period 10-22 October. MLA who are also members of ILAC, are now

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eligible to also become ILAC Full Members, members who have not as yet sought access to (sometimes more than one) have participated, i.e., Signatories to the ILAC Arrangement. the Members Area of the website, can do so on- and are scheduled to participate, in meetings ILAC now has three Recognised Regional line, via the ‘Home’ page of the website). of the CASCO CPC (Chairman’s Policy Cooperation Bodies - Asia Pacific Laboratory Committee), WG 27 (Drafting requirements Accreditation Cooperation (APLAC), European The BIPM/ILAC Accreditation Committee (AIC) for use in conformity assessment applications), Co-operation for Accreditation (EA) and Inter working group’s work on the dissemination of WG 29 (Revision of ISO Guide 65 – Product American Accreditation Cooperation (IAAC). traceability (eg Best Measurement Capability Certification), CASCO WG28 (Revision of ISO (BMC)/Calibration and Measurement Capability Guide 43 – Proficiency Testing), CASCO Plenary, ILAC continues to focus on enhancing a more (CMC)) was further progressed during the ISO TC212 (Technical Committee - Clinical widespread understanding of the benefits of recent meetings in Paris. A joint statement on laboratory testing and in vitro diagnostic test the Arrangement amongst the international the future use of CMC was recently approved systems), ISO TC 69 (Technical Committee - community, particularly governments and by both BIPM and ILAC. A metrology workshop Applications of statistical methods), ISO TC 176 regulators. was held on 9 March 07 and representatives of (Technical Committee - Quality Management the Regional Accreditation Cooperations and and Quality Assurance) and the IAF, ILAC and Joint ILAC/IAF Activities Regional Metrology Bodies once again shared ISO Joint Working Group. The joint activities between ILAC and IAF ideas on the topics of common interest to the continue to be managed through the Joint accreditation and metrology communities. ILAC was also actively represented at ISO Committee for Closer Cooperation (JCCC). Further meetings are scheduled for March REMCO (reference materials) which met in Currently operating under the stewardship of 2008. Tsukuba, Japan on 5-8 June 2007 and the this committee are the following: APLAC Workshop on reference materials held in conjunction with this ISO REMCO meeting. The ● Joint Working Group for Inspection (JWGI); A meeting of the CCQM (Consultative Committee meetings focussed on the review of ISO Guide ● Joint Development Support Committee on Amount of Substance – Metrology in JDSC); Chemistry) was held in April 07 – and this 34 General Requirements for the competence of reference material producers.. ILAC and ● Joint Working Group on Maintenance of A- included developments in Proficiency Testing Series Documents; and Reference Materials. ILAC was represented its Regional Cooperation Body members are continuing to contribute to the revision of this ● Joint Working Group on Training of Peer at meetings of the Joint Committee on Evaluators; Traceability in Laboratory Medicine (JCTLM) in important guide together with other related work on reference materials. ● Joint Working Group on Guidance for ISO/ Paris in December 2006 and is very active in the IEC 17011:2004; accreditation of medical laboratories. ILAC has also continued its cooperation with ● Joint Meetings of the ILAC Arrangement Management Committee (AMC) and the ILAC’s continuing close cooperation and liaison various ISO technical committees - eg TC 176 IAF Multilateral Arrangement Management activity with EURACHEM and CITAC supports (ISO 9000 series), TC 69 (Statistical Methods), TC 34 (Food Safety) and ISO TC212 (Medical Committee (MLA MC); these important metrological initiatives in Testing). ● Joint Working Group on Communications. chemical and biological measurement including Each of these Joint Working Groups reports on work on method validation, measurement ILAC and the World Anti Doping Agency (WADA) their work programs and progress at the Joint uncertainty and compliance with limits, the have continued the cooperation begun in 2003. Committee for Closer Cooperation (JCCC) use of “good quality” reference materials and ILAC now holds a seat on the WADA Laboratory meetings and also at the annual Joint General proficiency testing. Assembly. Committee (LC). WADA held its fourth training course for (Accreditation Body) Assessors The Memorandum of Understanding (MoU) in April 2007. It is pleasing to note the good signed between ILAC and OIML in November ILAC Liaisons progress this collaboration continues to make, 2006 has been expanded to include IAF in a The review of liaison activities continues to be as reflected by the fact that a Memorandum of Tripartite MoU. Final preparations are underway a major focus of the ILAC Executive Committee, Understanding between the two organisations for the signing of this MoU during the Sydney who seeks to ensure that ILAC interests are was signed in November 2007 in Madrid during meetings in October. Progress is also continuing represented in areas which have an impact on the World Conference on Doping in Sport. the activities of ILAC and its members. To assist on the ILAC and OIML Joint Work Programme, with the management of the ILAC liaisons, the with related items scheduled for consideration Liaison Database was established in the last and progression during the ILAC/IAF annual Secretariat Staff quarter of 2005. The volume of information in meetings in October 2007. The staff of the ILAC Secretariat has recently the database has increased substantially since undergone some changes for 2007. We are that time and it is available for the information ILAC continues its very active role in many ISO pleased to welcome Sharon Kelly as the Senior of all ILAC members. It can be accessed via Technical Committees and CASCO Working ILAC Coordinator. Sharon, who previously the members’ area of the ILAC website. (ILAC Groups. This year ILAC liaison officers held the role of Assistant Technical Manager at

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NATA, brings extensive accreditation experience navigate and there have also been a number of ILAC Membership to the role and will be a valuable asset for the back end changes to make the website more ILAC membership as of 27 November 2007 is as Secretariat. readily able to adapt to the changing needs of follows: the ILAC membership. As always we welcome all ● 58 Full Members (Signatories to the ILAC We are also pleased to welcome Amanda Stubbs feedback from members and other users. Arrangement) representing 46 economies; who joined the ILAC Secretariat on 15 May 2007, ● 19 Associates representing 18 economies; as the Administrator – ILAC Secretariat, a role The ILAC-MRA Mark registration process ● 20 Afﬁliates representing 19 economies; she shares with Alison Hay. Amanda replaced continues and, as at 31 January 2007, 39 ● 5 Regional Cooperation Bodies Nilla Merrigan who left the ILAC Secretariat, to ILAC Full Members had signed Licensing ● 1 National Coordination Body take on a role with another organisation, on 2 Agreements with ILAC, for the use of the ● 24 Stakeholders (including CITAC) May 2007. Combined MRA Mark (the Combined MRA Mark is the ILAC-MRA Mark used in combination The ILAC membership (total 127 bodies) now From 1 January 2007, Annette Dever has taken with the accreditation body’s own mark). covers a total of 83 different economies world on the role of ILAC Secretary from Alan Squirrell. wide and approximately 30,000 laboratories and Annette and Alan have worked together in the The ILAC Secretary met with the Secretaries of 5,000 inspection bodies are accredited by the 77 Secretariat for the past 6 years. Alan continues the International Accreditation Forum (IAF) ILAC Full Members and Associates. to support the work of ILAC and the Secretariat and the Regional Cooperation Bodies, both in as ILAC Executive Liaison on a part-time basis. Cancun and Sydney, to consider opportunities Further information on ILAC can be obtained for, and beneﬁts of, closer cooperation and from the ILAC website at www.ilac.org, or email The Work of the ILAC Secretariat communication between the Secretariats. the Secretariat on [email protected] The new ILAC website was launched on 15 The meeting was very productive and several October 2006 and it incorporates changes initiatives were put forward for consideration Mr. Alan Squirrell requested by the ILAC members and other and some of these are now in the process of ILAC Secretariat/CITAC Liaison users. In addition, the new website is easier to being implemented. Australia

IMEKO Technical Committee (TC-23) on Food and Nutritional Metrology

International Measurement Confederation known safety issues, expanding the activities in the area Objectives of TC-23 as IMEKO is a non-governmental federation of 36 of inorganic chemical metrology relevant to F&N F&N metrology is an emerging discipline that member organizations individually concerned with measurements. is helpful in strengthening the reliability of the advancement of measurement technology. analytical data, and integration of metrological Its fundamental objectives are the promotion concepts into the measurement process is the of international interchange of scientific and Food Safety Concerns and need of the hour. This step is necessary also technical information in the field of measurement Measurement Issues to ensure sustainability of the analytical QA and instrumentation and the enhancement of process. These tasks are looked upon as a twin In the world of food as a trading commodity, international co-operation among scientists and assignment under TC-23: (i) enhancing the engineers from research and industry. Founded we are moving towards a global but borderless- reliability of F&N measurements by introducing in 1958, the Confederation has consultative status trade situation. Food safety being a prime metrological concepts, and (ii) strengthening with UNESCO and UNIDO. IMEKO secretariat is concern under this scenario, reliable F&N the metrological capability of the professional based in Budapest, Hungary (for details please measurements take the centre stage in decision- pool (capacity building for young investigators), refer to www.IMEKO.org making. A measurement process characterized since the academic system in the F&N areas by metrological concepts enhances the reliability generally do not provide for adequate training IMEKO has recently approved a Technical of analytical results and ensures sustainability to that includes teaching metrology. Committee (TC-23) on Food and Nutritional the quality assurance (QA) needs. These steps For details how you can contribute to this effort, (F&N) Metrology. This is yet another important infuse authority to the F&N analytical results please contact: milestone for strengthening the reliability of F&N and enhance the user confidence in the ensuing measurements by an international organization public health decisions. Importantly, QA is also Prof. Venkatesh Iyengar supported by a host of outstanding metrology firmly linked to economic benefits at the national Chair of TC-23, IMEKO experts. The TC-23 facilitates addressing food levels. USA

● CITACCITAC NEWS NEWS ● FEBRUARY FEBRUARY 2008 2008 / / 9 RReportseports ooff InternationalInternational OOrganizationsrganizations EURAMET METCHEM Activity in Metrology in Chemistry

METCHEM is the technical committee of session with invited speakers. Specific subjects Report on electrochemistry EURAMET (European Metrology Association) were chosen and Portuguese field partners, Petra Spitzer reported on the activities of the dealing with metrology in chemistry: a joint particularly from EURACHEM, were invited to Electrochemistry WG. 16 participants attended committee between EURAMET and EURACHEM present their view and experience. As usual, part the meeting. At the meeting three presentations (the network association aiming to promote good of the session was dedicated to the most recent were given: one on some developments for the practices in analytical chemistry). METCHEM developments regarding training and education measurement of dissolved oxygen by INRiM delegates meet annually in February at one of in Metrology in Chemistry. (Italy), another on electrochemical metrology the European NMIs. The following points were activity in Estonia by the University of Tartu, and covered at the last meeting. The following eight topics were presented: the last on electrochemical measurements of ● Water analysis laboratories - European simple ions and glucose in complex mixture by directive METAS (Switzerland). Mandate of the Chairman ● Proficiency assays suppliers - traceability The mandate of Philippe Charlet (LNE, France) ● Producers of reference materials Concerning the projects, three are on-going: ended at the Euromet General Assembly in May ● Emergent sector - traceability in medical Project n° 843 on the evaluation and the 2007 (two mandates, 2003-2007). During 2006, sector calibration of pH on site measurement instrument the METCHEM chairman asked METCHEM ● Emergent sector - traceability in bio metrology is scheduled to end in December 2008. The two contact persons to provide names of candidates ● Measurement uncertainty revisited other projects are Project n° 898 on electrolytic for the position of chair. Two names were ● Alternative approaches to uncertainty conductivity at pure water level and Project n° proposed to the Euromet executive and elections evaluation by Bertil Magnusson (SP, Sweden) 918 on traceability of salinity measurements in were carried out in December 2006. The new ● The status of the European training and sea-water. Another project has been proposed: METCHEM chairman for the period 2007-2009, education initiatives by Philip Taylor a research project on traceability on ion activity at least, is Bernd Guettler from PTB, Germany. (IRMM) measurements (electrolytes in e.g. serum by ion ● International master study programme by selective electrode). The current convenors of the METCHEM sub- Ivo Leito (University of Tartu, Estonia) committees are: Report on gas chemistry ● Electrochemistry: Petra Spitzer, PTB, Research / Co-operation Trends Martin Milton reported on the activities of the Germany (status of projects and new cooperation developments) Gas Analysis WG. The attendees were from 22 ● Inorganic Analysis: Christophe Quétel, Report on inorganic analysis countries and 26 laboratories. The two mains IRMM, EU Christophe Quétel reported on the activities of topics were CMCs and projects. ● Gas Analysis: Martin Milton, NPL, UK the Inorganic Analysis WG and Bernd Guettler ● Organic analysis: Franz Ulberth, IRMM, EU reported on the on-going and proposed Martin Milton informed the assembly that projects. 22 participants attended the WG. The a workshop on “dynamic measurements of two mains subjects were the CMCs (Calibration NO2, SO2, CO at low ambient level and their Meetings and Measurement Capabilities) review and the comparability” will be held in March 14-17, 2007. In 2007, the METCHEM meeting plenary was held projects. A mini workshop was organised on the Concerning the comparisons, Milton gave the new at IPQ, Caparica, Portugal, February 8-9. Two traceability and characterisation of isotopic CRMs results on Projects n° 708, 883, 867 and 900. sub-committee meetings were held on February by means of synthetic isotopic mixtures. 6th (electrochemistry and organic) and two Four new projects were proposed on the others (inorganic and gas analysis) on February In addition two projects have been registered: following topics: 7th. Therefore, the meetings of the four sub- Project n° 894 deals with “Surface Enhanced ● optical spectroscopy as a potential primary committees were spread over two days in order Raman Spectroscopy - SERS - based metrology method to allow specialists to attend 2 or 3 SC meetings. at a primary level”. A work-plan was proposed ● purity analysis comparisons of nitrogen at sub This created stimulating exchanges, discussions by the coordinators NPL and PTB. It will be 50 nmol/mol and proposals. Visits of IPQ laboratories were interesting to add the project to the European ● bilateral comparison planned during these two days. 40 persons Metrology Research Program. ● ozone pre-cursor, already a Euromet from 24 European countries (plus IRMM Project n° 886 with 20 participants. A lot of representatives) attended the plenary meeting. Project n° 924 topic is on “the development components have to be studied from solvent, of a sustainable traceability and dissemination cleaning, chemical industry, bio-genics, active During the Plenary Session a follow up to last system providing Europe-wide comparable components, difficult to control and treat. year’s forum discussions between NMIs and measurement results in water analysis under the EURACHEM delegates on the “Strategies of WFD”. The project aims to support the Water Report on organic analysis NMIs to ensure adequate metrology capabilities Framework Directive, started in December 2006 Franz Ulberth reported on Organic Analysis WG. to users” was given by organising a special and should be completed in February 2009. The report concerned the CMC Cycle VIII review

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and the on-going projects. The question was to those laboratories was also a point raised. at the next inter RMOs (Regional Metrological raised on the necessity of keeping this group The laboratories are not intrinsically aware and Organisations) meeting in April. as there are no new proposed projects at the interested by metrology but just in the delivering moment. of CRMs. For some countries it can be difficult to Valuable contacts with the other RMOs and the motivate the laboratories to participate in such a CCQM were maintained at a high level (meetings, Project n° 878 was updated for “Crude protein group. The question of the future of the organic exchange of information, invitation to seminars in cereals”. Some new results were presented group is still open. No consensus was expressed and events, etc.). Furthermore, METCHEM was on Project n° 833 concerning PCB congeners by the Metchem contact person group. fully involved (TC chair) in the ad hoc working in organic solution to build up measurements group of BIPM that is currently elaborating a capacities. The results improved when compared Mutual Recognition Arrangement strategy regarding activities to be carried out at to the results given in 2004-2005. A questionnaire European NMIs often participate in CCQM the CIPM level on Materials Metrology. was sent in 2004-2005 on the activity and needs activities and coordinate CCQM comparisons. in the organic field. the questionnaire showed CCQM Working Groups are mainly chaired All during the year European NMIs have been fully that the community expressed a great interest by European Convenors (Inorganic by LGC, involved in the preparation of JRPs (Joint Research in training exercises and comparisons. However, Electrochemistry by SMU; Gas by NMi, Bioanalysis Projects) within the framework of a ERANET Plus there is no new proposal for future comparisons by LGC, Surface Analysis by BAM) and these program. Metrology in Chemistry was particularly and no real reason given. In Europe, some NMIs convenors are also very involved and active in concerned by the Targeted Program “Health”. have well-established capabilities, and it seems METCHEM activities. that they have other priorities. With these programs, European NMIs are entering into new cooperative activities aiming In 2006 and the beginning of 2007, as usual, a A discussion started on the difficulties large part of the activities of the convenors and to reach sustainable financial support from the encountered in this WG related to active delegates of the Technical Committee were European Commission, through Article 169. participation. There are many designated institutes devoted to the review and the submission of The new structure of the European Metrology (DI) in this field. DIs need encouragement from the next CMCs (Calibration and Measurement Association with the creation of EURAMET was NMIs to participate in the activity of this group. Capabilities) Cycle (Cycle VIII). 102 claims (new specifically designed to support the development There is certainly also a question of funds. and revised) proposed by 9 institutes were of research collaboration between NMIs. It seems important to the Metchem contact accepted during the discussion at METCHEM in persons to attract laboratories and potential mid-February and proposals sent to JCRB on Dr. Philippe Charlet DIs to share ideas and experiences. The lack March 1. They mainly concern the inorganic Past METCHEM Chair of communication and transfer of information analysis field. These proposals will be discussed LNE, France

