NNEWSE W S FEBRUARY 2010 FForewordo r e w o r d byb y thet h e ChairmanC h a i r m a n CITAC's Accent on Cooperation

of References 2007 and CITAC Strategy for formulating joint policies or documents, 2007-2010. The strategy for realization of participating in affairs and acting as an observer cooperation in practice included development at a meeting. A permanent CITAC liaison with of 1) CITAC membership, 2) a new CITAC a third party is organized on the basis of logo, 3) guidelines for liaison persons, 4) a official CITAC membership or observer status, procedure for the annual CITAC nomination according to the policy of the third party. In of the most interesting/important papers on particular, I am very satisfied by the decision MiC, 5) guidelines for CITAC projects, and 6) of the International Committee for Weights a procedure for CITAC participation in and and Measures (CIPM) at their 97th meeting support of conferences and workshops. in 2008 to accept CITAC as an observer of the Consultative Committee for Amount of A number of leading MiC specialists from Substance – Metrology in Chemistry (CCQM). different sectors of different economies from all continents were elected during the last years The annual CITAC nomination of the as CITAC members. Today there are 37 CITAC most interesting/important papers on Summarizing CITAC progress over the term members from 26 economies distributed by MiC, mentioned above, aims to highlight of my chairmanship, which is “suddenly” sectors as shown in Fig. 1. To emphasize the remarkable papers which may have not yet nearing completion, I would like first of all to worldwide character of this cooperation, the been “discovered” after their publication in congratulate the CITAC Award Winners – a new CITAC logo was depicted on a globe (see a national journal (in a local language); not good new tradition established during the last top of this page). readily accessible to the larger metrological/ three years. The most interesting/important analytical community; published in a papers on metrology in chemistry (MiC) by known international journal, but written in the CITAC version 2009 are: Luca Callegaro a sophisticated language, not clear enough et al. Accred Qual Assur (2009) 14:587-592; for the community; or simply papers that Samuel Wunderli and Hanspeter Andres. deserve attention because of their important Electroanalysis (2009) 21:1984-1991; and scientific content. This procedure, including Olaf Rienitz et al. Accred Qual Assur (2007) lectures by the authors of the winning papers 12:615–622 (see the message of Dr. Wynand at the closed CITAC members meeting and Louw, the Award Coordinator, and the author contributions to the CITAC News, contributions by the Winners in this issue of has allowed us to annually attract a number CITAC News). of prominent colleagues to CITAC activities, and thereby to add color and positive Since CITAC is an international organization, emotions to these activities. its members speak English with different accents. However, I am now happy to report Fig.1. CITAC members’ distribution by CITAC has a remarkable history of cooperation another accent developed in the last years by sectors. NMIs are national metrology with EURACHEM in the development of CITAC: the accent on cooperation with regional institutes; Int. Org. are international guidelines in the field of MiC, well known and international organizations active in the organizations. and widely used in analytical laboratories field of MiC. The purpose of this development throughout the world. Recently published was to increase the participation in CITAC documents are EURACHEM/CITAC Guide activities of specialists from wide chemical Liaison to regional and international “Use of uncertainty in the assessment of analytical and metrological communities, thus organizations in the field of MiC (third parties) compliance” and the EURACHEM/CITAC/ increasing CITAC productivity. is the important aspect of CITAC activities. EUROLAB/NORDTEST/AMC Guide “Estimation The Guidance on this topic outlines the duties of measurement uncertainty arising from Cooperation is an element of the CITAC and responsibilities of persons (liaisons) sampling”. In cooperation with IUPAC the acronym and one of the basic goals of the nominated to represent CITAC at meetings of first IUPAC/CITAC Guide “Selection and use CITAC co-founders in 1993. The only problem other organizations, in working groups, etc. of proficiency testing (PT) schemes for a is how to find optimal cooperation forms. In CITAC may liaise with third parties for a variety limited number of participants” was developed general, this task is described in CITAC Terms of reasons, such as negotiating an agreement, and published in 2010. Another project with

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IUPAC, “Investigating out-of-specification Isranalytica 2010 conference, January 19-20, Louw, the Vice-Chair, Dr. Philippe Charlet, (OOS) test results of chemical composition and the CITAC Workshop on January 21, Tel the Secretary, Prof. Wolfhard Wegscheider, based on metrological concepts”, is now Aviv, Israel. Organizers of a meeting related the Treasurer. Many thanks also to Dr. under development. The Guidelines for CITAC to MiC may apply for an “In cooperation Karin Schober, the Treasurer Assistant and projects will regulate planning and performing with CITAC” designation according to the Webmaster, and to every CITAC member who such projects with participation of specialists in Procedure for participation in and support of supported our work in any form, including MiC who do not need to be CITAC members. conferences and workshops by CITAC (the constructive criticism. The next Chair will documents mentioned above are available in be elected soon at the 25th CITAC Members Every year CITAC participates in the www.citac.cc). Meeting, LNE, Paris, April 11, 2010, according organization of international meetings in the to the CITAC Terms of References, and I wish fields of MiC and quality in analytical chemistry In conclusion, one can say that the past three him success. with local committees and other societies. years have been productive, but of course a lot For example, the International Congress on remains to be done. I would like to express Traceability in Laboratory Measurements my gratitude to the Executive Committee, Dr. Ilya Kuselman and Production Chains, São Paulo, Brazil, which shared with me the multitude of CITAC INPL November 9-13, 2009 (V METROCHEM), the problems during this term: Dr. Wynand Israel

MMessageessage ooff thethe CITACCITAC VVice-Chairmanice-Chairman aandnd AAwardward CCoordinatoroordinator

am sure it will continue to do so in the future. A Convenient and Economic Approach The CITAC process to find the most interesting to Achieve SI-traceable Reference or important papers in metrology in chemistry Values to be Used in Drinking-Water again yielded excellent and interesting papers Interlaboratory Comparisons being nominated. There was an increased Accred Qual Assur (2007) 12:615–622 participation in voting from members and I want to thank everyone for their time and Details are reported by the winning authors effort. The following three articles were in the present issue of the CITAC News. selected for special mention in 2009: Information about the winners will be distributed to the analytical and metrological Luca Callegaro, Francesca Pennecchi, Pier communities and our colleagues, who have not Giorgio Spazzini read these papers, will benefit from the CITAC Comparison of Calibration Curves Using Award procedure.

the Lp Norm Accred Qual Assur (2009) 14:587-592 On behalf of AFRIMETS, I would like to take this opportunity to wish readers of the CITAC Each year sees metrology in chemistry not only Samuel Wunderli, Hanspeter Andres News a successful and enjoyable 2010. If you advancing the level of traceability of all chemical Metrological Aspects of Glucose visit South Africa for the 2010 FIFA World Cup, analytical measurement, but expanding further Measurements by Biosensors remember that you are always welcome to visit into remote parts of the world. Since 1993 Electroanalysis (2009) 21:1984-1991 our National Metrology Institute (NMISA). CITAC played its role in spreading documents and traceability solutions to accredited (and Olaf Rienitz, Detlef Schiel, Bernd Guttler, Dr. Wynand Louw other) analytical and testing laboratories, and I Michael Koch, Ulrich Borchers NMISA, South Africa

2 / CITAC NEWS ● FEBRUARY 2010 TTableable ooff ContentsContents CCITACITAC NNewsews