Plenary meeting of METCHEM

● CITACCITAC NEWS NEWS ● FEBRUARY FEBRUARY 2008 2008 / /11 11 RReportseports ooff InternationalInternational OOrganizationsrganizations Bayesian Statistics to Improve Reference Values in Metrology in Chemistry: an ERANET-Plus Project The European Framework on the use of CRMs. These CRMs are usually called posterior, about the targeted quantity In May 2007, EURAMET e.V., the European produced by National Metrology Institutes and its associated uncertainty is improved. More Association of Institutes of Metrology, submitted (NMIs) and provided to laboratories for different specifically Bayesian estimates give a complete the proposal for an ERANET Plus (European specific purposes of Quality Control and Quality description of the uncertainty given observations Research Area Network) funded European Assurance. In addition, NMIs have implemented and prior knowledge. Here prior means before Metrology Research Program (EMRP) to the so called primary methods of measurements observations are made, so that prior information European Commission. The three pillars of the which ensure the traceability of measurements is elaborated from expert judgements and past EMRP are fundamental metrology, innovation to the SI and that are also used by NMIs to assign results. This prior information is modelled by a and quality of life, and technologies of the future the certified value to materials. probability density function (pdf) which is meant with the aim of demonstrating that coordination to best represent our degree of belief about of European Metrology is sustainable. As a part Value-assignment can also be based on data the possible values of the quantity before new of this program, a horizontal targeted program from an interlaboratory study. Consensus values observations. of the EMRP has been devised on metrology are based on the results of all participating underpinning “health”. Indeed, not only are laboratories or only on selected laboratories. So what’s new with Bayesian approach? Unlike health advances a policy priority in Europe According to the development or improvement classical frequentist statistics which works with but also an area where metrology can make a of analytical techniques by manufacturers and the sole new observations modelled by the significant impact swiftly. laboratories, NMIs are used to certify their likelihood, Bayesian approach allows, via the reference materials from time to time in order introduction of a prior, to take into account Starting from the observation that data and to obtain more reliable and accurate certified the most information at hand within a specific uncertainty analysis in the field of laboratory values through a re-certification process. statistical modelling framework to obtain more medicine and clinical chemistry are not yet well accurate estimates of parameters. established, European chemical experts have developed Joint Research Projects (JRPs). Among Re-certification: situation them the JRP entitled "Tracebioactivity" has Re-certification of a certified reference material Bayes’ Formula : from prior to been selected so that the European Commission can be performed either through interlaboratory posterior will provide its financial support, and it is not comparisons or by a single laboratory, typically Let θ be the random variable modelling the incidentally that this JRP includes a work package a NMI carrying out a primary method of targeted quantity and x = (x1,…,xn) be n new "Modelling and data analysis: - New methods and measurement. In both cases old and new data measurements. Let us define the following algorithms employing a Bayesian approach to are at hand. Old data are past measurements notations for the different notions introduced compute reference values from interlaboratory used to compute the past certified values. When above: comparisons in laboratory medicine” which will they were computed, the past certified values • The prior knowledge about θ is modelled be conducted by PTB (Germany), LNE (France) represented our best knowledge of the true by the pdf π(θ). and SP (Sweden) by 2008. value of the CRM. Nevertheless, by now this • The posterior updated knowledge is valuable information have been left out when modelled by the pdf π(θ|x). An important aspect underlying this project is computing each new certified value. • The data are still modelled by the likelihood the application to Certified Reference Materials p(x|θ). (CRM), so that this paper aims to shed light on Challenge: To take into account the most data at The Bayes’ formula is then given by: how Bayesian statistics can improve the reliability hand to get more accurate certified values and p(x|θ)π(θ) of the certified values of reference materials. associated uncertainties and thus to improve ------π(θ|x)= p(x) Before going any further let us first have a brief traceability. look at the crucial role of CRMs. Answer:: Bayesian statistics have a widespread where p(x)=∫p(x|θ)π(θ)dθ is the normalizing approach to science and technology. Recently constant so that the left member integrate to Certified Reference Materials: researchers have been trying to apply it to unity and be a density. the tool of the chemical analyst metrology and, more specifically to metrology Using the symbol of proportionality ∝, it appears Accreditation of laboratories for chemical in chemistry. then more clearly that the posterior density is analyses is an essential quality management proportional to the prior times the likelihood: tool and a means to obtain confidence and π(θ|x) ∝ p(x|θ) × π(θ) comparability of results. Due to the introduction Bayesian Approach of the international standard ISO/CEI 17025, Bayesian approach is a learning method based observations field laboratories have expressed their need on the Bayes’ formula, designed to update our of specific traceability schemes to ensure the knowledge of a quantity through the combination Posterior Prior reliability of chemical measurements. Actually of prior information about this quantity and knowledge about θ knowledge about θ these traceability schemes are mainly based new observations. As a result, our knowledge,

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Estimates of the mean and the variance of the quantity are then given by the mean and the variance of the posterior distribution π(θ|x) and are usually computed numerically.

Let’s give an easy example. Just consider that the prior pdf of the quantity θ and the pdfs of

the observations x1,…,xn are both Gaussian as described below: xi|θ~N(θ,σ2) θ~N(μ,τ2) In that case the posterior distribution of θ is:

θ|x1,...,xn~N(θ1,ø1) Where: (P)

Figure 1: Recertiﬁcation of a certiﬁed property of a CRM in a Bayesian statistical framework Notice that:

● The posterior mean θ1 is the weighted mean of When N laboratories are involved the expression precisely this idea of compromise that makes the prior mean μ and of the sample mean of the of the posterior distribution is more complicated Bayesian approach so attractive. observations where and because the expression of the likelihood is then heavier. Indeed, now let x be the jth measurement ● The posterior inverse variance ø -1 is the sum 1j Improving Reliability in 1 th of the inverse variance of the prior and of the of the i laboratory where each laboratory makes Recertification: providing n measurements that is j is between 1 and n inverse variance of the sample variance of the i i confidence on measurements observations . for i between 1 and N. In addition, suppose that the variances of the measurements in each In conclusion, working on new measurements which shows that Bayesian approach is a 2 together with previous reliable measurements laboratory are different, say σi for laboratory i. compromise between the prior and the The model then becomes: gives more accurate and reliable updated values. That way the new certified value and observations. x j|θ~N(θ,σ 2) i i its associated uncertainty is consistent with the θ ~ N(μ,τ2) Bayesian Approach in Metrology previous certified values and their uncertainties. The posterior distribution of θ is then given by: In addition, when updating the certified value, in Chemistry metrologists increase the traceability of CRMs by Undoubtedly Bayesian approach can be applied improving the knowledge of the best estimate of to the recertification process of CRMs. In this case the true value of the CRM. the recertified value and its associated uncertainty ֿ :Where are the updated values of the past certified values Finally many decisions in the clinical sector are and their past associated uncertainty through based on results of content measurements. Bayesian analysis. In particular the recertification That’s the reason why the JRP project will process through intercomparisons is illustrated first investigate the requirements of the in the Figure 1. European clinical sector for improved mathematical tools and then intends In the case where all the distributions are We observe that the posterior estimates of the to make the demonstration that Bayesian Gaussian, the example above may be considered probability theory is really the most promising as a special case. Indeed if one supposes that: mean and the inverse variance are still a weighted mean and the sum of the inverse of the variances approach to provide appropriate solutions for • θ is the certified property the improvement of reliability and comparability • the x i=1…n are the results of a sole respectively. In this respect it is worth noticing i of measurements. laboratory (case N=1) that this time, not only do we obtain a weighted mean between the prior and the observations but • the xi are issued from the same Gaussian distribution (mean θ, variance σ2 ) also the term standing for the observations is a Séverine Demeyer then the posterior distribution of θ is given by weighted mean of the means of the laboratories. LNE-CNAM, France expression (P). Thus all the information available has been taken This particular model can thus be applied when into account and weighted according to the new Dr. Philippe Charlet recertification is performed by one laboratory only. measurements and prior knowledge. And that’s LNE, France

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General Report comparisons and cooperation between ● APMP.QM-P07 (trace elements in soybean The 22nd APMP General Assembly and 6th TCQM APMP members and international powder) meeting were held at the “Habitat Centre” cooperation with other RMOs and BIPM were This programme was running parallel to New Delhi, India, December 13–16, 2006 in reported. CCQM-P64. Eleven NMIs participated cooperation with the National Physics Laboratory in the APMP study and 19 NMIs participated of India (NPLI) and APMP. Approximately 150 APMP TCQM Activities in 2006: Highlights in the CCQM study. According to the metrologists from member NMIs and guests from ● An International Symposium and Workshop coordinating lab, agreement of the data from CIPM, BIPM, RMOs (EUROMET and SADCMET), on Metrology in Chemistry was held in CCQM-P64 was better than the APMP QM-P07. ● metrology societies (IMEKO, NCSLI) and SRB Malaysia on 20-21 February 2006 to promote APMP.QM-P08 (SiO2 thickness on Silicon)

(APLAC, APLMF, PAC) were present. Brief the awareness of MiC and to draft a guideline SiO2 thickness on Silicon reports were presented from NSCLI meeting and document for setting up national measurement Coordinating laboratory reported that the CMC issue, COOMET GA 2006, APLAC GA system in MiC. 11 organizations (CSIR-NML, ITRI, KRISS, 2006, APLMF GA 2006, SIM GA 2006 and APEC/ ● 4th Workshop on Gas CRM for Calibration KOBELLO, NIMT, NMIJ, NRCCRM, NTT-AT, SCSC meeting 2006. Jordan National Metrology and Testing was held in Thailand from RENESUS, SAIT, and TRC) participated and Institute (JNMI) joined as a new associate 22-24 February 2006. The objective of the employed a range of measurement member of APMP. workshop was to exchange knowledge techniques such as ellipsometry, HR-RBS, between APMP TCQM and CCQM GAWG SIM, TEM, XPS and XRR. Update on APMP data in Appendix C members on the production of gas CRMs, ● APMP.QM-P09 (pH determination of Based on the agreement at 16th JCRB in April gas analysis, traceability system and phthalate buffer) 2006, APMP returned the list of QM CMCs to the uncertainty evaluation. Eleven organizations from seven JCRB Executive Secretary declaring the status of ● 5th APMP TC Chairs meeting was held on economies(CERI, DSS, IDTI, Kato Co, the QS supporting those of AU+CN+JP+KR. In 30-31 March 2006 in Singapore to facilitate KRISS,LIPI, NIMT, NMIJ, NML, NPLI and Wako response to JCRB’s inquiry, APMP sent additional and prepare the APMP’s presentation to the Co) participated. Two NMIs used pH primary explanation about JP+KR on 24th July 2006 and 16th JCRB meeting describing the QS review method with hydrogen electrode and others about AU on 28th July 2006. process in the region. used glass electrode method. ● The DEC meeting, QS workshop and APMP Asia-Paciﬁc Metrology Programme (APMP) strategic planning session were held on 10-14 Progress report on the following the 6th Technical Committee on Amount of July 2006 in the Philippines. The main theme supplementary, bilateral and trilateral Substance (TCQM) Meeting of the programme was to take a wider view comparison were also presented. ● About 40 delegates from 18 member states/ and develop an overall strategic plan for ● APMP.QM-SC1(Gravimetry) economies attended the meeting. APMP through collaborative efforts. ● APMP.QM-SC1(Impurity analysis in methane)

● ● ● Guests from other RMOs and BIPM were A working group was formed to establish a APMP.QM-K4.1(Ethanol in N2) ● invited to TC meetings to participate in guideline document for creating or APMP.QM- K1.d (SO2 in N2) ● comprehensive discussions on issues relevant improving a national infrastructure for APMP.QM- k1.c (NO in N2) to the APMP members and organizations. chemical measurement. Dr. Laurie Besley th ● Dr. Robert Kaarls, Secretary of CIPM and presented a draft document at the meeting The 5 APMP TC Chairs’ Meeting President of CCQM was invited to give a and invited members to give opinions and The 5th APMP Technical Committee Chairs’ presentation entitled “”CCQM progressֿ feedbacks. Meeting was held on 30 - 31 March 2006 in report 2006”. DR. Kaarls outlined the history ● A Chemical metrology symposium was held Singapore. hosted by SPRING, Singapore. and development of CIPM and its relationship along with Admet India 2007 in cooperation ● Each TC Chair and the delegate reported with other inter-governmental and with CITAC, APMP and NPL India. Quality System review status and APMP Key/ international organizations such as JCTLM, Supplementary comparisons status. ISO-REMCO, IAEA, ILAC, IUPAC, WADA etc. Progress Reports on Outstanding Pilot ● APMP Secretary explained the speciﬁc ● Delegates from member organizations who Studies/Key Comparisons procedure for Quality System review. regularly attended various CCQM Working Progress reports were given by representatives of It has been agreed that CMCs of APMP Group meetings gave updates on the latest coordinating institutes on the following studies: member NMIs already published in Appendix activities and programmes organized by the ● APMP.QM-P05 (Cd in Oyster tissue) C will be reviewed once a year in accordance CCQM Working Groups. The coordinating lab KRISS reported that six with the decision of APMP General Assembly. ● Representatives from member states gave NMIs (GLHK, KRISS, LIPI, NFI, NMIA and ● APMP TC Chairs have arranged BMC/CMC reports on the activities and future plans of TISTR) participated in the programme and deﬁnition to the satisfaction of APMP their respective countries/economies. those NMIs using IDMS methods showed a members in preparation for the 16th JCRB ● Results of calibration and measurement preferential agreement on reference values meeting held in April 2006. capabilities (CMC) reviews, pilot studies, key and MU than those of the non-IDMS. ● APMP TC Chairs have also agreed to a

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tentative procedure of APMP Quality meetings will be held in Sydney in October Akin (KIM_LIPI) as two new members of the System review criteria, which is effective until 2007 hosted by NMIA Australia. Executive Committee. The General Assembly December 2006. ● The General Assembly elected Indonesia as also approved the following new TC chairs: Dr R the venue of the 24th GA in 2008. P Singhal (NPL, India) – TCL, Dr Saito Terubumi Future Activities and Planning during the (NMIJ, Japan) – TCPR, and Dr Ho Seong Lee Meeting: New Appointments (KRISS, Korea) – TCTF. th ● 5 APMP TCQM Gas Analysis Workshop on The General Assembly elected Dr Kwang-Haw 23-25 May 2007 in Xian, China. Chung (from KRISS) as the chairperson-elect, Dr. Laly Samuel ● Workshop on MiC in mid June in China. Dr Vikram Kumar (NPLI) as the new DEC chair Measurement Standards Laboratory rd ● The next (23 ) APMP GA and related and Dr Vikram Kumar (NPLI) and Dr Hussein New Zealand

SADCMET Amount of Substance Annual Report to CITAC: 2007

In addition to strengthening metrology in Table 1: Measurement Toolkit rollout testing and updating of the primary standard the areas of trade measurement, the current mixtures. The measurement standard for carbon focus in the SADC region is on traceability for Country Date monoxide (CO) in nitrogen consists of primary measurement results in analytical chemistry and ...... standard mixtures over the concentration range medical diagnostics. Special programmes are Tanzania 18-19 May 2006 of 1 μmol.mol-1 to 10% mol.mol-1 and carbon being conducted to provide reference materials Ethiopia 13-14 June 2006 dioxide (CO2) in nitrogen ranges from 100 μmol. for food analysis and various proficiency Lesotho 2-3 July 2006 mol-1 to 20% mol.mol-1. The primary standard testing schemes have been piloted. Third party Mauritius 4-5 July 2006 mixtures for nitric oxide (NO) and sulphur accreditation of food health testing laboratories Brazil 31 July to 4 August 2006 dioxide (SO2) in nitrogen range from 10 μmol...... -1 -1 is progressing and traceability in medical mol to 1 % mol.mol . Established stability data diagnostics is receiving special attention. A SADC water proficiency testing (PT) workshop are now available for carbon monoxide and was held in Gaborone from 20-24 November carbon dioxide for over 2 years and for nitric oxide and sulphur dioxide for a period of 1 year Metrology in chemistry activities in the region 2006 to discuss the completed third phase of a and 6 months, respectively. All these reference (outside South Africa) focus primarily on the regional water PT scheme (sponsored by the PTB materials are now also commercially available. establishment of accredited analysis or testing with assistance from the SADCMET secretariat facilities in support of local export products. at NMISA). The fourth phase including The laboratory participated in a key comparison Traceability is sourced from outside the biochemistry, has since commenced. for carbon dioxide (CO ) in synthetic air at region and South Africa. Training is provided 2 ambient levels (360 μmol.mol-1). This was the particularly by the National Metrology Institute Participation in the activities of the Consultative biggest key comparison organised by the CCQM of South Africa (NMISA) and the Physikalisch- Committee on Amount of Substance (CCQM) gas analysis working group to date and the Technische Bundesanstalt (PTB). Training in of the International Committee of Weights laboratory performed well compared to the other metrology (measurement toolkit) was provided and Measures (CIPM) in SADC is primarily participants. The result of the laboratory was to more than 100 small and medium enterprises performed by the NMISA. Kenya and Egypt (associate members of SADCMET) are in the within 1% of the KCRV. However, the uncertainty in 5 countries, including Brazil (Table 1). process of submitting their first calibration quoted on the result was conservative compared and measurement capability (CMC) claims. to the other participants. Further projects included assistance to fourteen A summary of metrology in chemistry and food testing laboratories in Tanzania to the especially CCQM activities is provided below. The laboratory also participated in a key level where they could be assessed to ISO comparison for the gravimetric preparation 17025 (sponsored by the Danish International -1 of 100 μmol.mol oxygen (O2) in nitrogen. Development Agency - DANIDA). The PTB also Gas Metrology Only preliminary results for this comparison sponsored assistance to mass laboratories in The national measurement standards for ambient have been discussed at the CCQM gas analysis Botswana and Zimbabwe. air monitoring were maintained by stability working group meeting in April 2007.

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The laboratory also participated in a bilateral industry as well as in preparation of a CCQM key The laboratory also participated in the purity comparison with NMi VSL in the Netherlands. comparison. The laboratory will also develop assessment pilot inter-comparison. The samples The comparison was registered as a EUROMET the capability to prepare condensable gas were distributed during September 2006 and the project. The purpose of the comparison was mixtures in the coming year for the development results were submitted during January 2007. PTB to serve as a feasibility study to evaluate the of a primary standard for ethanol-in-nitrogen presented a possible study for the determination capabilities of the NMISA to act as coordinating for evidential breath testing. This technology of chloramphenicol (CAP) in milk (a veterinary laboratory for a key comparison of carbon will also be especially applicable to provide drug, CCQM-P90). Since the analysis of CAP is monoxide (CO) in nitrogen at 5 μmol.mol-1. After reference materials to SASOL and other polymer of concern for SA, the laboratory decided to several comparison rounds the two laboratories based industries. develop and validate a method for participation compare well, but the CCQM gas analysis in this study. The call for participation and working group indicated that they require During 2006 the accreditation of the laboratory study protocol was presented at the fall meeting more work to improve the uncertainty on the was maintained with an extension of the scope in Korea and the sample distribution was analytical capability of the NMISA, as well as the to include the gravimetric preparation of nitric planned for January 2007. Unfortunately due to purity analysis of the CO parent gases. oxide (NO) and sulphur dioxide (SO2) mixtures. homogeneity issues, the study has been delayed The laboratory also underwent its initial and the samples were only received in April For other regional comparisons, the laboratory assessment to ISO Guide 34 for the production 2007. The results are due in July 2007. participated in an APMP comparison for the of the certiﬁed gaseous reference materials. gravimetric preparation of 12,5 % nitrogen The laboratory was invited to present a paper

(N2) in helium with very good results. Finally Organic Metrology on the production of certified reference the laboratory also participated in a pilot study The organic group kicked off 2006/7 by materials at the Biological and Environmental for the gravimetric preparation of nitric oxide filling a large order for aqueous ethanol and Reference Materials (BERM 10) conference (NO) in nitrogen (30 to 70 μmol.mol-1). The sodium fluoride certified reference materials held in Charleston, South Carolina, USA. This laboratory’s results were excluded from the (preparation, assay and certification). This was a great opportunity to showcase SADC regression analysis of the results from the coincided with the preparation of three and some of the reference materials that are participants for the determination of the KCRV concentration levels for the second proficiency provided. Two posters were also presented due to problems with purity analysis of the NO testing (PT) scheme for ethanol. The matrices to highlight the ethanol and sodium fluoride parent gases. for the previous scheme were blood and certified reference solutions. Mention was also urine, while the second scheme was aqueous made of the gas primary standards that are in The laboratory is in the process of developing ethanol. The PT scheme continued for the rest production at our laboratory. The paper was a methodology for the purity analysis of of the year and comprised 12 different ethanol well received and published in the Accreditation reactive parent gases, such as nitric oxide concentrations over 4 rounds. The scheme has and Quality Assurance Journal “M.Archer, B-J

(NO) and sulphur dioxide (SO2) by Fourier served to assist laboratories with accreditation de Vos, MS Visser, The Preparation, Assay and transform infrared spectroscopy (FTIR). The and demonstrating in-house laboratory Certification of Aqueous Ethanol Reference purity analysis of carbon monoxide by gas capability for the analysis of ethanol in blood. Solutions, September 2006. chromatography with flame ionisation detection Shortly after this, two more large orders for in high purity nitrogen has been improved to CRMs were received. Dissemination of measurement criteria is vital the level where the carbon monoxide can now and the NMISA was invited to present a lecture be detected at concentrations of as low as 20 The Organic laboratory received accreditation at the Laboratory Management seminar on “A nmol.mol-1. Primary standard mixtures for to ISO 17025 during October 2006 and ISO practical approach to method development carbon dioxide (CO2) have been developed to guide 34 during February 2007. This was the and validation in metrology”. Dissemination include the balance gas of synthetic air over the first laboratory in SADC to receive SANAS of analytical skills were also effected through concentration range of 100 μmol.mol-1 to 1000 accreditation to ISO guide 34 for the preparation the presentation of a one day “Basics of Gas μmol.mol-1 for the key comparison. of certified reference materials. Chromatography” course. The course was given during May 2007 and was attended by The development of the national measurement During April 2007, the NMISA attended the 29 delegates from industry and government standard for ambient air monitoring will Organic Analysis Working Group meeting laboratories. be completed in the coming year with the (CCQM OAWG) at the BIPM in Paris. The development and preparation of the primary results for participation in CCQM-P31a.1 and The laboratory was also invited to visit PTB standard mixtures for sulphur dioxide (SO2) P31c.1 were within 2-5% of the gravimetric as part of a student program and a NMISA and nitrogen dioxide (NO2) in synthetic air. The values for the pesticides (lindane, 4,4’-DDT metrologist received training in the development laboratory will then continue to develop a suite and 4,4’-DDE) and the PAHs (phenanthrene, of an isotope dilution liquid chromatography- of multi component mixtures of permanent fluoranthene, benz(a)anthracene, benzo(a)pyrene, tandem mass spectrometry (LC-MS-MS) method and reactive gases, primarily for the automotive benzo(ghi)perylene). for the analysis of chloramphenicol extracted

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from milk. This was an excellent opportunity the recommended IDMS comparison values will have to be evaluated in some kind of round since SA had agreed to participate in the CCQM- were in the range of 0.03 to 1.1%. Selenium in robin in the near future. P90 inter-comparison. pharmaceutical supplement was determined with a relative difference of 0.3% from the After the successful commissioning and training Other activities included research into method comparison value. The estimated deviation of on the Time of Flight Secondary Ion Mass development and validation; the result for Pb in wine (a key comparison) Spectrometer (TOF SIMS), the SAM laboratory ● automation of the sodium fluoride primary from the projected KCRV is 0.35%. The relative participated in an inter-laboratory comparison method, thus implementing an additional differences for Cu and Fe contents in wine (a study with NPL on the repeatability and reference method for the established CRM, pilot study) are expected to be well within 1% consistency of TOF SIMS measurements on a ● re-modelling of a headspace sampler from the projected comparison values. Very polymer sample. The relative quantification to improve the peak area repeatability good results were achieved for Pb, Cd and of an organic matrix was also successfully from 4% to under 1,5%. This will assist particularly for Fe and Zn determinations in completed as part of this study. A further study with the development of a headspace gas bovine liver. The relative differences for Fe and in progress on TOF SIMS is the quantification of chromatographic method using flame Zn in bovine liver are expected to be less than trace metal analysis. This study already resulted ionization detection for ethanol stability 0.5 % from the comparison values. in very positive results which will be published studies, after the results are verified with other primary ● a theophylline purity assessment involved Plans for participation in future comparisons techniques. research into exactly how to assign a value are in progress. It is envisaged that the scope of to a high purity material, intercomparisons will include a number of new The SAM laboratory provided measurement ● pesticide research is ongoing, as are measurands in the field of food nutrients, food support to the CSIR nanotechnology group extraction and recovery methods for target contaminants, plastic materials and metal purity. on various projects. A joint project on nano- analytes from complex matrices. A new Preparation of primary element standards by the phosphors between the University of the Free project was also started for the preparation IPS laboratory and their use in the comparison State, University of Kwazulu Natal, CSIR Build of industrial solvent CRMs in the Forensic studies will be of high importance. Environment and the SAM laboratory delivered field. positive results and the project will be continued into 2007/8. Surface and Microanalysis Inorganic Plasma Spectroscopy The surface and microanalysis (SAM) laboratory On behalf of the South African Bureau of (IPS) continued with the project in assisting the Standards (SABS), the SAM laboratory hosted th Primary and certified, single and multi-element automotive sector with the measurement of the 13 plenary meeting of the ISO TC 202 calibration standards for inorganic elemental substances of concern (SOCs). Awareness, Microbeam Analysis Working Group. Several analysis are provided to the SADC analysis and through roadshows and popular articles, was members of the SAM group is actively involved testing community. The standards are obtained created among the various OEMs (original in the development of ISO standards for electron from National Metrology Institutes (NMIs), equipment manufacturers) in the automotive microscopy, and host a local mirror working accredited institutions for the production of industry. This will now be extended to include group to ensure that members of the South reference materials or prepared in the IPS the electrical and electronic equipment (EEE) African microscopy community are up to date laboratory at NMISA. The calibration standards industry and the SOCs will include the two with developments in the field. are only used within their validity period and brominated flame retardants (BFRs) targeted replaced as required. They are kept in a clean by the restriction of hazardous substances RoHS The SAM laboratory also participated in a pilot and temperature controlled environment. All Directive 2002/95/EC. study on the determination of the nitrogen measurement standards are used according to concentration in “Diamond-Like Carbon” (DLC) the ISO 17025 requirements and the IPS quality layers. In all the specimens provided, the SAM control procedures. Most of the original equipment manufacturers laboratory delivered high-quality results. (OEMs) in the automotive industry were The IPS laboratory participated with particularly contacted and their analytical capabilities The scope of measurements for polymer good success in a number of CCQM pilot accessed. A definite need for laboratories analysis has been expanded with the successful and key intercomparison studies. For most providing reliable results was identified. In this commissioning of a thermogravimetric analyzer of the measurands, the NMISA results and process a laboratory database was compiled by (TGA) and a pyrolysis-GC-MS. their respective associated uncertainty values NMISA and is hosted by the National Laboratory compare quite well and were one of the better Association (NLA). The database will be An international project on developing comparison results reported. extended as more and more laboratories come vapour phase corrosion inhibitors for the The relative differences for Ca, Fe, Cu and to the fore and express interest to do analysis of packing industry have been secured, and a Zn contents in non-fat soybean powder from the substances of concern. These laboratories collaborative research project with the Royal

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Table 2. NMISA Substance comparisons

International Number Laboratory Description Participation in International 1 CCQM-K27 Organic Ethanol in aqueous solution Comparisons 2 CCQM-P20e Organic Theophylline purity In total, the NMISA participated in 15 amount of substance comparisons, listed in Table 2. 3 CCQM-P73 Gas 30 to 70 µmol/mol CO in nitrogen 4 EUROMET 900a Gas 5 µmol/mol CO in nitrogen Finally, a signiﬁcant event in the region was 5 CCQM-K52 Gas 360 µmol/mol CO2 in air 6 CCQM-K53 Gas 100 µmol/mol O2 in nitrogen the establishment of the National Metrology Determination of Essential Toxic elements in 7 CCQM-P85 Inorganic Institute of South Africa on 1 May 2007 through Bovine liver the Measurement Units and Measurement 8 CCQM-P86 Inorganic Analysis of total Se in Pharmaceutical supplements 9 CCQM-K30 Inorganic Analysis of Pb in wine Standards Act (Act No. 18 of 2006) of South 10 CCQM-P12.1 Inorganic Analysis of Fe, Cu and Cd in wine Africa. The new institute was established from 11 CCQM-P75 Inorganic Stable isotope data of H,C, N, O & S in methionine the National Metrology Laboratory (NML), which 12 VAMAS 2002 SAM Static TOF-SIMS Inter-laboratory study was part of the CSIR. All personnel and assets 13 CCQM-P80 SAM C amount in precipitates in Fe were transferred to the new entity. 14 CCQM-P81 SAM N amount in surface layers of Fe 15 CCQM-P-95 SAM Determination of light elements-N doped C layers The NMISA is an independent public entity under the auspices of the Department of Trade Institute of Sweden on measurement techniques measurement requirements of the South African and Industry of South Africa, the DTI. to characterise biodegradable polymers/ plastics, polymer and rubber communities in plastics have been established through the South Africa will be further explored in 2007/8 Dr. Wynand Louw National Research Foundations South Africa/ through the First Polymer Technical Advisory SADCMET Amount of Substance WG Sweden Memorandum of Understanding. The Forum in August 2007. South Africa

Report from SIM

Since 1995 when SIM was reactivated, Chemical Chemical Metrology Working Group activities In the last SIM Chemical Metrology WG meeting metrology has been one of the most strategic on training and capability assessment rather in Rio de Janeiro, 07-08 program plans were fields to be developed among member countries than participation in MRA-driven key and discussed. Some of the topics discussed were: in SIM. Especially since 1997 when the first supplemental comparisons This has been ● Chemical metrology in the Americas SIM Chemical Metrology kick-off meeting was accomplished through: Symposium to be held in conjunction with organized in Rio de Janeiro, many efforts have ● Outreach and awareness activities within the 2007 SIM GA during the week of Sept 24-28, been made to promote chemical metrology in ANDIMET CAMET, CARIMET and SURAMET 2007 in Ottawa SIM. subregions ● Subregional activities focused on Impact ● Chemical measurement proficiency of Chemical Metrology on Trade and Quality In the last 10 years the SIM Program in Chemical assessment comparison studies and follow-up of Life Metrology had particular characteristics: NIST activities – CARIMET (St. Lucia in 07?) and NRC have led this initiative and the newly ● Training in CMC preparation and review – ANDIMET (Ecuador in 07) born CENAM played a complementary role to ● awareness seminar focused on various demonstrate what a small economy can do. The long-term goal is to promote improved approaches for delivery of chemical capabilities in chemical metrology in the region measurement services In order to most effectively address the and increase participation of SIM members in ● guidelines for establishing a chemical unique needs of all 34 countries within SIM, CCQM and CIPM MRA-related activities, and metrology program whose capabilities in chemical metrology now, Brazil, Chile Uruguay and Argentina are – CAMET (Honduras in 08 in conjunction with GA) span a very broad range, SIM has focused its participating in CCQM activities. – SURAMET (Paraguay in 08)