Foreword by Chairman: CITAC's Accent on Cooperation / I. Kuselman ...... 1 CITAC News published by: Message of the Vice Chairman and Award Coordinator / W. Louw ...... 2 Laboratoire National de Métrologie et d'Essais (LNE) Editorial: The 24th CITAC Members' Meeting / P. Charlet ...... 4 29, avenue Roger Hennequin Reports of International Organizations 78197 TRAPPES Cedex ● An Update from the CCQM / R. Kaarls ...... 5 France ● ILAC Update / A. Squirrell ...... 7 Tel +33 1 30 69 21 95 ● Information from DAC of EuCheMS /H. Emons and J. Andersen ...... 10 Fax +33 1 30 69 12 34 ● AFRIMETS MiC Report 2009 / W. Louw and J. de Vos ...... 10 ● APMP Liaison Report 2009 / L. Samuel ...... 15 E-mail: [email protected] ● Activities of the COOMET TC 1.8 “Physical Chemistry” / L.A. Konopelko, Y.A. Kustikov and O.V. Efremova ...... 17 Internet: http://www.citac.cc ● Activities of the EURAMET Technical Committee for MiC in 2009 / B. Güttler...... 19 ● Recent Activities of the SIM Chemical Metrology Working Group / W. May ...... 21 ● Update on ISO/REMCO / H. Emons and J. Hammond ...... 22 Internet administrator: Prof. Wolfhard Wegscheider Most Interesting/Important Papers on MiC in 2009 University of Leoben, Austria ● Comparison of Calibration Curves Using the Lp Norm / L.Callegaro, F. Pennecchi and P.G. Spazzini ...... 23 ● Metrological Aspects of Glucose Measurements by Biosensors / Newsletter Editor: S. Wunderli and H. Andres ...... 26 Dr. Philippe Charlet, LNE, France ● A Convenient and Economic Approach to Achieve SI-traceable Reference Values to be Used in Interlaboratory Comparisons Concerned with Water Analysis / O. Rienitz, D. Schiel, B. Guttler, M. Koch and U. Borchers ...... 30 Newsletter designed and produced by: Mr. Aryeh Lewis Discussion Papers ISAS International Seminars ● Should We Look More Closely at the Measurement Results We Compare? / P. De Bièvre ...... 33 P.O. Box 34001, Jerusalem 91340 ● NMIs: Extended Outreach is Critical for Enhancing Confidence in Food Israel and Nutritional Measurements / V. Iyengar ...... 36 Tel: +972 2 6520574 ● Simple Basic Principles for Chemical Measurement: Identifying and Counting Fax: +972 2 6520558 / P. De Bièvre ...... 39 E-mail: [email protected] Meeting Reports ● V METROCHEM - Brazil / M.B V. Agostini, O. P. de Oliveira Jr. and V. Poncano ...... 40 No liability is accepted for the ● ISRANALYTICA 2010 and the CITAC Workshop in Israel / I.Kuselman ...... 41 ● 14th International Metrology Congress / S. Gazal ...... 43 accuracy of the information and the views expressed are not Announcements necessarily the official policy ● International Summer School Euromaster Measurement Science in Chemistry I. Leito ...... 44 of the CITAC Working Group ● Teaching Analytical Chemistry at the Beginning of the 21st Century / I. Leito ...... 44 members’ institutes or national ● International Symposium “The Future of Reference Materials - Science and Innovation” governments. / H. Emons ...... 45 ● 7th Workshop on Proficiency Testing in Analytical Chemistry, Microbiology and Laboratory Medicine / E. Okandan and B. Brookman ...... 46 For additional copies of the ● Visit CITAC Website / K. Schober ...... 46 CITAC News, please contact the newsletter editor. Updated CITAC Members' List ...... 47

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Message from the CITAC Secretary The 24th CITAC Members’ Meeting in Paris, April 19, 2009

meeting. Dr. Maire Walsh gave an update of the ● The IUPAC / CITAC Project is investigating recent ILAC activities. She mentioned that ILAC out-of-specification test results of chemical is currently working on the harmonization of composition based on metrological criteria between ISO Guide 34 and ISO 17025 concepts, by Dr. Ilya Kuselman; for the accreditation of RM producers, which ● IUPAC project on "Metrological Traceability is obviously a very important topic for CITAC. of Measurement Results in Chemistry" by A compromise resolution to take into account Prof. Paul De Bievre; the different approaches in Europe is being ● The "Measurement Science in Chemistry elaborated. Euromaster Consortium, by Dr. Anneli Kruvi; ● IUPAC / CITAC Project on PT for a limited Much of the meeting was dedicated to the number of participants, by Dr. Ilya Kuselman. reports of the CITAC activities including: The question of a better promotion of CITAC ● Examination of the draft procedure for participation in and the support of was also mentioned during the meeting. Dr. conferences and workshops by CITAC, Laly Samuel has proposed that the CITAC The 24th CITAC Members’ Meeting was held aiming to increase the visibility of CITAC. newsletter could be distributed electronically to a large number of potential interested people again in Paris at LNE. The members and/or ● Development of a procedure for planning their representatives, several invited speakers and performing CITAC projects sparked and therefore giving CITAC the opportunity to and observers, a total of seventeen participants debate among members of CITAC. set up networks at national levels. The idea from the entire world, including India, Brazil, was welcomed by the members, but it would Japan, Hong Kong and European countries, The Chair indicated that the basic idea of probably be necessary to ask people to register participated in the meeting (Fig. 1). the proposal is to increase CITAC activity, to on the CITAC web site to be on a mailing list for attract a CITAC member to lead a project or to receiving CITAC News. As usual, our treasurer presented the financial participate in such a project. The discussion report. The situation is healthy with a very focused on the nature of the projects for which This issue of CITAC News presents reports positive balance, allowing efforts to increase CITAC has an involvement. This important from international organizations, summaries the quality of the CITAC News and enlarge the discussion will continue next month. It shows and updates of publications awarded as the number of pages with important papers on the dynamism of the CITAC members to best contributions of 2009. Three important Metrology in Chemistry. The chairman raised develop activities. contributions are presented in the Discussion the possibility of obtaining funding through Papers section. They concentrate on the industry sponsorship and advertisements The meeting also provided an opportunity to development of concepts and principles in in CITAC News. We still need to define the discuss other important work for CITAC and metrology in chemistry and their applications priorities of CITAC’s budget. the scientific community: to end users, such as in food and nutrition with an original paper of Prof. Venkatesh A highlight of the meeting was the Iyengar. Reports and information on CITAC Awards for the best publications conferences related to metrology in in the field of metrology in chemistry. chemistry are presented, in particular The Award Certificates were delivered Metrochem V in Brazil this fall. The to Dr. Michael Ambrose, Prof. Paul 2010 events are also announced. De Bievre and Dr. Andrew Brown. The Chair congratulated the authors 2010 will see the change of the for their essential contribution to the Executive Committee of CITAC after development and dissemination of 3 years of duties. I was personally metrology concepts. A new round proud and happy to have served as of nominations will be conducted CITAC Secretary during this mandate in 2010. The recognition of the best and have welcomed the members of publications has become a milestone CITAC at LNE. I wish full success to in the activity of CITAC. the new CITAC Secretary.

Reports of CITAC liaison officers were Fig. 1. Participants of the CITAC meeting 2009 Dr. Philippe Charlet forwarded to participants before the after the CITAC dinner, Paris, France LNE, France

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An Update from the CCQM

Areas of Priority and Challenging “Frontiers of Traceability in Chem/Bio WG on Gas Analysis. Good progress is being Developments Measurements and Primary Methods”, made with the WMO GAW concerning the The interest of NMIs and other (potential) addressing Mass Spectrometry in realizing realization of SI traceable Volatile Organic designated institutes in metrology in chemistry biological relevant measurands, ID-SERS, Compounds (VOCs) at the parts-per-billion and subsequent participation in the CCQM Digital PCR for nucleic acid quantification, level. VOCs play a role in the generation of and its working groups is still rapidly growing. Count based Quantitation of trace level macro ozone in the troposphere. Driven by the needs of the economy, industry, DNA molecules using high sensitivity Flow traders and society in most of the countries Cytometry and Quantitative Cellular Analysis. Dr. A. Fajgelj (IAEA and IUPAC) reported on the following areas of high priority have been activities by IUPAC. He mentioned that the determined: During the meeting of the CCQM plenary, first draft IUPAC document “Metrological ● Food safety analysis, microbiology interesting reports and presentations were Traceability of Measurement Results in ● Analysis in healthcare given on progress in the Avogadro project, Chemistry”, composed by Prof. de Bièvre and (diagnostic, therapeutic, pharmaceuticals) discussing isotope ratio measurements on Dr. Dybkaer, has received many comments. ● Environmental measurements natural and enriched silicon for Si spheres and In the meantime an updated version is almost ● Purity analysis IDMS method for the Relative Molecular Mass ready. Dr. Fajgelj also noted that 2011 has ● Natural gas of Silicon. Concerns were expressed regarding been approved by the 63rd Assembly of the ● Forensic sciences the quality and credibility of measurements United Nations as the “International Year of of isotope amount ratios of silicon on Chemistry”, celebrating the achievements of Development in metrology in chemistry samples at both natural and enriched isotopic chemistry. lags behind the stage of development in composition. the physical measurement area. The field of Dr. I. Kuselman, chair of CITAC, presented chemical measurements is extremely wide CCQM Plenary a short overview of CITAC activities and compared to the physics area, and the demands The CCQM met on 22-24 April 2009 at the achievements, and a message from ILAC. from industry, trade and society are nowadays BIPM. As usual, the meeting was attended by very high, highlighting the enormous task still some 80 persons from about 45 organizations, ahead of us. Therefore, most of the CCQM not only representing NMIs and other Redefinition of the Mole Working Groups continue to have two working Designated Institutes, but also representing In 2007, the CCQM established a working group meetings per year. the intergovernmental organizations and group chaired by Dr. M. Milton to redefine international bodies IAEA, IUPAC, IFCC, ILAC, the mole. Other members are Drs. L. Besley, As usual, in April 2009, just before the meeting JCTLM, WHO/NIBSC, WMO, ISO REMCO and M. Salit, R. Wielgosz, R. Kaarls and Prof. de of the CCQM plenary, all CCQM Working CITAC. Bièvre. Dr. Milton presented a progress report Groups met at the BIPM. During the second and a clear presentation on the essence and half of 2009, all the CCQM Working Groups In addition to reports by the different CCQM consequences of the proposed changes. It met in Rio de Janeiro, hosted by INMETRO, WGs, several presentations were given by or on was made very clear that by redefining the Brazil. behalf of a number of stakeholders discussing mole based on fixing the value of the Avogadro and informing the CCQM about metrological constant we are deliberately breaking the link The meetings of the CCQM WGs on Bio issues of importance now being dealt with with mass, decoupling it from the kilogram. and Organic Analysis are also attended by these organizations and for which cooperation This is very helpful because there has always representatives of the Joint Committee on with the CCQM is considered desirable if not been confusion between amount of substance Traceability in Laboratory Medicine (JCTLM), essential. and mass when units were defined on the National Institute of Biological Standards basis of the fixed mass of carbon. Although and Control (NIBSC, a prime lab of the Dr. S. Westwood (BIPM) reported on the the redefinition of the mole will not have any WHO) and the US Pharmacopoeia (USP). activities of the World Anti Doping Agency consequences on the daily work of chemists, These organizations contribute actively to (WADA), noting that he was now serving on the concerns are expressed regarding the the activities of the Bio Analysis WG and the WADA Laboratory Committee as an external acceptance of the proposed new definitions by Organic Analysis WG. The meeting of the member with expertise in metrology, replacing the wider chemistry community. It is felt that CCQM WG on Gas Analysis is also attended by Prof. Siekmann. insufficient communication and education is representatives of the WMO. taking place informing the chemical community Dr. M. Milton (NPL) reported on the increased about the proposed changes, and this may During the April 2009 meetings, a very cooperation between the WMO Global endanger the understanding and acceptance interesting CCQM workshop was held on Atmospheric Watch committee and the CCQM of a new definition of the mole.

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A draft “mise-en-pratique” has been prepared, (RMOs) as an RMO Key Comparison. The In the Organic and Inorganic WGs, different presented to and discussed by the CCQM, and RMOs are now also organizing more RMO types of Key and Pilot Study Comparisons will presented to the CCU. supplementary comparisons. The results of all be developed: these comparisons are underpinning more than ● KCs testing specific core competencies The CCQM supports the proposal for a 4300 chemical Calibration and Measurement needed for carrying out chemical redefinition of the mole in terms of the Capabilities (CMCs) available at the participating measurements and value assignment in the Avogadro number. NMIs and DIs and which have been published in organic and/or inorganic area (including the KCDB at the BIPM web site. essential sample preparation procedures However, concerns about the quality and as well as measuring technique dependent credibility of the isotope amount ratios The CCQM WG on the quality of KCs and procedures); measurements, combined with concerns of published CMCs has decided to carry out, over ● KCs that assess the equivalence of acceptance by the wider chemical community a period of a few years, a careful screening Measurement Services actually provided, have been expressed in a Recommendation to of all published chemical CMCs in order to such as Certified Reference Materials and the CIPM and the CCU. check whether these are all still valid and Value Assignment of Proficiency Testing sufficiently underpinned by the results of KCs samples; Metrology for Bio-fuels and eventually other additional information ● Key Comparisons in emerging areas Dr. Ph. Charlet (LNE) summarized the and evidence. of global interest and importance with outcomes of the first European meeting on accompanying pilot study comparisons; metrology for bio-fuels. The CCQM Gas Analysis Working Group is ● Capability assessment studies to allow preparing a first comparison on air-borne assessment of measurement capabilities Drs. Kaarls and May, as well as colleagues nano-particles within ambient air, vehicle being established in new areas for an NMI/ from INMETRO, IRMM, LNE, VSL and others emissions and industrial workplaces; data DI. attended meetings on bio-fuels on 19-20 March which ultimately will be used to improve 2009 in Brussels, organized by the European human health and monitor climate change. BIPM Program of Work Commission, INMETRO and NIST. Reference Measurands are particle number concentration, Dr. Wielgosz presented the progress and was made to the tri-partite “White Paper on size distribution, surface area concentration, results of the work by the Chemistry Section Bio-Fuels”. morphological and chemical characterization. of the BIPM.