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● Interlaboratory Proficiency Assessment possibilities to deliver reference measurement ● How could the project motivate the transfer Studies services of a higher metrological order. of knowledge and experience among ● Database on CCQM and RMO key countries in each group and among groups? comparisons and CRM development plans As an invited speaker, Dr. Laurie Besley of NMIA ● How could the project provide assistance to Potential CMWG Studies for 07 and 08 gave a talk on value-assigning PT sample, and a whole group and at the same time attend to ● SIM.8.12P1 Automotive Exhaust Emissions also Dr. Robert Kaarls, Dr. Willie May (NIST) specific needs of a country? ● SIM.8.21P Natural Gas and Dr. Mariana Arce (CENAM) presented their ● SIM.8.16P1 Toxic Metals in Seafood II (could experiences on metrological services in chemical Under the theme of Chemical Metrology in the include pesticides) metrology. Americas: Current Practices and Future Needs, a ● SIM.8.22P Cholesterol and Toxic Metals in symposium was held in conjunction with 2007 Meat Homogenate (include pesticides?) It is expected that SIM NMI metrology in SIM GA during the week of Sept 24-28, 2007 in ● SIM.8.19P Carbon Dioxide in Stack Emissions chemistry managers are aware of the possibilities Ottawa. (carbon dioxide?) and characteristics of different approaches to ● Trace Elements in Water (connect to CCQM deliver reference metrological services of a ● Plenary Session on Current State of the Key Comparison) higher metrological order. In this event PTB Practice In May 2007, SIM CMWG Awareness Seminar technical cooperation provided conceptual input ◆ Impact on trade and quality of life “Various Approaches for Delivery of Chemical and detailed report. ◆ Worldwide infrastructure Measurement Services of Higher Metrological ◆ 10-years progress in SIM Order in the Food Sector” was organized in Inen The follwing are recommendations derived from ● Poster session on current activities for each Ecuador. this seminar for a second phase project in MiC: Being that political support is critical to implement country The SIM-CMWG conducted discussion rounds an infrastructure in MiC, it is recommended to ● Needs for developing economies (focused on in the context of its subregional awareness organize specific activities, such as seminars or trade and quality of life) raising activities in Lima, Perú (June 2005) and individual meetings, to address policy decision ● New emerging technologies Montevideo, Uruguay (May 2006) on how to makers. During these activities, the impact of ◆ Energy design Metrology in Chemistry Programs on MiC on trade, environment and health should be ◆ Bio and Health the national level. The need for orientation clearly explained. ◆ Nano of responsible management level staff on the existing possibilities to deliver measurement Also recommended to ensure the continuity of For more details please contact Dr. Willie May: services on reference level became evident. the effort: [email protected] The objective of this seminar was to enhance ● How could the project fulfill the expectations knowledge at SIM NMIs and/or designated stated during this first workshop? Dr. Yoshito Mitani institutes on the range and nature of existing ● What kind of interaction will be among groups? CENAM, Mexico

Sampling - Validation, Quality Control and Uncertainty Estimation

Method validation and quality control have been ISO 17025 [3] for analysis, an accreditation that uncertainty are easily identified as the next implemented in analytical laboratories since requires validation and quality control of applied important targets in controlling measurement the late 1970s, e.g.: [1]. With the publication of analytical methods. Most operators specified uncertainty. guidance documents for uncertainty estimation, quality requirements to the analysis, although e.g.:[2], implementation of uncertainty only half of them actually verify the analytical With the guidance of the recently published estimation in analytical laboratories has been quality obtained. On the other hand, only 1/3 of Eurachem/EUROLAB/CITAC/Nordtest/AMC well under way since the mid 1990s. Still, the the operators applied quality control procedures Guide: Measurement uncertainty arising from use of concepts such as validation, quality of sampling and only 10% required accredited control and uncertainty estimation has been sampling. sampling: a guide to methods and approaches confined to the analytical processes. A recent (available at, http://www.eurachem.org) the first inquiry to the 20 major Danish operators of As sampling uncertainty may be considerably steps towards making this practicable have been groundwater investigations demonstrated the larger than analytical uncertainty (examples taken. Accordingly, quality control of sampling all used laboratories accredited according to in [4]), estimation and reduction of sampling is recommended in the guidance document

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on groundwater monitoring published by the well known concepts of random and systematic Furthermore, the requirements for competence European Commission [5]. errors. A range of tools are presented for the of both samplers and samplings planners are estimation of different types of uncertainty, see discussed and the required documentation of The Nordtest handbook on uncertainty e.g.: Table 1, including equations for calculating sampling is described in details. The minimum from sampling sampling uncertainty. documentation stipulated is: A handbook has now been prepared supported by Nordtest under the Nordic Innovation Table 1 Uncertainty contributions from random and systematic effects Centre on uncertainty from sampling [4]. The Random (precision) Systematic (bias) Nordtest handbook is an extract of and based upon the principles, methods and text of the Analysis Analytical variability – including sample Analytical bias (combined effect of bias Eurachem guide on uncertainty from sampling splitting/preparation and handling sources) [6]. The handbook provides practical guidance (combined contribution of random on sampling uncertainty estimation in the effects) Nordtest handbook format and will be freely available at the Nordtest web site at http://www. Sampling Sampling variability (dominated by Sampling bias (combined effect of nordicinnovation.net/nordtest.cfm, under NT heterogeneity and operator variations) selection bias, operator bias etc.) technical reports, report number NT tec 604. Until the final report is available on the Nordtest web site, a final draft of the Nordtest handbook is Validation and quality control of ● Written sampling procedures based upon available at http://www.samplersguide.com sampling defined sampling methods The concepts of method validation and quality ● sampling field report Sampling purpose and quality control familiar from analysis are then explained ● sampling report stating uncertainty of sampling requirements as tools that can be used for sampling as well. A The first part of the handbook emphasizes major barrier is here, that sampling may appear Whereas this may seem trivial as seen from the the fact that all measurements are done for a either as one or a few samples taken at each world of analytical chemistry, these requirements purpose and that sampling in most cases is an occasion, or as large sampling campaigns at one are not commonly met for sampling. The Danish integrated part of the measurement process. site. The use of validation and quality control is inquiry mentioned above demonstrated that ¼ Therefore the target of the sampling and the described in order to accommodate to different of the major Danish operators of groundwater required sampling quality depends upon the types of sampling without requiring an excessive investigations did not apply a written procedure purpose. The role of sampling in the uncertainty number of quality control samples (and derived and even when a written procedure existed, and decision chain can be seen from Figure 1. costs) compared to the samples required anyway only 15% of the procedures were based upon a In the handbook, examples are given on how to for the measurements. standard method. Less than 1/3 of the operators quantify the required sampling uncertainty, e.g.: would be able to provide estimates of sampling on setting sampling quality objectives. The methods presented are the replicate uncertainty. method for both validation and quality control, Sources of uncertainty in addition to a time series based control chart Uncertainty estimation To support efforts to control sampling type of quality control. The major part of the Nordtest handbook uncertainty, the contributions to sampling describes the methods that can be used for uncertainty are discussed and divided into the estimating the sampling uncertainty. The methods are based upon the replicate design, and the statistical methods are range statistics and two types of ANOVA. The methods are described in details showing all calculations in order to facilitate implementation. Guidance is given with respect to selecting the most appropriate statistical methods for the purpose, although the differences caused by using different statistical approaches in some case may seem very minor, see Table 2.

Figure 1. Sampling in the uncertainty and decision chain Finally, the use of variography as an alternative tool is described.

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Table 2. Example of calculation of uncertainty contributions using different statistical methods Data from sampling vitamin A in baby food

Practical examples stationary systems irrespective of sector Leonardo program under contract DK/06/B/ Perhaps the most important part of the Nordtest supported by Nordtest/Nordic Innovation F/PP-145.622, see also handbook is a series of worked examples Centre www.sampler-education.dhi.eu. demonstrating in details the use of the methods • Implementation of personnel certification presented for different sectors: groundwater of environmental samplers, also in a Nordtest References (environmental monitoring), iron ore scheme 1. Water Research Centre. Manual on Analytical (production control), baby porridge (product • Preparation of textbooks and exams for Quality Control for the Water Industry. 1978. quality control) and wastewater (environmental/ education of sampling staff supported process control). The examples are given showing by the European Leonardo program for the 2. ISO. Guide to the expression of uncertainty all data used and all steps of the calculations in implementation of a European Community from sampling. 1993. order to facilitate understanding of the principles vocational training policy. and methods. 3. ISO. General requirements for the Although the process of understanding and competence of testing and calibration Perspectives controlling sampling uncertainty to the same laboratories. ISO 17025. 2005. The main message of the handbook is that extent as analytical uncertainty has thus been uncertainty from sampling can be estimated with started at the technical level, implementation and 4. Grøn, C., Hansen, J B, Magnusson, B., reasonable effort and following steps that are enforcement will not be realized until required Nordbotten, A., Krysell, M., and Lund, comparable to those used in quality assurance by regulations and by the customers. U. Uncertainty from sampling - A Nordtest of laboratory analysis: method validation and Handbook for Sampling Planners on quality control. Still, the main emphasis has until Acknowledgements Sampling Quality Assurance and Uncertainty now been upon the uncertainty contributions The contributions of my co-authors of the Estimation. 2007. Nordtest. from random effects. Nordtest handbook: Jette B. Hansen, DHI, Bertil Magnusson, SP Technical Research Institute of 5. European Commission. Guidance on We urgently need practical tools for controlling Sweden, Mikael Krysell, Ulla O. Lund and Kirsten groundwater monitoring. WFD CIS the uncertainty contributions to sampling from J. Andersen, Eurofins A/S, Denmark and Astrid Guidance Document no. 15, Technical systematic errors comparable to those available Norbotten, Food Safety Authority, Norway are report 002-2007. 2007. European in analytical chemistry: proficiency tests and gratefully acknowledged. The inquiry to Danish Commission. certified reference materials. Examples of such operators of groundwater investigations was methods that are still only sparsely available are: initiated and performed by Mogens Wium, GEO, 6. Eurachem, EUROLAB, CITAC, and •Sampling method studies a contribution that was essential for describing Nordtest. Measurement uncertainty arising •Sampler proficiency tests the importance and the perspectives of the from sampling - A guide to methods and •Sampling reference sites Nordtest handbook. approaches. 2007. Among the efforts currently in progress in order to further enhance implementation of The Nordtest handbook and the workshop were uncertainty control in sampling are: supported by Nordic Innovation Centre/Nordtest Dr. Christian Grøn • Preparation of horizontal sampling under contract 04130. The sampler education DHI, Denmark standards for sampling of dynamic and textbook preparation is supported by the

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Measurement Uncertainty Revisited: Alternative approaches to uncertainty evaluation

This EUROLAB Technical Reports, Measurement designed and conducted so as to comprise valid approach. Concerning the use of laboratory Uncertainty Revisited: Alternative approaches to the effects from as many relevant uncertainty performance data from proficiency tests, some uncertainty evaluation is focussed on reviewing, sources as possible. The data utilised in these proposals have been published but the approach comparing and giving some examples of the approaches are typically precision and bias is still under debate. currently available approaches for evaluating data obtained from within-laboratory validation measurement uncertainty of quantitative studies, quality control, interlaboratory method Outline of the Eurolab Report: test results. After more than ten years since validation studies, or proficiency tests. Such Chapter 1 provides a summary of the current publication of the 1st edition, the Guide to the approaches are fully compliant with the GUM, main approaches for uncertainty evaluation: Expression of Uncertainty in Measurement, provided that the GUM principles are observed. (i) the modelling approach, (ii) the single- known as the GUM, is acknowledged as the laboratory validation approach, (iii) the inter- master document on measurement uncertainty Focusing on the first principle from the bullet laboratory validation data approach and (iv) throughout the testing community. The term points above, the basic requirements for any the proficiency testing approach. The use of “measurement uncertainty” is recognised to valid uncertainty evaluation are: PT data is still under debate and authoritative apply to all types of quantitative test results, and • a clear definition of the measurand, i.e. references are few. Therefore in chapter 2 a the GUM principles are fully accepted. Among the quantity to be measured full description of the approach using PT data others, these principles require that • a comprehensive specification of the • uncertainty evaluation is comprehensive, measurement procedure and the test is given. Chapter 3 is devoted to technical accounting for all relevant sources of items issues pertinent to comparison, validation and measurement error; • a comprehensive analysis of the effects revision of uncertainty estimates. As the core • uncertainties arising from random impacting the measurement results. part of this report, chapter 4 presents a range of and systematic effects are treated alike, examples. These are case studies from various i.e. are expressed and combined as Given a comprehensive list of relevant effects/ testing fields, where different approaches were variances of associated probability uncertainty sources, uncertainty evaluation may used to evaluate the relevant uncertainty and distributions; be carried out using various different approaches. the results so obtained were compared. Some • statistical evaluation of measurements They range from individual quantification and conclusions and recommendations complete the (Type A) and alternative techniques, combination of input uncertainties to collective main body of the document. Finally the Annex based on other data / information (Type quantification, e.g. using a reproducibility presents a compilation of selected standards, B), are recognised and utilised as equally standard deviation for a standard test procedure. guidelines, books and websites on measurement valid tools; Handling of uncertainty information requires uncertainty. • uncertainties of final results are expressed due attention to the scope and the form of The report is available under Documents at as standard deviations (standard the data concerned. For example, the results www.eurolab.org uncertainty) or by multiples of standard obtained using “empirical” approaches normally deviations (expanded uncertainty) with a refer to the typical performance of a specified Bertil Magnusson specified numerical factor (coverage test procedure on specified test objects, SP Technical Research Institute factor). while uncertainty estimates obtained using Sweden the modelling approach most often refer to on behalf of the Working Group that consisted However, when it comes to evaluating the individual measurement results. of Werner Hässelbarth, BAM (convenor) uncertainty of the results for a (quantitative) test Stephen Ellison, LGC, Manfred Golze, Anita procedure, the GUM almost exclusively treats a Concerning empirical approaches for uncertainty Schmidt BAM, Ulf Hammerschmidt, PTB, single approach for uncertainty evaluation: the evaluation, the use of the reproducibility Wilfried Hinrichs, Materialprüfanstalt modelling approach based on a comprehensive standard deviation from an interlaboratory für das Bauwesen, Ulrich Kurfürst, Fulda mathematical model of the measurement method validation study has recently been firmly University of Applied Sciences, Teemu procedure. Following the GUM principles established (see ISO/TS 21748). The use of Näykki, Finnish Environment Institute, experimental approaches have only recently within-laboratory data, that is, data from method Marc Priel, LNE, Burkhard Peil, DACH, received greater attention. They are based on validation studies and quality control carried out and Pedro Rosario Ruiz, Real Casa de whole-method performance investigations in the laboratory is also widely recognised as a Moneda.