After discussion, it was decided that the EU- The CCQM Bio Analysis Working Group The work of the BIPM Chemistry Section INMETRO-NIST BIOREMA project will be reported good results of the KC on the was well commended. The work on ozone linked to comparisons on bio-ethanol and quantitation of a linearized plasmid DNA. measurement standards has been quite FAME (diesel) carried out by the CCQM WGs successful, leading to smaller uncertainties. on Organic and Inorganic Analysis and with The CCQM Surface Analysis Working Group The same good results have been obtained by respect to pH by the Electrochemical Analysis published good results of their first KC on the BIPM comparisons of some green house WG. silicon-oxide on silicon. gases.

The original proposal to create a separate In particular, CCQM Gas, Inorganic and In the area of organic purity analysis a study is CIPM/CCQM working group for bio-fuels has Organic Analysis Working Groups discussed being carried out investigating the optimum been withdrawn. the introduction of a more effective and number of purity analysis comparisons and efficient system of comparisons underpinning CRMs needed to judge the capabilities and CCQM Working Groups the claimed CMCs. competences of the NMIs (molecular weight All CCQM Working Groups reported about – polarity mapping). the work carried out. At present 121 different For binary gases and natural gas analysis, Pilot Study comparisons and 83 different Key the Gas Analysis WG will be able to make Further, the Chemistry Section acts as the Comparisons (KCs) have been carried out, are decisions on capability and competence of the secretariat of the JCTLM and liaises with several in progress or are planned for the near future. participating NMIs and DIs by making use of other international organizations and bodies, In addition, several Key Comparisons are statistics derived from a large number of KCs including the Codex Alimentarius Commission, followed up by a subsequent Key Comparison carried out over a period of many years. Inter Agency Meeting (IAM), International Dairy under the same code number, or are repeated Federation (IDF), USP, European Network of by the Regional Metrology Organizations Forensic Sciences Institutes (ENFSI), WMO,

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ISO REMCO and other ISO TCs, like clinical Physiological Quantities been re-established with an aim of expressing chemistry and nano-technology. On 16-17 November 2009 a workshop on how to make statements on traceability. physiological quantities and the SI was held at JCTLM the BIPM. Part of this workshop was dedicated IAEA Dr. Wielgosz presented a report on the current to the non-SI traceable bio-chemical quantities, The BIPM and the IAEA are strengthening their status of the JCTLM and its WG1 on “Higher expressing bio-chemical activity rather than cooperation, in particular with respect to: Order” Reference Materials and Measurement defining the exact chemical composition. In Methods. In October 2009 some 226 CRMs most of these cases reference is made to the ● ionizing radiation measurements, are currently listed along with 146 reference WHO International Standards and International dosimetry, radionuclide containing methods spanning 71 analytes. Units. However, when we better understand materials, nuclear data (CCRI), the relationship between the biological activity ● chemical measurements, CRMs (CCQM), Prof. L. Siekmann, chair of the JCTLM Working and the chemical composition it will be possible to make these quantities SI traceable, Group 2 on Reference Measurement Laboratory ● the “Vienna Standard Mean Ocean Water” Services and inter-laboratory comparisons providing medicines and healthcare at greatly standard (CCT) and reported on the progress in establishing reduced costs. and publishing a list of reliable reference ● the CIPM MRA measurement laboratory services and the Codex Alimentarius Commission results of PT schemes carried out among the Dr. R. Josephs (BIPM) presented a report on Conclusion participating laboratories. the Codex Alimentarius Commission, the Inter In 2009, good progress has been made Agency Meeting and the MoniQA, being the in broadening the scope of metrology in Currently 111 services from 19 laboratories are EU Network of Excellence funded project on chemistry. New challenging areas have been listed on the JCTLM database. the Monitoring and Quality Assurance in the entered, addressing needs in industry, trade Food supply Chain. The BIPM has contributed and society. The CCQM Working Groups The number of measurands in the IFCC to two workshops on “Method Performance are studying more efficient and effective Proficiency Testing scheme has risen to 195. and Analytical Uncertainty” and on “Method ways of assessing the claimed calibration and Some 38 (potential) reference laboratories Performance and the Criteria Approach: Truth measurement capabilities of the NMIs and are participating in this External Quality and Consequences”. DIs. Guidance is being developed for justified Assessment Scheme (EQAS). applications of statistical methods for the calculation of the Key Comparison Reference WMO Still there is a need for a wider CCQM Program Value and the degrees of equivalence of the The BIPM-WMO workshop on Metrology and of comparability studies of listed CRMs of NMIs and DIs participating in the CIPM MRA. Climate Change will be held at the premises of higher order, underpinning the results of the the WMO in Geneva on 30 March-1 April 2010. work carried out by the WG 1 and its sub- Also in 2010, workshops dedicated to specific groups and as published in the JCTLM data- sectors and lack of traceability in important base. Unfortunately, still not many NMIs are ISO REMCO areas will be organized, like a workshop able to participate in these comparisons. Prof. Emons (IRMM) reported on the activities on forensics and a workshop addressing in ISO REMCO. ISO Guide 33 is currently under traceability in micro-biology. A discussion with the EU is continuing with revision, getting a wider scope and addressing respect to the formal recognition of the JCTLM calibration. Other Guides under revision are Dr. Robert Kaarls database by the EU. Guide 31 (vocabulary) and Guide 32 (Labels and Certificates). An ad hoc ISO REMCO WG President CCQM on “CRMs and Metrology and Traceability” has The Netherlands

ILAC Update

CITAC is a stakeholder member of ILAC and representatives of each organization CITAC were represented at the CCQM Plenary and continues to contribute to ILAC’s work attend relevant meetings – for example, (April, Paris) by the CITAC Chair, Dr Ilya program, particularly in relation to issues in 2009, the ILAC Chair of the Laboratory Kuselman. In addition, ILAC contributes to the involving metrological traceability in chemistry. Committee, Maire Walsh, attended the CITAC work of CITAC/EURACHEM Working Group CITAC also has official liaison status with ILAC Members Meeting (March, Paris). ILAC and on Traceability and Measurement Uncertainty

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and documents emanating from this group are The ILAC Arrangement before consideration could be given to posted on the ILAC website. As of 9 November 2009, there were 65 following any particular direction. Signatories (Full Members) to the ILAC In maintaining this close cooperation with Arrangement, representing 51 economies. The Task Force is composed of the Chairs CITAC, ILAC has been able to continue its and Vice-Chairs of ILAC and IAF, the Chair or efforts to strengthen the links between Further progress was made during the recent nominated representative from each region, accreditation and metrology and this is much meetings in Vancouver towards establishing a representative of the unaffiliated bodies appreciated. the ILAC and IAF Arrangement for Inspection and stakeholder representatives from the and applications have been received from ILAC Laboratory Committee, the IAF industry A general update on ILAC activities for 2009 APLAC, EA and IAAC, the current Recognized representative and the IAF conformity follows: Regional Cooperation bodies, for evaluation to assessment bodies representative. The Task join the IAF/ILAC Inspection Arrangement. Force has had two meetings during 2009, ILAC Meetings one in January and one in May. The progress The mid year meetings of the ILAC Executive ILAC also continues to focus on enhancing made by the Task Force was reviewed during and the ILAC Arrangement Management a more widespread understanding of the the JCCC meeting in London and details of the Committee (AMC) were hosted by UKAS in socio-economic and trade benefits of the information package to be provided to ILAC London during the week of 22 June 2009. Arrangement amongst the international members, in preparation for the discussions The week also included meetings of the IAF, community, particularly governments and in Vancouver in October, were finalized. ILAC and ISO Joint Working Group, the Joint regulators. This information package was distributed to Committee for Closer Cooperation (JCCC) the members of ILAC (and IAF) prior to the and the various ILAC and IAF arrangement ILAC Membership meetings in Vancouver. management committees. ILAC membership as of 9 November 2009 was as follows: As agreed during the Vancouver Joint General The meeting of the IAF, ILAC and ISO Joint ● 65 Full Members (Signatories to the ILAC Assembly and confirmed during the ILAC Working Group included work on a Joint Arrangement) representing 51 economies; General Assembly, in October 2009, (JGA Communiqué on the Management system Vancouver Resolution 6 – Future Direction of requirements of ISO 15189:2007. This ● 23 Associates representing 23 economies; IAF and ILAC and ILAC Resolution GA 13.31 & Communiqué has now been finalized and Attachment) a 30 day ballot was undertaken, a copy of the Press Release and a link to the ● 20 Affiliates representing 18 economies; in mid November 2009, to determine which of Communiqué was provided to all members the proposed options for the future direction and ILAC liaison partners, on 4 November ● 4 Regional Cooperation Bodies of ILAC and IAF the memberships of both 2009. organizations would like to implement. ● 1 National Coordination Body The final ILAC meetings for the year were The adoption of JGA Vancouver Resolution held in Vancouver in October. The meetings ● 25 Stakeholders 5 – JCCC during the meetings in Vancouver, were very productive with many work items marked the end of the Joint Committee being finalized and a number of items seeing The ILAC membership (total 138 bodies) for Closer Cooperation, which held its final significant progress. now covers a total of 88 different economies meeting on 17 October 2009 in Vancouver. worldwide and approximately 33,000 This committee is being replaced with joint Special thanks go to our colleagues from CALA, laboratories and over 6,000 inspection bodies sessions of the ILAC and IAF Executive the hosts of the 2009 annual meetings, for the are accredited by the 65 ILAC Full Members. Committees. The first official joint session is excellent logistical arrangements and support scheduled for Monday 8 March 2010 in Paris. provided throughout the meetings. Joint ILAC/IAF Activities As many will be aware, discussions regarding ILAC Executive The Executive meetings for 2010 are scheduled the future development of ILAC and IAF were Two members of the ILAC Executive will be for 8-9 March in Paris, 23-26 June in Mexico City held during the first half day of the 2008 Joint stepping down from their respective roles on and during the annual meetings in October in General Assembly (JGA). It was agreed during 31 December 2009, namely Llew Richards, Shanghai. These meetings will be hosted by the JGA that a Task Force would be established ILAC Arrangement Management Committee our colleagues from COFRAC, EMA and CNAS to consider, in detail, the issues highlighted by (AMC) Chair, and Maribel Lopez, Joint respectively. the members as requiring further investigation Development Support Committee (JDSC) Co-

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Chair. The significant contributions made to to determine how we might best cooperate and Publication of ILAC Documents has been the work of ILAC, by both Dr Richards and Ms in areas of mutual interest and involvement. published. This document replaces ILAC Lopez, were acknowledged during the recent A meeting took place in July in Lyon, France S1:2003. The publication of this new document ILAC Arrangement Council and ILAC General between WHO representatives and the has resulted in the re-classification of the S- Assembly meetings in Vancouver. ILAC Chair, Daniel Pierre, to continue these series documents. These documents are now discussions. listed as Rules or R-series documents and the As of 1 January 2010, Andreas Steinhorst, ILAC website has also been updated to reflect from DGA, Germany and Dorsaf Zangar from The ILAC Chair, Daniel Pierre, was invited to this change. TUNAC, Tunisia will take on the roles of Acting speak on behalf of ILAC at a major symposium Chair of the ILAC AMC and Acting Co-Chair of held by BIPM, in October this year. The Please note that while the number and date the JDSC respectively. Elections for all (elected) Symposium was held to mark the 10th of the S-series documents have been updated positions on the ILAC Executive Committee Anniversary of the CIPM Mutual Recognitions to reflect the change in classification and, in will be held during the annual meetings in Arrangement. ILAC also gave a short a few cases, changes in cross-referencing to October 2010. presentation at the WADA Foundation Board other former S-series documents, there have Meeting, held in Stockholm in December 2009, been no changes to the actual content of these ILAC Liaisons to mark the 10th Anniversary of the World Anti- documents. The review of liaison activities continues to be a Doping Agency (WADA). major focus of the ILAC Executive Committee, A complete list of all documents, that have who seeks to ensure that ILAC interests are ILAC thanks all of the ILAC liaison officers, and been (or are being) circulated to members for represented in areas which have an impact on their organizations, who give up their time to either comments or voting, can be obtained the activities of ILAC and its members. Action assist ILAC in carrying out these activities for from the ILAC website in the Members Section items arising out of ILAC’s liaison activities are the benefit of the ILAC members. under Ballots. addressed during each Executive meeting, as well as on a continuous basis throughout the ILAC Secretariat The ILAC-MRA Mark registration process year. The ILAC Secretariat staff is as follows: continues and, as of 9 November 2009, 45 ILAC Annette Dever – ILAC Secretary; Alan Squirrell Full Members had signed Licensing Agreements The Liaison Database, located in the members – ILAC Executive Liaison Officer; Sharon with ILAC for the use of the Combined MRA area of the ILAC website, continues to serve Kelly – Senior ILAC Coordinator; Alison Hay Mark (the Combined MRA Mark is the ILAC- as the main repository for the ever increasing – ILAC Administrator and Rose Bevins – ILAC MRA Mark used in combination with the number of reports and documents that are Administrator. accreditation body’s own mark). produced as part of ILAC’s liaison activity. It can be accessed via the members area of the The Secretariat continues to develop the ILAC The April and October 2009 editions of ILAC ILAC website. website, with several improvements being News have been distributed in hard copy and carried out in conjunction with the ILAC electronic versions are available to download Since April 2009 ILAC has participated in a Marketing and Communications Committee from the ILAC website under the ‘News’ number of liaison activities including CASCO (MCC). Further ‘user-friendly’ improvements section. Past editions of ILAC News are also WG 29 (Revision of ISO Guide 65 – Product are planned for the first quarter of 2010. available to download from the website. The Certification), CASCO WG28 (Revision of ISO next edition of ILAC News will be published in Guide 43 – Proficiency Testing), ISO TC212 The Secretariat is now preparing a revision April 2010. (Technical Committee - Clinical laboratory of ILAC R5, which is the ILAC Complaints testing and in vitro diagnostic test systems), the Procedure. The revised document will be Further information on ILAC can be obtained BIPM Joint Committee for Guides in Metrology considered by the Executive during their from the ILAC website at www.ilac.org, or by (JCGM), the Joint Committee for Traceability in March 2010 meeting. Once the Executive have emailing the Secretariat on [email protected]. Laboratory Medicine (JCTLM), CITAC, CCQM, finalized their input, the draft document will EURACHEM, ISO REMCO, BERM 12 and be sent to members for a 60 day comment meetings of the WADA Laboratory Committee. period. Mr. Alan Squirrell ILAC has commenced general discussions As a result of the successful ballot held a few ILAC Executive Liaison with the World Health Organization (WHO) months ago, ILAC-R1:09/2009 Classification Australia