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Information from the EuCheMS Division of Analytical Chemistry

After nine year in office, Heiner Korte retired Sanz-Medel of Oviedo University, Spain held via DAC-EuCheMS”. This work resulted in several as the secretary of the DAC and the secretary the Robert Kellner Lecture that is sponsored by publications including the latest contribution to elect is Jens E.T. Andersen of the Danish Springer Verlag. The Merck Award was awarded Analytical Chemistry of Italy published this year Chemical Society. The new secretary, the former to Alexander Makarov of Thermo Finnigan for preceding the conference in Turin 2008. secretary and the chairman Bo Karlberg met his development of the orbitrap analyzer of in Copenhagen in October to prepare for the mass spectrometry and to Prof. Shuming Nie of It is important to DAC to maintain networking takeover. The decision was made at the annual Georgia Institute of Technology for introducing with the other divisions of EuCheMS which are meeting of DAC held in conjunction with the quantum dots to clinical analysis and diagnosis. concerned with parallel scientific issues. This Euroanalysis XIV conference held in Antwerp, cooperation is ensured by appointing liaison September 9-12. At this meeting it was also Euroanalysis XV with the motto “The Impact persons who relate to education, history, life decided that DAC supports continuation of the of Analytical Chemistry on Quality of Life” is sciences, food, environment, electrochemistry, Study Group of Quality Assurance. Jens E.T. planned for Innsbruck, September 6-11, 2009, computations, microsystems, IUPAC and Andersen took over from Wolfhard Wegscheider can be viewed at www. EUROANALYSIS2009.at. Eurachem. The developments of quality after his long time position as head of the Study assurance and quality control are followed with Group. Jens E.T. Andersen was also appointed as In 2008 DAC will contribute to the Second General great interest because these subjects have a the liaison person to EuraChem and to CITAC. Conference on Chemistry in Turin September profound impact on a wide range of applications 16-20. DAC focuses on metrology in chemistry that are also considered and supervised by The Euroanalysis conference is the main event of and thus promotes the continuing effort within the European commission. Although highly the DAC, and was excellently organised by Koen the field of quality assurance Prof. Manfred specialised conferences are increasing in number Janssens and Luc Van't Dack under the auspices of Grasserbauer will present a lecture entitled “The and popularity, it is important to communicate Flemish Chemical Society KVCV. The conference Environmental Challenge for Analytical Sciences”. actively across the borders defined by technologies was held under the general theme “The role This work continues the process of involving in to ensure a high level of science, education and of analytical chemistry in the preservation of DAC the analytical chemists of the public sector, innovation. The contact with other divisions, with mankind’s natural and cultural environment”, industry and academia. supranational boards and with non-European and it was attended by 650 participants from 50 societies is maintained by observers. Updated countries world wide providing more than 800 Europe has a central role over the centuries information on DAC activities may be found at contributions. The stimulating scientific program, in developing analytical chemistry and Prof. www.dac-euchems.org including fully booked poster sessions, was Duncan Burns continues his effort within the flavoured with interesting booths of instrument framework of DAC with “Contributions to the Dr. Jens E.T. Andersen manufacturers and publishers. Prof. Alfredo History of Analytical Chemistry in Europe made JETA, Denemark

Heiner Korte on the left, Jens E.T. Andersen on the centre and Bo Karlberg on the right

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The aim of the CITAC award for the most The links can be followed for the complete The handbook is written for environmental interesting/important papers on Metrology articles and brief abstracts are provided below. testing laboratories in the Nordic countries, in in Chemistry winners for 2007 is to highlight order to give support to the implementation of remarkable papers in the field of Metrology David L. Deuwer, How to combine results the concept of measurement uncertainty for their in Chemistry which may not have been having stated uncertainties: to MU or routine measurements. The aim is to provide a “discovered” by the wider community after their not to MU? published in: Ales Fajgelj, Maria practical, understandable and common way of publication in a national journal (for example in Belli, Umberto Sansone (Eds.) Combining and measurement uncertainty calculations, mainly a local language) and are not readily accessible reporting analytical results. Royal Society of based on already existing quality control and to the larger metrological/analytical community. Chemistry, London (2007), pp 127-142. validation data. Practical examples, taken directly The award is normally awarded to three papers. from the everyday world of environmental CITAC also strives to “explain” publications This comprehensive report paper deals with laboratories are presented and explained. in known international journals written in the widely accepted issue that knowledge of “sophisticated language” to communities. Finally, the expected uncertainty of a measured value is The handbook covers all steps in the analytical it aims to draw attention to papers with scientific necessary for judging the measurement’s fitness- chain from the arrival of the sample in the content important to the wider community. for-purpose, but some experienced data analysts laboratory until the data has been reported. The argue against using measurement uncertainty approach is very general and should be applicable The nomination is coordinated by a CITAC (MU) in even relatively simple univariate to most testing laboratories in the chemical member elected for three years at a CITAC applications such as using interlaboratory data field. It is therefore envisaged that many more members meeting. For 2007-2009, Dr Wynand to assign the expected value of a measurand in laboratories over the world will benefit from this Louw, the current Vice-chair, was selected as particular materials. The question is then if MU wider exposure the “CITAC Coordinator for Nomination”. Any is not expected to be useful for univariate tasks, member can nominate a paper by sending a can it be useful in multivariate applications? Venkatesh Iyengar, Metrological concepts supporting letter and an abstract (by e-mail) of More generally, can estimates of MU provide for enhancing the reliability of food and the paper in English. The supporting letter should quantitatively useful chemical information when nutritional measurements published in the include the name of the paper’s corresponding there may be significant bias among the data Journal of Food Composition and Analysis 20 author and his/her e-mail address. The deadline analyzed, such as when measurements are from (2007) 449-450, for the nomination is 1 September, to enable the more than one source or are taken over a long process to be concluded by 1 October of the same period of time? year. The Coordinator sends the nominations to The paper deals with the concept that to CITAC members by e-mail to vote for the three incorporate metrological approaches into the most appropriate papers. All votes received by 1 This report describes the use of publicly measurement process enhances the reliability of October are counted. The winners are notified available CCQM (Consultative Committee for analytical findings. These developments include: by 1 November. Amount of Substance) data to explore whether high-quality reference standards, validated appropriately evaluated MU estimates can be methods, robust sampling practices, proven For 2007, three nominations were received. After useful in combining results from interlaboratory calibration approaches, natural matrix reference verification that the nominated papers fulfill studies. Three different approaches to using MU materials, speciation chemistry, assessment of the selection criteria, all three were selected as are evaluated (weighting, bootstrap resampling, measurement uncertainty and establishment winning papers, and the CITAC committee on and mixture-models) relative to the performance of traceability links, certified reference behalf of the members wants to congratulate of a number of commonly used or recently materials to facilitate one aspect of traceability, Venkatesh Iyengar, Bertil Magnusson et al and proposed evaluation metrics. and proficiency testing, among others. David L. Deuwer with the selection of their Abbreviated versions of the papers are published papers and the contribution made to metrology. Bertil Magnusson, Teemu Näykki, Håvard in this newsletter. The readers of CITAC News The authors will each receive a "CITAC Award Hovind and Mikael Kryssel, Handbook for are invited to access the full documents. Winner" certificate at the next CITAC Members' Calculation of Measurement Uncertainty meeting in 2008. Results of the CITAC award in Environmental Laboratories published Dr. Wynand Louw procedure (including abstracts of the papers) by Nordtest Tekniikantie 12, FIN-02150 Espoo, Award Coordinator will be published in ACQUAL and other journals. Finland; www.nordtest.org NMISA, South Africa

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estimate of defined confidence. The source of value with about 68 % confidence, u(xij) [4]. For every datum in these studies is fully attributed. normal distributions .

Reliable RVs, assigned either by gravimetric Just as each measurement kernel, N(xij,u68(xij)), sample preparation or extensively debated expert represents the expected probability density review, are available for all measurands. function (PDF) of the true location given the

measurement, the sum of the nj kernels defines a Data mixture-model PDF (MM-PDF) for the combined As of October 2007, data are publicly available for set of measurements . 171 Key Comparison (KC) measurands evaluated This alternate kernel density and PDF by the member organizations of the CCQM [3]. representation of the CCQM measurements is also displayed in Figure 1. The PDF at the right KCs are formal studies designed to establish j the extent of measurement agreement among of the graph is a marginal distribution for the It is widely accepted that knowledge of the the participating CCQM member organizations combined results. expected uncertainty of a measured value is and their official delegates for necessary for judging the measurement’s fitness- particular measurands. All of the for-purpose. Considerable effort continues to measurement values submitted be expended on how to best estimate and report for a particular KC are made measurement uncertainty (MU) for chemical public with the formal acceptance and biological measurands. It is therefore of the study’s Final Report. perhaps surprising that some experienced data Depending on the type of sample analysts argue against using MU to help estimate and measurands investigated, consensus values for interlaboratory studies some form of RV is established 1 2 [ , ]. for all measurands. Many of these RVs are assigned through The primary concern of those who advise gravimetric preparation verified against using MU is that estimating MU is not by measurement, others are yet sufficiently routine and standardized to assigned through a combination ensure that different participants interpret of consensus technical judgment and report the uncertainties in their values and statistical analysis. No in a consistent manner. Any enquiry into the participant’s KC result can be potential utility of MU for assigning consensus withdrawn from publication values to interlaboratory study materials once submitted; however, results therefore requires, at a minimum, that there be that are technically suspect are Figure 1. Measurement Equivalence Graph for CCQM- philosophically consistent MU estimates for all generally not used in assigning RVs. K11: Total Glucose in Human Serum, Material I of the reported measurements and trustworthy reference values (RVs) for the studied Measurement results for all KCs must be reported Location Estimators measurands. Few, if any, “routine” interlaboratory as values with an associated MU of defined studies currently meet this standard. There are a very large number of summary confidence. For all of the data in the published statistics that are routinely used or have been CCQM studies, the confidence intervals are proposed for estimating a measurand’s “true Beginning in 1993, a number of very non-routine symmetric about the expected value and are value” from interlaboratory study results. Each interlaboratory studies involving various expanded with the intent to include the true of these location estimators makes somewhat chemical measurands have been performed value with about 95 % confidence. The data for different assumptions about the nature of the data under the auspices of the Consultative th th the i participant in the j data set can thus be being combined and summarized. The extent of Committee for Amount of Substance – denoted: x ±U (x ) and displayed as a dot-and- ij 95 ij agreement between the estimated location and Metrology in Chemistry (CCQM). The member bar in a measurement equivalence graph as in “truth” depends upon how well the observed organizations of the CCQM have considerable Figure 1. However, since all of the MUs in these data match these underlying assumptions. Only expertise in chemical metrology and experience CCQM studies are expressed as symmetric 95 % a few, hopefully representative, estimators are with MU evaluation. All of the samples used in confidence intervals, the CCQM measurements examined in this report: the MU-ignoring mean, the CCQM studies are thoroughly characterized can also be interpreted as normal kernel densities median, H15, L1 ½ and shorth; and the MU-using for homogeneity and stability.All of the individual with expected value x and standard deviation ij Graybill-Deal (WtU) and Mandel-Paule (WtMP) values are reported with a symmetrical uncertainty proportional to U (x ) but covering the true 95 ij weighted means and the relatively novel MM-

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PDF-based MMmode, MMmedian and MMshorth. challenges presented in the evaluation of the 171 most of the robust MU-ignoring estimators: Except for the mean, the MU-ignoring estimators measurands will have similar score coefﬁcients, while chemical MU estimates can provide useful are relatively robust to “outlier” values. The WtU cmn, where m is the estimator (row) index and n information, as always the devil is in the details has been recommended as the “best” estimator is the factor (column) index. It is convenient to of how that information is used. when all of the xij are believed to represent quantitatively summarize the similarities of the a single normally distributed population and different estimators with the Euclidean score The article is extracted (and lightly updated) all U95(xij) are credible [5]. The WtMP has from: Ales Fajgelj, Maria Belli, Umberto been recommended for use when some of the distance: , Sansone (Eds). Combining and reporting

U95(xij) may be underestimated. The MMmode analytical results. Royal Society of Chemistry, is the location where the MM-PDF is largest, where p and q are the row designations for London (2007), pp 127-142. the MMmedian is the location which divides two estimators. Should the two estimators the PDF into two sections of equal area, and have exactly the same properties, the value of References the MMshorth is the mid-point of the shortest Dp,q will be 0.0; the value of Dp,q will increase as interval that spans half of the area of the PDF. the similarity between the estimators’ behavior 1. P.J. Lowthian, M. Thompson. Bump-hunting These and other estimators are fully deﬁned in decreases. for the proﬁciency tester – searching for the complete report and elsewhere [6,7]. multimodality. Analyst, 2002, 127, 1359. 2. M.G. Cox. A discussion of approaches for Figure 2 displays the Dp,RV for the ten estimators examined relative to the RV. The estimators determining a reference value in the analysis Results and Discussion are sorted in order of decreasing similarity to of Key-Comparison data, NPL Report CISE 42/99. 1999. www.npl.co.uk/ssfm/download/ As discussed in the complete report, the majority the RV. These distances suggest three broad nplreports.html of the CCQM KC measurement values agree well conclusions. First, none of the estimators 3. BIPM. kcdb.bipm.org/AppendixD/default.asp with the assigned RVs and most MU estimates provides locations that are closely related to 4. P. Ciarlini, M.G. Cox, F. Pavese. G. Regoliosi. appear realistic. However, about 10 % of the x the RV: unguided statistics do not replace ij The use of a mixture of probability are location “outliers” (more than two dispersion expert evaluation. Second, of the estimators distributions in temperature interlaboratory units from the RV) and about 30 % of the U (x ) evaluated, the MMmedian is the most similar 95 ij comparisons. Metrologia, 2004, 41, 116. are under-estimated (the x ±U (x ) interval to the RV: chemical MU estimates can provide ij 95 ij 5. M.G. Cox. The evaluation of key comparison does not include the RV). Given data. Metrologia, 2002, 39, 589. these imperfections and the number 6. D.L. Duewer. A robust approach and diversity of the measurands, the for the determination of CCQM key KC data should present the various comparison reference values and estimators with a variety of non- uncertainties. Working document ideal data structure to challenge CCQM/04-15, BIPM, 2004. www.bipm. their performance. Comparison of info/cc/CCQM/Allowed/10/CCQM04- the estimator values to the assigned 15.pdf RVs over all of the KC data sets may 7. D.L. Duewer. A Comparison of thus provide a realistic assessment of Location Estimators for Interlaboratory estimator properties. Data Contaminated with Value and Uncertainty Outliers. Submitted to The expected location of each of the Accreditation and Quality Assurance, in 171 publicly available CCQM KC data press (15-Feb-2008). sets was estimated with the various 8. PDF_Maker, available on request location estimators described above from [email protected] using purpose-built spreadsheet 9. R.G. Brereton. Chemometrics: software [8]. The redundancy in Data Analysis for the Laboratory the resulting 11 row (10 location and Chemical Plant, Wiley, estimates plus the assigned RV) by 171 Chichester, 2003. www.chm.bris.ac.uk/ column (measurands) data matrix was Figure 2. Factor-Score Distance of Location Estimators to org/chemometrics/ removed using principal components Reference Values analysis [9]. The resulting 11 row Dr. David L. Duewer by 10 abstract-factor score matrix NIST captures 100 % of the covariance information quantitatively useful location information. Third, USA contained in the original data matrix. Location the (MU-using) WtU and WtMP weighted mean estimators that respond similarly to the various estimators are less similar to the RV than are

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By using existing and experimentally determined quality control (QC) and method validation data, the probability of including all uncertainty contributions will be maximised.