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This year’s main DAC event, the Euroanalysis XV congress2010.org). Information about the Bioanalytics - The aim of the Bioanalytics study conference was held in Innsbruck, Austria (see International Year of Chemistry 2011 (IYC11) group is to search for ways to bring the analytical www.EUROANALYSIS2009.at). EUROANALYSIS can be found on http://www.chemistry2011.org. and bioanalytical chemistry communities has become one of the most important broad- closer. George Horvai reported that several spectrum analytical conferences covering all analytical journals have strongly moved into aspects of analytical sciences. It is held every Some information from the various DAC the direction of bioanalytical chemistry, and two years in different European countries Study Groups: that a large fraction of the authors publishing and is organized under the umbrella of DAC- bioanalytical papers in analytical chemistry EuCheMS. In 2009, this conference was Education - The EChemTest (an evaluation journals are from outside the traditional organized by the Austrian Society of Analytical tool dedicated to student’s mobility and analytical workplaces. Moreover, important Chemistry (ASAC) represented by the chairmen chemistry knowledge assessment) of the journals which are dealing with areas other Wolfgang Buchberger and Wolfgang Lindner. European Chemistry Thematic Network than analytical chemistry have moved deeply The organizers welcomed approximately 700 (ECTN) is now fully operational, and university into the analytical field, for example "Nature participants from 53 countries. 130 lectures faculties are encouraged to apply the examples Methods". The conference Euroanalysis XV and 640 poster presentations under the motto to their teaching. had three sessions on bioanalysis, involving “The Impact of Analytical Chemistry on Quality some twenty lectures, and there were about of Life” formed a very attractive program which Quality - Hendrik Emons reported on new as many bioanalytical lectures in the other demonstrated the broad diversity of analytical initiatives on legislation. For instance, Germany sessions. sciences. introduced a new regulation on accreditation as a result of harmonizing with the new EU legislation. European Analytical Chemistry on the Web - Prof. Slavica Ražić is organizing Euroanalysis He also raised awareness about the ISO Guide 99 The website of EAConweb is maintained by XVI in Belgrade, Serbia, on 11-15 September on concepts and terminology of metrology which Bo Karlberg with the support of the Swedish 2011 (see http://www.euroanalysis2011.rs). At contains a lot of information relevant for analytical Chemical Society (http://www.anchem.su.se/ the DAC Annual Meeting in Innsbruck, it was chemistry. This guide, also known as VIM 3, is euchems/countries.asp). decided by the delegates that Euroanalysis XVII freely available at the BIPM webpage under www. will be organized in Warsaw, Poland, on 25-29 bipm.org. It is also important to enlighten students August 2013. Other conferences mentioned about the topic. Prof. Hendrik Emons are the 10th Meeting of Kinetics in Analytical EC-JRC-IRMM Chemistry (Pretoria, Republic of South History - The main activity of this study group Liaison Person DAC-CITAC Africa), the 13th ISRANALYTICA (Tel Aviv, is the production of a series of publications, Belgium Israel, 19-20 January 2010), ANALYSDAGARNA “People and Places Important in the History (Uppsala, Sweden, 14-16 June 2010), and of Specific Countries”, particularly the Hosts Dr. Jens E.T. Andersen the 3rd European Congress on Chemistry of Euroanalysis Conferences. The list of those DAC Secretary in Nuremberg, 2010 (http://www.euchems- completed is available on the DAC website. DTU, Denmark

AFRIMETS MiC Report 2009

Introduction (RMO) representing Africa. During 2009, Egypt All structures of AFRIMETS are now in During 2007, the Intra-Africa Metrology System was instrumental in establishing a SRMO in place and the first technical working group (AFRIMETS) was formed with, as principal Northeastern and Western (English speaking) meetings were held during the General members, the five sub-regional metrology Africa, incorporating the four ordinary Assembly meeting in July 2009. The first official organizations (SRMOs) in Africa. Four countries members. Libya and Sudan joined the new AFRIMENTS comparison was registered in the not part of a SRMO became ordinary members SRMO, called NEWMET. Mauritania also joined field of temperature. Protocol for comparisons (Nigeria, Egypt, Ethiopia and Ghana), extending AFRIMETS (through MAGMET), increasing in photometry and radiometry and dc voltage the countries represented in AFRIMETS to the total membership of AFRIMETS to 44 were considered. For metrology in chemistry, forty one. In October 2008, AFRIMETS officially countries. 15 countries attended the first MiC working became the regional metrology organization group meeting and the results of the first

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proficiency testing scheme were discussed. A across Africa; to provide a link to the activities work program for the next few years was drawn of the BIPM and OIML and to operate as a up and three comparisons will be conducted fully fledged RMO, fulfilling the obligations during 2009/10. as stipulated in the Mutual Recognition Arrangement of the International Committee The Structure and Members of for Weights and Measures, the CIPM MRA. AFRIMETS The six SRMOs are: AFRIMETS now spans the continent. The sub (1) Southern African Development Community regional map of AFRIMETS is shown in Fig. 1 Cooperation in Measurement Traceability and the country members of the SRMOs are (SADCMET); shown in Table 1. AFRIMETS thus covers the (2) East African Metrology Program (EAMET); continent with the exception of a few countries (3) Economic and Monetary Community of on the eastern and western side of Africa with Central Africa Metrology Cooperation very little or no metrological infrastructure. (CEMACMET); Fig. 1. Map of the sub-regional metrology (4) Secretariat for Metrology of the Economic A Work Program for 2009/2010 organizations of AFRIMETS Community of West African States One of the most frequent requests that (SOAMET); AFRIMETS receives is for traceability in MiC, melamine in milk, pesticides and mycotoxins) (5) Maghreb Metrology Cooperation and traceability in chemical and microbiological and training (wet chemistry, chromatography, (MAGMET) and measurement is therefore a high priority. Issues mass spectrometry, etc.). The requests are (6) Northeastern and Western Africa metrology under discussion include the manufacture diverse and differ from sub-region to sub- program (NEWMET). or provision of certified reference materials region, making it difficult to prioritize. (CRMs), value assignment of PT scheme The primary aim of AFRIMETS is to harmonize samples, the development of methods The Needs of the SRMOs scientific, industrial and legal metrology issues for current issues in food safety (such as EAMET Table 1. The individual SRMO members of AFRIMETS In East Africa, since 2004, Kenya’s tea production increased to the point where Kenya SADCMET/MEL SOAMET CEMACMET EAMET MAGMET NEWMET is currently the third largest producer and the single biggest exporter of tea in the world [1]. Angola Benin Cameroon Kenya Morocco Egypt A big advantage is that Kenyan tea stems from Botswana Burkina Faso Central African Rep Tanzania Algeria Nigeria a variety that is resistant to most pests and very DRC Guinea-Bissau Chad Uganda Tunisia Ethiopia little (or no) pesticides are used. One concern Lesotho Mali Congo Brazzaville Rwanda Mauritania Ghana is the quality of water used for both irrigation and processing, and accurate measurement Madagascar Niger Equatorial Guinea Burundi Libya is important for monitoring of water quality. Malawi Senegal Gabon Sudan Kenya participates in the SADCMET (now Mauritius Togo Sao Tome* expanded to AFRIMETS) water proficiency testing (PT) scheme [2]. Since its inception Mozambique Côte d’Ivoire in 2004, the PT scheme has focused on the Namibia chemical analysis of water covering all chemical Seychelles parameters including sulphate, chloride, South Africa manganese, lead, copper, nitrate etc. To date over 42 water testing laboratories participated Swaziland in the scheme which ultimately contributes to Tanzania ensuring that the water used in the region is Zambia within acceptable chemical limits, making it Zimbabwe safe for human consumption (and suitable for the production of agricultural products, etc). * Sao Tome is a member of CEMAC but membership of CEMACMET has not been confirmed.

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The PT scheme has been so successful, with a SADCMET is currently being established in Tunisia. Both vast number of laboratories participating, that The Southern African Development Tunisia and Morocco are in the process of the next PT round (started in July 2008) also Community (SADC) was formed in 1992 [4]. It establishing metrology in chemistry facilities. included the microbiology field. currently has fifteen member states (see table 1). The objectives of SADC include achieving SOAMET and CEMACMET The Kenya Bureau of Standards (KEBS) active development and economic growth; The West African Secretariat for Metrology established a Metrology in Chemistry section in alleviating poverty; enhancing the standard (SOAMET) is the sub-regional metrology 2007/2008. A regional metrology in chemistry and quality of life of the people of Southern grouping of the West African Economic and conference was held in Nairobi in August 2008, Africa, amongst others. As part of the quality Monetary Union (UEMOA) countries (see table with the focus on the provision of certified infrastructure, SADCMET was formed at the 1). UEMOA countries only account for 0.1% reference materials and the assignment of same time [5]. The MiC needs of SADCMET of global trade in manufactured goods, and reference values to proficiency testing samples. overlap with that of the other SRMOs especially intra-trade is only 6% of total trade. The main Close collaboration has been established with for primary and intermediate commodities exports of the UEMOA countries are agro-food the National Metrology Institute of South Africa (food, ores, etc.), but in addition, traceability products, fish products and cotton. The main (NMISA) and the first collaborative project on is needed for processes used in manufactured export market is the EU [7]. the value assignment of a wheat flour sample goods, for example chemicals and automotive. for an EAMET proficiency testing scheme was In September 2001, to enhance the completed. KEBS has observer status at the The NMISA is the only NMI in the region with participation of the UEMOA countries in CCQM and attended WG meetings and the official MiC facilities and that participates in regional and international trade, the EU, United plenary during 2009. the activities of the CCQM. It currently focuses Nations Industrial Development Organization its activities on the monitoring of toxic or (UNIDO) and UEMOA launched a Quality Tanzania has the largest agricultural carcinogenic substances in environmental Program as part of the UNIDO Trade Capacity contribution to the Gross Domestic Product samples and agricultural products (especially Building Initiative. The Program is assisting (GDP) of the EAC countries (41% of GDP). foodstuffs), towards improving the global with establishment and/or strengthening of Although a member of the EAC, Tanzania acceptance of manufactured goods. institutional and human capacities in laboratory participates in SADCMET and its measurement accreditation; the development of product traceability needs are mostly catered for MAGMET and material testing laboratories (chemical, through this well established SRMO. A program MAGMET is based on a cooperation of Arabic microbiology, etc.) according to international to accredit 14 food testing laboratories is well countries in North Africa, Maghreb, meaning standards; standards formulation, adoption underway and the first group of laboratories “place of sunset” or “western” in Arabic. It is and dissemination; the development and have already received third party accreditation generally applied to all of Morocco, Algeria and implementation of quality policies; instituting to ISO 17025. Tunisia but in older Arabic, usage pertained quality awards; and the development of only to the area of the three countries between consumer protection laws and associations. EAC trade liberalization has led to problems the high ranges of the Atlas Mountains and the for countries such as Rwanda, where the Mediterranean Sea. The Arab states of North Initially, the focus of the Program was on local market was flooded by sub-standard Africa established the Arab Maghreb Union in food processing. In early 2003 the focus was and counterfeit products [3]. The response 1989 to promote cooperation and economic extended to fish. In September 2003, the focus was that certain products were banned, for integration [6]. was further extended to cotton [8]. example plastic polyethylene bags, batteries, cosmetics containing hydroquinone, mercury The economy of Algeria is mostly reliant on CEMAC (from its name in French, and cortisones (except if being imported petroleum and natural gas, whilst Morocco and Communauté Économique et Monétaire de by a pharmacist) and all non-conforming Tunisia rely on Atlantic fisheries and fruit and l’Afrique Centrale) is an organization of States products and counterfeits. This has placed an vegetables. Due to a relatively large and well of Central Africa established to promote added responsibility on the Rwanda Bureau trained working force, nearly 50% of exports economic integration among countries that of Standards (RBS) [3] to provide metrology from these two countries are intermediate share a common currency, the CFA franc. The and testing for this purpose. The MiC activity and finished manufacture. The destination is region shares a high dependence on oil and is still largely confined to testing, but the sub- mostly the EU region, with the USA second. forestry and is subject to volatile economic regional interaction increased the awareness of Established metrology infrastructure, especially growth, weak intra-regional linkages and a lack traceability and the acceptance of test results. in Morocco, already supports international of transportation infrastructure. The zone is export, and a basic measurement infrastructure dominated by Cameroon and Gabon whose