Flow Scheme for Uncertainty Calculations The flow scheme presented forms the basis for the method outlined in this B. Magnusson T. Näykki H. Hovind M. Krysell handbook. The flow scheme, involving 6 defined steps, should be followed in all cases. The aim with this handbook is to provide a Eurolab guide 2007 (Measurement Uncertainty The example with NH4-N in water shows the practical, understandable and common way of revisited, www.eurolab.org). The English version way forward for calculating the measurement measurement uncertainty calculations based [1] is available at www.nordicinnovation.net, uncertainty using the flow scheme. For each on already existing quality control and method Nordtest, Tecn. Report TR537. step, there may be one or several options for validation data for test procedures in routine finding the desired information. use. To illustrate the approach the estimation Introduction Background for the NH4-N example – automatic of measurement uncertainty for some routine There are several ways that a laboratory can photometric method: The laboratory has methods in environmental laboratories are choose to estimate measurement uncertainty participated in 6 interlaboratory comparisons presented. for results from a method in routine use. We recently. All results have been somewhat higher propose a model where either the reproducibility than the nominal value. The laboratory therefore The approach follows the general ISO and EA within-laboratory (Rw) is combined with concludes that there may be a small positive bias. guidelines for measurement uncertainty and estimates of the method and laboratory bias, On average, the bias has been +2.2 %. This bias uses the possibility of grouping the individual or the reproducibility sR is used more or less is considered small by the laboratory and is not uncertainty components into different categories. directly, ISO Guide 21748.The alternative way corrected for in their analytical results, but exists, The first category is the intermediate precision within a laboratory, here called reproducibility Table 1. Results for a laboratory from interlaboratory comparisons of NH4-N in water within laboratory, u(Rw) and the second category is the method and laboratory bias, u(bias). Exercise Nominal Laboratory Bias sR Number of The third category is the reproducibility from value xref result xi labs interlaboratory studies, u(R). The error model μg/L μg/L % % used is a simplification of the model presented 1999 1 81 83 2.5 10 31 in the ISO guide 21748. However the first and most important step 2 73 75 2.7 7 36 is always definition of the measurand and 2000 1 264 269 1.9 8 32 specification of the required measurement 2 210 213 1.4 10 35 uncertainty. Starting with this information the 2001 1 110 112 1.8 7 36 handbook then tries to cover all steps in the 2 140 144 2.9 11 34 analytical chain from the arrival of the sample in the laboratory until the data has been reported. x + 2.20 8.8 34 It is important to notice that vital parts of the RMS (Root Mean Square) 2.26 - total measurement uncertainty are not included, e.g. sampling, sample transportation. is to construct a detailed fish-bone diagram and and is thus another uncertainty component. It is recognised that while the recommendations calculate/estimate the individual uncertainty The data from the interlaboratory comparisons presented do form a valid approach to the contributions. This approach may prove very are shown in Table 1. For this method, the evaluation of measurement uncertainty for many useful when studying or quantifying individual main sources of uncertainty are contamination purposes, other suitable approaches may also uncertainty components. It has been shown, and variation in sample handling, both causing be adopted especially the EURACHEM/CITAC though, that in some cases this methodology uncertainty components. These uncertainty Guide (www.eurachem.com) which, in the underestimates the measurement uncertainty, sources are included in the calculations below. second edition, also stresses the use of method partly because it is hard to include all possible validation data. Another good source is the uncertainty contributions in such an approach.

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Table 2. Flow scheme for uncertainty calculations

Step Action Example – Ammonium NH4-N

1 Specify Measurand Ammonium is measured in water according to EN/ISO 11732/11/. The customer demand on expanded uncertainty is ± 10 %

Quantify R comp. A: Control limits are set to ± 3.34 % 2 w A control sample (95 % conﬁdence limit) B possible steps not covered by the control sample B: The control sample includes all analytical steps.

3 Quantify bias components From interlaboratory comparisons over the last 3 years the % difference from nominal value were 2.4; 2.7; 1.9: 1.4; 1.8: and 2.9. The root mean square (RMS) of the bias is 2.26 %. The uncertainty of the nominal values is u(Cref) = 1.5 %. (see Table 1)

4 Convert components to Conﬁdence intervals and similar distributions can be converted standard uncertainty u(x) to standard uncertainty [2,3]. u(Rw) = 3.34/2 = 1.67%

=√2.26²+1.5² = 2.71%

5 Calculate combined standard Standard uncertainties can be summed by taking the square root uncertainty, uc of the sum of the squares

u1 6 Calculate expanded uncertainty, The reason for calculating the expanded uncertainty is to reach a high enough conﬁdence (app. 95 %) in that the “true value” lies within the interval given by the measurement result ± the uncertainty. % or 7 %.

* (u(bias) denotes the uncertainty contribution from the bias estimate to the measurement uncertainty. It is not the uncertainty of the bias value. The bias is here estimated by single results (differences) from PT rounds. If CRM is used several determinations over a longer timeperiod of each CRM is used to estimate the bias.

The measurement uncertainty for NH4-N will thus be reported as ± 6 % or 7 % at this concentration level.

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Table 3. Summary table for uncertainty calculations

Summary table for uncertainty Value Relative Comments calculations u(x) The results of the calculations done in the ﬂow scheme will then be summarised in a Reproducibility within-laboratory, Rw summary table. Control sample Rw Control limits is set 1.67 % Ammonium in water by EN/ISO 11732 = 200 μg/L to ± 3.34 % Measurement uncertainty U (95 % Other components -- conﬁdence interval) is estimated to ± 7 Method and laboratory bias %. The customer demand is ± 10 %. The calculations are based on control chart Reference material bias -- limits and interlaboratory comparisons. bias RMS Interlaboratory bias= 2.25 % 2.71 % comparisons u(Cref) = 1.5 % Combined uncertainty, uc is calculated from the control sample limits and bias estimation from interlaboratory Recovery test bias -- comparisons. The sR from interlaboratory comparisons [4] using the same method Reproducibility between laboratories can also be used if a higher uncertainty Interlaboratory R -- 8.8 % Data - see Table 1 estimation is acceptable. comparisons

Standard method R -- 8 % EN/ISO 11732 at level 200 μg/l

Table 4. Measurement uncertainty for Ammonium in water

Measurand Combined Uncertainty uc Expanded Uncertainty U

Ammonium 3.18 · 2 = 6.4 7 %

Theoretical Part of the Handbook It is full compatible with the GUM principles, the use of repeatability, reproducibility and In the following sections of the handbook the however not giving and details of the magnitude trueness estimates in measurement components within-laboratory reproducibility of different uncertainty sources that would be uncertainty estimation. ISO, Geneva. and bias are treated in detail as well as obtain needed for further optimization of the method measurement uncertainty from interlaboratory but this approach combining within-laboratory data. reproducibility with bias uncertainty covers most Dr. Bertil Magnusson of the individual uncertainty components. SP Technical Research Institute Examples Part of the Handbook Sweden In this section are given some examples of References uncertainty calculations and also an example with 1. Nordtest technical report 537, Mr. Håvard Hovind the concentration dependence of measurement www.nordicinnovation.net NIVA uncertainty 2. BIPM, IEC, IFCC, ISO, IUPAC, IUPAP, OIML Norway (1995). Guide to the expression of Conclusions uncertainty in measurement. (GUM). ISO, Dr. Mikael Krysell This handbook has now been used for several Geneva Euroﬁns A/S years and has been found to give reliable 3. EURACHEM/CITAC (2000). Quantifying Denmark estimates of measurement uncertainty for Uncertainty in Analytical Measurement methods in routine use where a quality control is (QUAM). 2nd Internet edition. 2000. www Mr. Teemu Näykki in place and validation data for the bias estimate eurachem.ul.pt, last accessed April 2006. SYKE can be obtained. 4. ISO (2004) ISO/TS 21748 Guidance for Finland

● CITACCITAC NEWS NEWS ● FEBRUARY FEBRUARY 2008 2008 / /29 29 AAwardward WWinnersinners 20072007

Metrological Concepts for Enhancing the Reliability of Food and Nutritional Measurements

the extent of variability of results due to this measurement uncertainties are assessed), and must be understood for a meaningful data procedures adopted for assessment of sampling interpretation (Iyengar 1989). The sampling metrology issues. In addition, inter-disciplinary part of the metrology reflects its own problems: (physiological and nutritional) expertise is also valid sampling through sample quality, required. Other measurements assessed by quantity, validity and stability (Heydorn 1984). indirect methods include body composition, Identifying sources of uncertainty followed by dietary energy intake and energy expenditure by establishment of traceability (i.e. internationally traditional methods that lack evidence of a proven accepted credibility links) of measurements in traceability link. However, these deficiencies life sciences can be accomplished by adopting are amenable for metrological improvements metrological concepts used in physical and using stable isotope techniques based on single chemical measurements. or double-labeled water and utilizing mass Metrology is a specialized discipline that deals spectrometry for ratio measurements. In this with the science of measurements irrespective Metrology in physics and chemistry is well context, it should be stressed that systematic of the field of application and regardless of advanced, although not in all cases with respect studies designed for estimating measurement the size of the measurement uncertainty. to chemical measurements. The high accuracy uncertainties are lacking (Iyengar and Parr 2005). Incorporating metrological approaches into the measurements in physics for length, mass, time, Bone mineral density as a tool for nutritional measurement process enhances the reliability temperature, electric current, etc., are carried assessment (e.g. Ca nutrition and osteoporosis) of analytical findings. These developments out by definitive methods (measurements based using dual-energy X-ray absorption method is include: high quality reference standards, on a specific natural phenomenon). Metrology another example, since multiple parameters validated methods, robust sampling practices, in chemistry is also advanced as demonstrated have to be met for a valid measurement to be proven calibration approaches, natural matrix by physical chemistry (e.g. molar relationships, accomplished. reference materials, speciation chemistry, volume, pressure, etc), which follows the assessment of measurement uncertainty and principles of metrology in physics. Further, Broader application of metrological concepts establishment of traceability links, certified examples are available through classical analytical for food and nutrition (F&N) measurements is reference materials to facilitate one aspect of chemistry (e.g. gravimetry for preparing high still in its infancy. The silver lining is that many traceability, and proficiency testing, among purity standards, related definitive analytical of these measurement processes are amenable others. techniques, among others). However, a for harmonization and facilitate comparability transition is seen in dealing with chemical (a vital requirement when results from different A comprehensive assessment of dietary intake of measurements in complex chemical matrices laboratories are evaluated). Comparability is nutrients and toxicants involves measurements (mixed entities, complex compositions), as it broadly understood here as internationally that encompass physiological and metabolic adds an additional parameter, namely indirect recognized measurement procedures offering processes. In this context, it is essential to measurements (e.g. AAS determination of Zn in some degree of flexibility to address the SI understand (i) the impact of the potential sources foods, mixed diets). This practice is common in issue because of practical reality faced in of errors arising from the “bio”dimension field assays and calls for extra steps to account F&N laboratories (de Bievre 2004). Examples of a living system, and (ii) how to minimize for traceability to satisfy reliability concerns. are: successful integration of metrological such errors to enhance the reliability (i.e. principles into food safety (i.e. food labeling) reduce uncertainty) of the analytical findings. Metrology in biology (i.e. metabolic, physiologic, measurements by internationally accredited The sources include: (i) conceptual errors clinical, food, nutritional and toxicological laboratories; certification of natural matrix arising from our limited understanding of the measurements, etc.) requires that biological food based materials for fat, protein, and other presampling factors such as biological variations, parameters should also be considered as part of dietary measurements (Sharpless et al 1997); short- and long-term variations reflecting an analytical evaluation. This is particularly true and the IAEA database for reference materials influence of food intake, environmental impact when measurements such as the bioavailability (Arunachalam et al 2006). and seasonal variations (e.g. variation of iodine of nutrients are carried out in human subjects. content of milk), among others (Iyengar 1982); Typically, the bioavailability measurement F&N metrology is an emerging discipline and (ii) analytical errors stemming from sampling, involves knowledge of nutrient composition the public health and nutrition investigators sample preparation and matrix effects. of the food, chemical species of the nutrients, should develop awareness for current concepts Variations arising from biological properties methodologies used (definitive or indirect in measurement practices. It is essential for and pathological shifts are identifiable but are methods, and if indirect, what measures are projecting the reliability of food compositional not always quantifiable (Iyengar 1981). Yet, adopted to account for traceability and how data, among others. Food safety has become

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a global issue and it should be recognized that forgotten agenda in our academic practices (de comparability of results in food measurements: in some parts of the world, movement of foods Bievre (2004). a CCQM workshop at BIPM on comparability has assumed the status of borderless-trade. In and traceability of food analysis. Accred. this context, integration of metrology into F&N References Qual. Assur. 9, 521-522. measurements strengthens the very base of 1. Iyengar, G.V. (1982). Presampling factors 7. Sharpless, K.E., Schuller, B., Margolis, S.A., the institutional measurement infrastructure in the elemental composition of biological Thomas, J.B., Iyengar, G.V., Colbert, J.C., efforts supported by the Food and Agricultural systems. Anal. Chem. 54, 554A-558A. Gills T.E. and Wise, S.A. (1997). Certification Organization (FAO 2004). 2. Iyengar, G.V.( 1981). Autopsy sampling and of Nutrients in SRM 1846:Infant Formula. J. elemental analysis: Errors arising from post- AOAC International, 80, 611-621. mortem changes. J. Pathology, 134, 173-180. 8. Arunachalam, J., Bleise, A., Mahwar, R.S., In conclusion, the society, as a client and as an 3. Iyengar, G.V.( 1989). Elemental Analysis of Ramadevi, P., and Iyengar, G.V. (2006). The end-user, looks at quality assurance (QA) in natural matrix reference material database terms of net economic benefits gained by solving Biological Systems. Vol. 1, CRC Press, Boca of the International Atomic Energy Agency: real-life problems that contribute to national Raton, FL. development. Thus, economic benefit can serve 4. Heydorn, K. (1984). Neutron Activation Reference materials in support of as a measurable parameter, demonstrating the Analysis for Clinical Trace Element Research. dietary investigations. J. Food Comp. Analysis, role of QA in a larger context. Steps undertaken Vol. 1, CRC Press, Boca Raton FL. 19, 241-249. to strengthen laboratory outcomes infuse 5. Iyengar, G.V. and Parr, R.M. (2005). 9. FAO (2004). OCEANIAFOODS Laboratory authority to the F&N measurements as a whole International Atomic Energy’s contributions gains accreditation for nutrient analyses. and therefore, enhance the value of ensuing to advances in nutritional http://www.fao.org/infoods/data2_en.stm public health decisions. In addition, integration of and environmental metrology. Accred. Qua.l metrology into F&N measurements strengthens Assur. 10, 393-402. Prof. Venkatesh Iyengar the very base of nutrition education, a nearly 6. De Bievre, P (2004). Traceability and Tufts University, USA

IV International Brazilian Congress on Chemical Measurements, Traceability and Quality Assurance

The Congress was held in São Paulo, a city that Brazilian Network of Measurements in Chemistry three years. This was an important moment for does not deny its work mania and business (RBMQ) provided insights on the impact of us, the user community and for the Congress. vocation. It was the efforts of its citizens that measurements of known quality to national At the beginning of next year we will publish a made São Paulo the most important State of productivity and international competitiveness. book for the proceedings, including papers, Latin America, in the economic aspect. presentations, talks, summary of meetings and The Congress was focused on issues concerning courses. The Congress photos are available at About 210 attendees including twenty four both theoretical concepts and practical aspects the website www.metrologiaquimica.org.br specialists from twenty different countries took for providing traceability and increased quality part in the Congress. There were researchers of chemical measurements. It was an important In addition I can say, São Paulo wasn’t all about and practitioners from the international and forum for exchanging information among leaders the work. Thousands of cultural events, excellent Brazilian communities of testing, calibration and of national and international communities. The restaurants, malls, shows, exhibitions, bars other industrial laboratories, research centers, presentations, courses and discussions focused and one of the best nightlife in the world also technological institutes and universities, from on concepts and tools for establishing primary attracted the attention of Congress participants. government and several economic sectors and references and disseminating traceability for It was really pleasure. geographic regions. In particular, participation chemical measurement results. of members of the Cooperation on International Dr. Vera Maria Lopes Ponçano Traceability in Analytical Chemistry (CITAC) The 22nd CITAC Members' Meeting was held President of the Organizing Committee enhanced the quality and scope of the Congress. during the Congress where new ofﬁcers were IV Metrochem The participation of several members from the elected to lead the organization for the next IPT, Brazil

● CITACCITAC NEWS NEWS ● FEBRUARY FEBRUARY 2008 2008 / /31 31 MMeetinge e t i n g RReportse p o r t s Workshop on Sampling Validation, Quality Control and Uncertainty Estimation

The First International Workshop on Validation, Workshop contents Participant satisfaction Quality Control and Uncertainty Estimation of The workshop presentations started with a Feedback demonstrated that the participants were Sampling was held in Hillerød, Denmark April general introduction to measurement, sampling, generally satisfied with 4 out of 5 (highest) being 14-15, 2007. The purpose of the workshop was and analytical uncertainty. Methods for estimating the most abundant mark. It is, however, difficult to present and discuss a new Nordtest handbook the uncertainty were listed and discussed. to satisfy all participants because of their very on uncertainty from sampling. The workshop Examples of an empirical method, the duplicate variable expectations, knowledge on the subject was attended by 60 experts from 15 European design, were presented more thoroughly and and theoretical background. countries. interpretation of the uncertainty estimations and fitness for purpose of the sampling methods Perspectives The Nordtest handbook were discussed. The workshop demonstrated, that methods The Nordtest Handbook is an extract of and and software are now available that allow for based upon the principles, methods and text After an introduction to the Nordtest handbook, estimation of the random contribution to sampling of the recently published Eurachem/EUROLAB/ the main general points in the handbook were uncertainty. For the systematic uncertainty CITAC/Nordtest/AMC Guide: Measurement highlighted: component, tools such as method studies for uncertainty arising from sampling: a guide to • Design of the sampling program, including method evaluation and sampler proficiency tests methods and approaches (available at http:// sampling purpose, sampling target, and for sampler performance evaluation are not www.eurachem.org. The handbook provides quality objectives readily available, and sampling reference sites for practical guidance on sampling uncertainty • Uncertainty in measurements-sources and both purposes have only been established for a estimation in the Nordtest handbook format and types of uncertainty few matrices. will be available at the Nordtest web site http:// • Principles of quality assurance in sampling- www.nordicinnovation.net/nordtest.cfm under validation and quality control. An additional outcome of the workshop was a NT technical reports, report number NT tec 604. Worked examples from the handbook were groundwater sampler proficiency test. It was Until the final report is available on the Nordtest presented on ground water monitoring, industrial organized by workshop participants in Denmark web site, a final draft of the Nordtest handbook is product control of iron ore, food sector control in the autumn of 2007 and further steps along this available at http://www.samplersguide.com This and waste water monitoring. road are in preparation. handbook is the latest in a series of handbooks on validation, quality control and uncertainty On the second day of the workshop, two Furthermore, a Eurachem workshop is arranged estimation of laboratory analysis and field presentations were demonstrating sampling for April 15-16, 2008 in Berlin entitled Sampling measurements, all available from the Nordtest uncertainty as the dominant source of Uncertainty and Uncertainty for Compliance web site. measurement uncertainty: one on sampling Assessment, see www.eurachem.org for more info. of waste water using variography and one on The main message of the handbook is that sampling of contaminated soil. For the soil Acknowledgements uncertainty from sampling can be estimated with example, it was shown that the evaluation of the The contributions of my co-authors of the reasonable efforts and following steps that are contamination level of a site was significantly Nordtest handbook, Bertil Magnusson, SP comparable to those used in quality assurance different when sampling uncertainty was Technical Research Institute of Sweden, Mikael of laboratory analysis: method validation included. The calculation tool used was robust Krysell, Ulla O. Lund and Kirsten J. Andersen, and quality control. The most useful tools in ANOVA, and a calculation program to perform Eurofins A/S, Denmark and Astrid Norbotten, sampling uncertainty estimation are replicate this, ROBAN, was demonstrated. Finally, group Food Safety Authority, Norway, as well as the measurements (random errors) and sampler work was done with the aim of giving the additional contributions as organizers and proficiency tests or method studies (systematic participants “hands on” experience of the tools lecturers at the workshop by Anke Oberender and errors). presented. Jette B. Hansen, DHI, Mike H. Ramsey and Katy Boon University of Sussex and Pentti Minkkinen, Table 1: Illustration of the combined use of validation and quality control of sampling Lappeenranta University of Technology, Finland are gratefully acknowledged. One method used for many sampling One method used repeatedly for one targets sampling target The Nordtest handbook and the workshop Initial validation yielding generic performance Target validation yielding the performance data for the were supported by Nordic Innovation Validation data for the method specific target and the method used Centre/Nordtest under contract 04130.

Quality control with target speciﬁc veriﬁcation Spot quality control verifying the performance data Quality control of generic method performance data consistency over time Dr. Christian Grøn DHI, Denmark

● 3232 / /CITAC CITAC NEWS NEWS FEBRUARY ● FEBRUARY 2008 2008 MMeetinge e t i n g RReportse p o r t s The 1st International Proﬁciency Testing Conference, Romania 2007

Motto: "There is no science without measurements, no quality without testing and no global market without standards."

The Commission of the European Union

The First International Proficiency Testing Norway, Portugal, Romania, Russia, Spain, Conference was organised by the Institute Sweden, United States, Thailand and Turkey of Research, Engineering and Consulting shared and disseminated their experience, for Cement, Lime and Plaster CEPROCIM knowledge and innovative ideas. SA, Bucharest, Romania under the auspices of the Research Excellence Programme The proceeding includes 64 papers, which CEEX initiated by the Romania's Ministry of were presented during the conference as Education and Research. The Conference oral, or poster presentations and they have was held between 11th and 13th October greatly contributed to the scientific and 2007, in Sinaia, Romania and was dedicated research activities and also to the professional to the specialists from the analysis and work. During the Conference proceedings, 8 testing laboratories in many fields (asphalt, exhibitors from Romania, United Kingdom biochemistry, bitumen, chemistry, and United States showed their products. construction materials, drugs, electrical Local Organizing Committee engineering, environmental, food and feed, (VTM); Uncertainty of measurement (UM); In the second day of the conference, the marine sediments, mechanics, metallography, Metrology and traceability (MT); Standardisation course “Training Metrology in Chemistry” metallurgy, microbiology, petrochemistry, (St); Research, development and education in the which proceeds under the responsibility of physics of lasers, plasma and radiation, plastics, laboratory activity (RDE); Accreditation, Quality TrainMiC® European Programme will provide precious metals, soils, textiles, veterinary management in testing laboratories (AQM). new information on issues related to the quality medicines, water, residual water, etc.). Approximately 150 specialists from 26 countries, of measurement results. namely, United Kingdom, Australia, Belgium, The themes of the conference included: Bulgaria, China, Croatia, Denmark, Estonia, Dr. Graziela Guslicov st Proficiency testing schemes (PTS); Reference Finland, France, Germany, Greece, Hungary, 1 Proficiency Testing Conference Pres. materials (RM); Validation of testing methods Ireland, Israel, Lithuania, The Netherlands, Romania

BERM 11 11th International Symposium on Biological and Environmental Reference Materials October 29 - November 2, 2007, Tsukuba, Japan

The 11th International Symposium on Biological by about 180 participants from 19 countries and measurement process, with emphasis on and Environmental Reference Materials (BERM various fields/sectors. CRMs related to public health, such as clinical 11) was held on October 29 - November 2, 2007, As a continuation of the symposia series, held laboratory medicine, food safety and nutrition at the Tsukuba International Congress Center alternately in the EU and the USA since 1983, labeling, and environmental monitoring. A EPOCHAL in Tsukuba, Japan. BERM 11 was the BERM 11 was intended as a forum to address special emphasis was also placed on the Asian first BERM held in the Asia-Pacific region and issues related to the development of biological CRM (ACRM) network program between China, also the first big event on metrology in chemistry and environmental reference materials and Korea and Japan. hosted by the National Metrology Institute of their role in the quality assurance of analytical Japan (NMIJ) since its establishment in 2001. It measurements. The scientific program of BERM The symposium comprised 11 oral sessions with was a very successful symposium and attended 11 focused on the role of CRMs in the analytical 75 presentations including invited lectures and 2

● CITACCITAC NEWS NEWS ● FEBRUARY FEBRUARY 2008 2008 / /33 33 MMeetinge e t i n g RReportse p o r t s

poster sessions with 84 papers. The sessions and •L. Sander (NIST) “Analytical methods for Development of analytical techniques invited talks were as follows: analysis of botanical dietary supplements” • N. Furuta (Chuo U) “Bulk analysis and single particle analysis of size-classified International activities on metrology in Biological RMs airborn particulate matter” chemistry • H. Emons (IRMM) “Reference materials for • G. Turk (NIST) “ICP emission spectrometry • R. Kaarls (CIPM/CCQM) “CCQM activities on life sciences from IRMM” for high-precision comparisons of elemental metrology in chemistry” • M. Salit (NIST) “Standards and measurement standard solutions” • R. Wielgosz (BIPM) “BIPM international assurance for microarray gene expression comparisons in support of the equivalence of measurements” RMs for proficiency testing chemical measurements” • S- R.Park (KRISS) “Development of higher • Y. Mitani (CENAM) “roficiency testing scheme • H. Emons (IRMM) “Towards further order analytical methods for certification of internationally harmonized guidance on DNA reference materials” for harmonization and comparability of reference mateials - from REMCO to analytical measurement” application notes” RMs and QA/QC for laboratory medicine • I. Kuselman (INPL) “Traceability, • S. Wood (LGC) “Guidance for the production • J. Betz (NIH) “Development and use comparability and compatibility of of non certified reference materials” of certified reference materials for biomedical pro ficiency testing results based on the use • S. Ellison (LGC) “International guides on research applications” of reference materials as test items” measurement uncertainty” • K. Kuwa (Tsukuba U) “Proficiency teting activities at JCCLS using human pooled Asian collaboration on CRM development Recent development of CRM production serum and matrix reference materials in • H-Y. So (KRISS) “Asian CRM network • A. Herrero (IRMM) “New challenges for laboratory medicine” program, activities at KRISS” reference materials in the Omics era” • C. Cherdchu (NIMT) “The first activity on • S. Wise (NIST) “Recent trends in the RMs in food and safety chemical reference material production at development of environmental, food, dietary • A. Yasui (NFRI) “Food CRMs and PTs in National Institute of Metrology (Thailand)” supplement, and clinical nutrition SRMs” Japan” • K.Chiba (NMIJ) “Recent NMIJ Activities in the BERM 11 was closed after the presentation by Dr. certi fied reference material program” Environmental RMs K. Okamoto, Chair of BERM 11, on “30 years on • S. Wood (LGC) “Production of certified • H. Haraguchi (Nagoya U) “Certified reference reference materials at LGC” materials required for metallomics research” reference materials; my first-, second- and third- • J. Vogl (BAM) “Reference material generation reference materials” characterization by IDMS applying multi Greenhouse gas RMs collector instruments” • H. Mukai (NIES) “Standards for GHGs and Dr. Kensaku Okamoto • H. Emteborg (IRMM) “IRMM’s reference ozone monitoring in Japan” NMIJ, Japan materials for food and environmental analysis”

BERM 11 participants at the end of a conferece day

● 3434 / /CITAC CITAC NEWS NEWS FEBRUARY ● FEBRUARY 2008 2008 AAnnouncementsn n o u n c e m e n t s

THE REVISED VIM IS OUT! The revised VIM: “International Vocabulary of In addition, a draft report of the IUPAC project MB)” from where you have access to the full Metrology – basic and general concepts and “Metrological Traceability of Measurement Results document. I am available for further questions associated terms (VIM) ISO/IEC 99” can be in Chemistry” is out for public scrutiny on the and information on both the revised VIM as well purchased from ISO since 2007-12-14 on the IUPAC website: http://www.iupac.org/projects/ as on the IUPAC project, that includes specialized address: http://www.iso.org 2001/2001-010-3-500.html “Control + click” lectures and seminars on the above documents, Look for “ISO/IEC 99”. on the above html and you access the project description; at the end of the project description, if so desired. In February/March 2008, it will be hyperlinked to go to “provisional recommendations”; at the end the BIPM website where it can then be accessed of these, you will ﬁnd: “download full text of the Prof. Paul De Bièvre and downloaded for free: www.bipm.org Provisional Recommendations (pdf ﬁle - 1.28 Consultant, Belgium

Symposium: Advances in Understanding-Chemical Measurement Quality Societal Impact, Turin, 18-19 September, 2008

The aim of this symposium, organised by the Examples will cover measurement quality in Bertil Magnusson, SP Technical Research Institute Division of Analytical Chemistry (DAC) of areas such as environment, health, industry, of Sweden ([email protected]), Enzo EuCheMS in cooperation with EURACHEM trade, and forensics. Ferrara, Istituto Nazionale di Ricerca Metrologica, (website: http://www.euchems-torino2008.it/ Italy ([email protected]), and representing DAC is site/home.asp) is to demonstrate the impact of Short contributions and posters covering all the Bo Karlberg, Stockholm University, Sweden (bo. measurement quality on various societal activities areas are welcome. [email protected]) based on analytical chemical measurements. The conveners representing EURACHEM are

The 17th International Conference of the Israel Society for Quality November 18-20, 2008 Jerusalem, Israel

It is a privilege to invite you to take part in the We look forward to welcoming you and your • Measurement methods and their validation 17th International Conference of the Israel colleagues in Jerusalem. • Measuring instruments and their qualiﬁcation Society for Quality, to be an active partner • Measurement standards (etalons) and in a challenging and fruitful endeavor and to Dr. Ilya Kuselman reference materials (RMs) contribute to its success. CITAC Chairman • Uncertainty estimation in measurement and INPL, Israel testing/chemical analysis The Israel Society for Quality biannual • Traceability, comparability and compatibility international conferences are very popular Metrology Track Topics • Inter-laboratory comparisons and proﬁciency and generally attract 1700-2000 participants. • Trends in metrology testing (PT) Both specialists in metrology (measurement, • Metrology as a business • Conformity assessment calibration and testing, including chemical • Metrology in chemistry, petrochemistry, • Accreditation of calibration and testing/ analysis) and quality professionals will again pharmaceuticals, environmental and clinical analytical laboratories, RM producers and PT have an opportunity to network with each other, analysis providers interact with senior management and learn how • Measurements of properties of nano-particles • Legal metrology to bring the “message” to as many people as • Software for metrology possible. • Teaching metrology and quality • Ethical problems in metrology The 17th Conference is supported by CITAC, which will organize a metrology track at the Abstracts of 200 words in MS WORD format are event. invited on all the suggested topics. For further information please see Joining us at the conference will also enable you www.isas.co.il/quality2008 or contact the to enjoy exploring the Land of Israel, birthplace Conference Secretariat at tel: +972-2-6520574, of the three great monotheistic religions. fax: +972-2-6520558.

● CITACCITAC NEWS NEWS ● FEBRUARY FEBRUARY 2008 2008 / /35 35 AAnnouncementsn n o u n c e m e n t s 6th Workshop on Proﬁciency Testing in Analytical Chemistry, Microbiology and Laboratory Medicine Rome (Italy), (5)-6-7 October 2008

The EURACHEM Proficiency Testing Working Full papers, to be submitted for peer Group www.eurachem.org, in co-operation review, drafted according the journal with CITAC www.citac.cc and EQALM recommendations, should be delivered to www.eqalm.org, welcomes you to attend the the Workshop Secretariat, before or at the 6th event of a series of workshops addressing workshop (electronic format or as 6 printed current practice, problems and future copies). directions of interlaboratory comparisons in chemical and biological analyses. These Venue events are structured to include both key-note One of the most ancient cities in Europe, lectures and discussions in working groups, founded over 2700 years ago, Rome has to enable interactive participation and cross- will be organised on the day before the workshop become the biggest open-air museum in fertilisation of ideas. (5th October), providing opportunities for Europe. Heritage, complemented by pleasant training for both PT/EQA organisers and end- weather, Italian cuisine and a lively atmosphere, users. continues attracting visitors over the centuries. Scope of the Workshop Completely opposite styles of art and life manage Focus is on developments in Proficiency Testing Who Should Attend? to live side by side here making Rome a unique (PT) and External Quality Assurance/Assessment PT/EQA scheme organisers, QA managers, city. Rome is located in the middle of the Italian (EQA) in analytical chemistry, microbiology and internal and external assessors, participants in peninsula, at the centre of the Mediterranean laboratory medicine. Lectures, presented by PT/EQA and the laboratories' customers. basin. Connections with the rest of Italy and the invited speakers, and working group tasks will Support to delegates from developing countries world are assured by means of two airports and highlight the following topics: can be sought applying to: excellent highway and train systems. ● Frequency of PT/EQA and monitoring Umberto Sansone, International Atomic performance over time; Energy Agency (IAEA), Agency's Laboratories The workshop will be held at ● Developments in PT/EQA within the EU; Seibersdorf, Chemistry Unit, A-2444 Seibersdorf Centro Congressi Frentani ● PT/EQA in developing countries; (Austria) Email: [email protected] (http://www.congressifrentani.it/?lang=eng), ● PT/EQA in microbiology; in the heart of the University district and on ● PT/EQA in forensic science; Contributions and Exhibitions easy reach from both Termini and Tiburtina ● The new standard for PT/EQA: ISO 17043; Poster contributions are welcome. railway stations. Further information on how to ● End-user perspective of PT/EQA; Abstracts, according to the instructions given get to the workshop venue is available on the ● Quality of test items used in PT/EQA. on the website, should be sent to the workshop workshop website and will be included in the secretariat by 15th June 2008. second circular (March 2008). Programme The workshop starts on 6th October. Four Products and services related to PT/EQA and Registration and Accommodation lectures will be given each morning followed laboratory activities can be presented in the The first circular, registration and hotel booking by the poster session and afternoon discussions exhibition area. Requests should be sent to the forms are available from the secretariat and on within working groups. Feedback from working workshop secretariat by 1st September 2008. the workshop website. groups will be presented each day at the closure session. Proceedings Workshop Secretariat The event shall be submitted for approval under Abstracts of invited lectures and accepted Phone: +390649902562 the Italian Ministry of Health Programme for contributions will be collected in an abstract Fax: +390649387077 Continuous Education in Medicine. book. All participants will receive a copy of the e-mail: [email protected] A get together party and a workshop dinner will book of abstracts. website: www.iss.it/eurachem be organised for participants and accompanying persons. Full papers of invited lectures and accepted contributions will be considered for publication Marina Patriarca, Antonio Menditto Opportunities for Training in a special issue of Accreditation and Quality Chairs of Local Organising Committee Two training courses, open to workshop Assurance (Springer Verlag). For example, Istituto Superiore di Sanità, Rome, Italy participants only, and addressing the topics: contributions from the previous edition of ● Statistics for Proficiency Testing this series of workshops were published in the Dr. Brian Brookman ● Selection, use and interpretation of PT/EQA special issue of Accred. Qual. Assur. 2006: 11(8- Chair of EURACHEM PTWG Schemes 9), 371-484 LGC Standards, UK

● 3636 / /CITAC CITAC NEWS NEWS FEBRUARY ● FEBRUARY 2008 2008 CCITACITAC SStrategytrategy fforor 22007-2010007-2010 ((Draft)Draft)

According to the CITAC Terms of industries, regulatory bodies, universities, purposes, history, developed documents References (TOR) adopted at the 22nd metrology, standardisation and accreditation and planned activities. CITAC Members' Meeting in Sao Paulo, bodies; Brazil, 17.07.07, the CITAC strategy for the In addition the following strategically next three years includes the following: 6. To organise seminars, symposia and important CITAC activities are planned for workshops and to participate in conferences 2007-2010: to promote the message of traceability; 1. To provide a broad international forum for 1. To prepare CITAC Bylaw; the exchange of information with respect to 7. To work closely with other international worldwide metrological traceability of organizations, e.g. CCQM/BIPM, ISO- 2. To check expediency, cost and possibility of results of chemical measurements; REMCO, IUPAC, ILAC, AOACI, regional the registration of CITAC as a legal entity in and national professional chemistry societies one of the member countries; 2. To assist analytical laboratories with tools and institutions, like EURACHEM and DAC- for establishing traceability to “stated EuCheMS, – without duplicating work 3. To renew the CITAC logo; references”; already being conducted by other groups – using these societies and institutions to 3. To share views, clarify important concepts act as a conduit to the field laboratories; 4. To attract to CITAC membership active and raise awareness of the needs and representatives of new NMIs, universities possibilities leading to traceability in 8. To organize annual nomination of and industry (individual CITAC members), chemical laboratories; the most interesting/important papers on as well as organizations, institutions and metrology in chemistry; companies (collective members); 4. To develop, distill and disseminate globally key traceability concepts and issues; 9. To prepare an annual newsletter "CITAC 5. To explore the possibility of consultation News" describing CITAC activities and to industry as a new CITAC activity. In 5. To prepare discussion and scientific international achievements in the field of the framwork of the consultation to initiate papers for journals in relation to traceability, metrology in chemistry; and, where needed, coordinate work for uncertainty and quality assurance issues, the harmonisation and validation of and guides for analytical laboratories, 10. To keep an updated website, informing analytical methods based on traceability which could play a bridging role between the community about CITAC and its and other metrological concepts.

Two new proposed logos

CITAC NEWS ● FEBRUARY 2008 / 37 MMessagesessages ffromrom NNewew MMembersembers

Message from Venkatesh Iyengar

CITAC’s role in IMEKO TC-19, TC-23 and TC-24 international should be introduced in such a way that the strengthening conference in Budapest in September 2008 and chosen students appreciate that it is a privilege, the application the proposed session on Food and Nutrition and the membership should be free of cost. of metrology in Metrology (F&N Metrology) at the International Further, a select group of young and upcoming various spheres Congress of Nutrition of the International Union professionals who are already in the measurement is self evident. of Nutritional Sciences in Bangkok in late 2009. arena should also be contacted, and they should Its dynamic be offered membership with very modest fee relationship with While CITAC is striving to strengthen the (starting with a no-fee introductory year). With many national metrological base in several areas across the time, this concept would mature and hopefully metrology world of measurement, it would be desirable a new and vibrant group of members would be institutes is a key to examine the ways and means for expanding developed. feature in its successful and effective networking. the membership base. In my view, this should CITAC’s growing mutually supportive relationship be done by casting the net to attract the student I am glad to be a member and will strive to with IMEKO through various technical committees community (those doing advance degrees in enlarge the young membership drive, if adopted is an excellent pathway to further strengthen several disciplines with links to metrology) as by CITAC. its ability to be a crucial player in spreading the well as the young professionals. With the help metrology message. We are likely to see further of the existing members in various countries, Prof. Venkatesh Iyengar consolidation of CITAC-IMEKO relationship an effort should be made to attract A Few Core Tufts University in speciﬁc future activities e.g. the proposed Student Members From Each Country. This USA

Message from Chainarong Cherdchu Having been best measurement and its traceability has become community has evolved enormously in all sectors elected as a an important element of my daily practice. during the past three years. I myself envision that new member of Metrology – the science of measurement – has participating closely and tightly with CITAC will CITAC is not only shed some light and underpin my belief of science further enhance the MiC activity for our Asian the matter of for human beings wealth and health. Certainly, region chemical metrology community greatly. honor but really it is a solution to one’s quality of life providing Therefore, I am looking forward to an active and attributed to that this quality system and the related ones have a fruitful collaboration among our Thai chemical several traceable been implemented properly and fairly. metrology, the CITAC and other organizations. consequences that I am experiencing CITAC mission – to improve traceability of the now. After joining results of chemical measurements everywhere Dr. Chainarong Cherdchu NIMT at the Department of Chemical Metrology – seems to catch our interest deeply since NMI and Biometry since October 2004 the value of the growth of metrology in chemistry in Thai Thailand

Message from Koichi Chiba

It is my great one of the most important elements for the very complicated. In Japan, as you know, BERM11 honor to be a measurement values and procedures. The was held in Tsukuba on October of last year, and new member of coverage fields of CITAC have expanded from a I believe that BEAR11 was a great opportunity for CITAC. CITAC conventional chemical metrology to new fields Japanese scientists to reaffirm the significance of has been playing such as bioanalytical and clinical chemical ones, traceability and to understand an international a great role in even after I joined chemical metrology in NMIJ trend in chemical metrology. I hope to contribute establishment of at Chemistry Division in 2002. The chemical to a fruitful collaboration among CITAC, Asian the traceability metrology is shining a light on an essential part regional chemical metrology community and concept in of science for our quality of life, that is, human chemistry and beings’ wealth, health, safety and so on. CITAC Japanese communities including NMIJ. dissemination of mission - to disseminate the traceability to all the idea to the chemical measurement fields the chemical measurements - is a main stream of Dr. Koichi Chiba and it becomes a worldwide success in recent analytical chemistry in all sectors, although the NMIJ years. The traceability is now recognized as traceability in chemistry in the real world is still Japan

38 / CITAC NEWS ● FEBRUARY 2008 CCITACI T A C MMembers’e m b e r s ’ LListi s t

Dr Celia Puglisi Prof Dr Hendrik Emons Prof Timo Hirvi INTI Institute for Reference Materials and Center for Metrology and Accreditation CC 157 Measurements (IRMM) P.O.Box 9 San Martin Joint Research Centre European Commission FI-02151 Espoo BUENOS AIRES 1650 Retieseweg 111 FINLAND ARGENTINA 2440 Geel Tel +358 9 616 74 50 Tel +54 11 4754 5151 BELGIUM Fax +358 9 616 74 67 Fax +54 11 4713 5311 Tel +32 14 571 722 E-mail timo.hirvi@mikes.fi E-mail [email protected] Fax +32 14 571 548 Dr Philippe Charlet (CITAC Secretary) Dr Laurie Besley E-mail [email protected] National Measurement Institute Laboratoire National de Métrologie et d'Essais PO Box 264 Dr Vera Ponçano (Past CITAC Chair) (LNE) Lindfield NSW 2070 Instituto de Pesquisas Tecnologicas 29, avenue Roger Hennequin AUSTRALIA PO Box 0141, Sao Paulo - SP 78197 TRAPPES Cedex Tel + 61 2 9449 0159 BRAZIL FRANCE Fax + 61 2 9983 1398 Tel + 55 11 3767 4540 Tel +33 1 30 69 21 95 E-mail [email protected] Fax + 55 11 3767 4009 Fax +33 1 30 69 12 34 E-mail [email protected] E-mail [email protected] Mr Alan Squirrell ILAC Secretariat Mrs Gabriela Massiff Dr Ioannis Papadakis 7 Leeds Street Fundación Chile Consultant RHODES, NSW 2138 Av. El Condor 844, Ciudad Empresarial Megistis 25, 17455 Alimos, Athens AUSTRALIA Huechuraba, Santiago GREECE Tel + 61 2 9736 8374 CHILE Tel +30 6977 190905 Fax + 61 2 9736 8373 Tel + 56 2 242 8180 Fax +30 2107 212909 E-mail [email protected] Fax + 56 2 242 8182 E-mail [email protected] Dr Ales Fajgelj E-mail [email protected] International Atomic Energy Agency Dr Arun K. Agrawal Wagramer Strasse 5, P.O. Box 100 Dr Tai Lun Ting National Physical Laboratory (NPLI) Vienna A-1400 Government Laboratory Dr K.S. Krishnan Marg AUSTRIA 7/F, Ho Man Tin Government Offices New Delhi - 110012 Tel + 43 1 2600 28233 88 Chung Hau Street, KOWLOON, Hong Kong INDIA Fax + 43 1 2600 28222 CHINA Tel +91 11 25734649 E-mail [email protected] Tel + 852 2 762 3701 Fax +91 11 25726938 Fax + 852 2 714 4083 E-mail [email protected] Prof Dr Wolfhard Wegscheider E-mail [email protected] (CITAC Treasurer) Dr Máire Walsh Dept. of General & Analytical Chemistry Prof Yu Yadong Consultant University of Leoben National Institute of Metrology (NIM) Newtown, Celbridge, Co. Kildare Franz-Josef Strasse 18 18, Bei San Huan Dong Lu, Chaoyangqu IRELAND A-8700 Leoben 100013 Beijing Tel + 353 1 6271522 AUSTRIA CHINA Fax + 353 1 6271522 Tel +43 3842 402 7000 Tel + 86 10 6427 1638 E-mail [email protected] Fax +43 8342 402 7012 E-mail [email protected] Fax + 86 10 6422 8404 E-mail [email protected] Dr Ilya Kuselman (CITAC Chair) Prof Dr Paul De Bièvre National Physical Laboratory of Israel (INPL) Independent Consultant on Metrology in Prof Dr Miloslav Suchanek Givat Ram, Jerusalem 91904 Chemistry EURACHEM-CZ ISRAEL Accreditation and Quality Assurance Department of Analytical Chemistry Tel + 972 2 5661856 Duineneind 9, B 2460 Kasterlee Institute of Chemical Technology (ICT) Fax + 972 2 6520797 BELGIUM 166 28 Prague 6 E-mail [email protected] Tel +32 14 851 338 CZECH REPUBLIC Fax +32 14 853 908 Tel + 42 02 20443685 E-mail [email protected] E-mail [email protected]

● CITACCITAC NEWS NEWS ● FEBRUARY FEBRUARY 2008 2008 / /39 39 CCITACI T A C MMembers’e m b e r s ’ LListi s t

Dr Koichi Chiba Dr Wynand Louw (CITAC Vice Chair) Mrs Cathy Burns National Metrology Institute of Japan (NMIJ) National Metrology Institute of South Africa Food and Drug Administration National Institute of Advanced Industrial Private Bag X34 6th Ave and Kipling St, DFC-Bldg 20 Science Lynnwood Ridge, 0040 Pretoria Denver, CO 80225 and Technology (AIST) SOUTH AFRICA USA Higashi 1-1-1 Tel +27 12 8414227 Tel +1 303 236 3021 Tsukuba Central 5-2, Tsukuba 305-8565 Fax +27 12 8413382 Fax +1 303 236 3551 JAPAN E-mail [email protected] E-mail [email protected] Tel + 81-298-61-4420 Fax + 81-298-61-4420 Dr Chainarong Cherdchu Dr Venkatesh Iyengar E-mail [email protected] Department of Chemical Metrology and Friedman School of Nutrition Science and Biometry Policy Dr Hun Young So National Institute of Metrology Tufts University Division of the Quality of Life, KRISS Thailand Boston MA P O Box 102 Yuseong, Daejeon 306-600 Tel +66-2-577 5100 ext 2342 USA KOREA Fax +66-2-577 5096 Tel +1-301 320 6274 Tel +82-42-868-5840 E-mail [email protected] E-mail [email protected] Fax +82-42-868-5800 E-mail [email protected] Dr Robert Kaarls Dr Willie May BIPM – CIPM - CCQM Analytical Chemistry Division NIST Dr Yoshito Mitani Nakanishi Klaverwydenstraat 13 100 Bureau Drive, ms 8390 CENAM ( Metrologia de Materiales) 2381 VX Zoeterwoude Gaithersburg, MD 20899-8390 Apdo Postal 1-100 centro THE NETHERLANDS USA CP 76000 Queretaro, QRO Tel + 31 71 580 22 31 Tel + 1 301 975 3108 MEXICO Fax + 31 71 580 47 77 Fax + 1 301 926 8671 Tel + 52 442 2110 560 E-mail [email protected] E-mail [email protected] Fax + 52 442 2110 569 E-mail [email protected] Dr Steve Ellison Mr Peter S. Unger Laboratory of the Government Chemist American Association for Laboratory Dr Laly Samuel Queens Road, Teddington Accreditation Measurement Standards Laboratory of New Middlesex, TW11 0LY 5301 Buckeystown Pike Zealand UNITED KINGDOM Frederick, MD 21704 Graceﬁeld Road, PO Box 31-310 Tel + 44 181 943 7325 USA Lower Hutt Fax + 44 181 943 2767 Tel + 1 301 644 3212 NEW ZEALAND E-mail [email protected] Fax + 1 301 662 2974 Tel + 64-4-569 0490 E-mail [email protected] Fax + 64-4-569 0003 Dr Bernard King E-mail [email protected] Analytical Measurement Consultant Dr. Wayne Wolf 25 Bolton Gardens, Teddington Beltsville Human Nutrition Research Centre Prof Yuri Karpov Middlesex, TW11 9AX Agricultural Research Service State R&D Institute of Rare Metals Industry UNITED KINGDOM US Department of Agriculture 5 B. Tolmachevskij Pereulok Tel + 44 208 977 2360 10300 Baltimore Blvd. 109017 Moscow Fax + 44 208 977 2360 Beltsville, MD 20705 RUSSIA E-mail [email protected] USA Tel +7 095 9538791 Tel + 1 301 504 8927 Fax +7 095 9538791 Dr Martin Milton Fax + 1 301 504 8314 E-mail [email protected] National Physical Laboratory E-mail [email protected] Hampton Road, Teddington Middlesex, TW11 0LW UNITED KINGDOM Tel + 44 181 943 6826 Fax + 44 181 943 6755 E-mail [email protected]

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