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economies account for more than two-thirds of Laboratory (NRL) for the Department of Reference Material and Measurements (IRMM) the region’s GDP. Environmental Affairs and Tourism (DEAT) in in Belgium, and resulted in the NMISA further December 2008. investigating the following options: CEMACMET is the metrology program of CEMAC, but only exists in name, and there An advisory forum consisting of experts in ● A reference measurement for mycotoxins are no coordinated scientific and industrial air quality management will be required to in South African maize/animal feed/wheat/ metrology activities in the region. The PTB [9] develop and maintain the quality procedures wine and donor agencies such as UNIDO are active for the virtual NRL. The NMISA sees its ● A proficiency testing scheme for mycotoxins in programs to establish SQAM infrastructure in role as the provider of traceability for flow in South African maize/animal feed/wheat/ the region, but progress is slow. New activities and reference materials for the calibration wine are being planned for the near future. laboratories. Mobile monitoring stations are ● A reference material for mycotoxins in foreseen that can be used to audit monitoring South African maize/animal feed/wheat/ NEWMET stations as well as a training facility for which wine The metrology program in Northeast and NMISA would act as custodian. Auditing of the Western Africa stems from a memorandum monitoring networks will be accomplished The first outcome of the study was an agreed of understanding between the ordinary by encouraging ISO/IEC 17025 accreditation collaboration between the Southern African members (countries not part of a sub-region) so that this endeavor can be overseen by the Grain Laboratory (SAGL) and the NMISA of AFRIMETS. Libya and Sudan then joined. South African National Accreditation System that led to the signing of a memorandum Three countries (Egypt, Ghana and Ethiopia) (SANAS). of understanding (MoU) in support of have well established metrology infrastructure, technical cooperation for the analysis of including metrology in chemistry (Egypt and Automotive Sector: Proving organic contaminants in grains and related starting in Ghana), with the other countries International Competency products. The initial focus will be on reference all with some facilities and in the process of in Automotive Emission measurements for mycotoxins in maize. Further improving or expanding. work under the mycotoxins project, namely Measurements method validation for the determination of MiC activities include certified reference The gas metrology laboratory completed Ochratoxin-A in wine, continues as planned. material production (Egypt) and accredited participation in the international comparison testing facilities at most of the other institutes. for the preparation of gas mixtures intended With the analytical focus still strongly on for the testing of automotive emissions, pesticide residues in agricultural produce, The first GA will be held in Accra (Ghana) in Euramet 1113. The study, organized by the whether for export or local consumption, February 2010 and intra-regional comparisons European regional metrology body, Euramet, several African laboratories require are expected to commence soon. requires that participants accurately prepare measurement traceability to underpin their a prescribed mixture of propane, carbon measurements in this field. The NMISA is Participation in CCQM Activities monoxide and carbon dioxide in nitrogen currently developing a screening method The MiC laboratory at the NMISA is currently gas. The gas metrology laboratory has recently for various pesticides in agricultural crops, the only laboratory in Africa actively expanded its preparative capabilities to include including tea and wine, which can assist participating in CCQM comparisons and with multi-component mixtures and this study will these countries with more affordable CMCs in chemistry. The laboratory therefore serve to underpin this new capability. and robust analytical methods. With the plays a leading role in providing advice to collaborative efforts established through other countries in Africa that are establishing Metrology in Organic and AFRIMETS, measurement equivalence will MiC facilities, and as a pilot laboratory for Biochemistry also be coordinated through participation AFRIMETS comparisons. The organic metrology group at NMISA is in a proficiency testing scheme for selected currently investigating what role it can play in pesticides (e.g., p,p’-DDT). A few of the activities at the NMISA during the assisting South African analytical laboratories in past year included: analyzing mycotoxins in foodstuffs and feeds. The IUFoST World Congress is being hosted in This work is critical because it affects several Cape Town, SA, in August 2010. The theme for Developments on Establishing large South African industries trading in food this congress is “Food Science Solutions in our a NRL for SA Air Quality and wine, involving thousands of jobs. The initial Evolving World” and the focus is to encourage Measurements 2008 investigation on mycotoxins included a young scientists from Africa to participate. The NMISA prepared a proposal for the survey of SA analytical laboratories involved in The NMISA will be participating in the establishment of a National Reference mycotoxin analyses and a visit to the Institute of scientific program. This can serve as a forum

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for disseminating measurement competence comparison (CCQM-K79): Comparison of [3] T. Kimbunga, Applying Quality Standards for selected parameters like pesticides and Value-Assigned CRMs and Proficiency Testing to Products, www.eac-quality.net/better- mycotoxins in agricultural produce. Materials for Ethanol in Aqueous Matrix (0.1 business-with-quality/benefits/imports. mg/g to 500 mg/g). html The CCQM organic analysis and bioanalysis [4] The Southern African Development working groups have expanded the Participation in International website, see: www.sadc.int measurement focus to include large molecules Comparisons [5] The SADC Cooperation in Measurement of interest to both groups and this has afforded NMISA participated in 14 comparisons in Traceability website, see: www.sadcmet.org the NMISA bioanalysis laboratory the potential metrology in chemistry during 2009. A list of [6] Maghreb, from Wikipedia, the free to establish measurement capability for amino the comparisons is provided below in Table encyclopedia, http://en.wikipedia.org/ acid quantification (hydrolysis of peptides and 2. In addition, three AFRIMETS comparisons wiki/Maghreb proteins) using both fluorescence detection are being planned in the fields of organic and [7] Economic Community of West African and tandem mass spectrometry. Participation is inorganic chemistry. States,http://en.wikipedia.org/wiki/ planned in the upcoming CCQM-P58.x protein Economic_Community_of_West_ analysis study next year. At the end of 2010, the AFRIMETS MiC will be African_States able to report on the first pilot studies and [8] UNIDOScope 2004, http://www.unido.org/ The newly developed certified reference comparisons conducted in the region. index.php?id=o27363 material (CRM) for ethanol in 20% glucose has [9] PTB, www.ptb.de received a favorable reception from the wine References industry. Wine testing laboratories use the new [1] M. Heiss and R. Heiss, The Story of Tea, CRM to calibrate equipment that measures the A Cultural History and Drinking Guide, p quantity of ethanol in wine. In order to uphold 241, http://books.google.co.za Dr. Wynand Louw the laboratory’s calibration and measurement [2] D. Masuku and S. Prins, “SADC Water Ms. Jayne de Vos claims for these reference materials, the Proficiency Testing Scheme,” www.nmisa. NMISA laboratory is participating in an international org/news/200804.html South Africa

Table 2. List of international comparisons that NMISA participated in or started during 2009

No International Number Laboratory Description 1 CCQM-P122 Organic & Bio Chloramphenicol in pig muscle 2 CCQM-K79 Organic & Bio Comparison of value-assigned CRMs and PT materials for ethanol in aqueous matrix, 0.1 mg/g to 500 mg/g 3 CCQM-P90 Organic & Bio CAP in milk 4 CCQM K-67 SA The quantification of Fe-Ni binary alloy thin films 5 VAMAS TWA2-A3(d) SA Static SIMS interlaboratory study: part 1, linearity of the intensity scale 6 CCQM-K75 & P118 Inorganic Toxic metals in algae (Pt, Ni) Toxic metals in algae (Cd, Cr, Hg, Pb) 7 CCQM-P119 Inorganic Analysis of Pb in a lead-free solder 8 CCQM-K71 Gas Multi-component stack gas mixture

9 CCQM-K74 Gas 10 ppm NO2 in nitrogen by FTIR

10 CCQM-P110 Gas 10 ppm NO2 in nitrogen by FTIR 11 BIPM.QM-K1 Gas Ambient level ozone 12 EURAMET 1092 Gas 120 ppm ethanol in nitrogen 13 EURAMET 1113 Gas Preparative comparison for automotive emission gases

14 APMP.QM-K41 Gas 10 ppm H2S in nitrogen

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APMP Liaison Report 2009

Fig. 1. Participants of the APMP TCQM meeting 2008, Jakarta, Indonesia

The 24th APMP (Asia Pacific Metrology Program) the status of the APMP CMC intra-review will be 2009 and the second working group meetings General Assembly and the 8th meeting of APMP- monitored on the APMP website. of the year Would be in INMETRO, Rio de TCQM (Technical Committee on Amount of The status of CMCs submitted by APMP were Janeiro, Brazil from 4-6 November 2009. Substance) were held in Jakarta, Indonesia monitored to find out whether there were Progress reports on the latest activities carried from 3-7 November 2008. Metrologists from any CMCs delayed for a long time without out by the TCQM Working Groups were member NMIs and guests from CIPM, BIPM, recognition. The status of CMCs monitored presented by each representative. RMO’s, NCSLI and specialist regional bodies from the BIPM KCDB was found to differ from attended the meeting. Two new members the reports by TC chairs. Therefore the status Highlights of APMP Activities – HSA (Health Science Authority) Singapore, of CMCs will be confirmed. The meeting discussed 2007-2008 APMP- in the field of chemistry, designated by ASTAR TCQM activities, including the on-going and and OAP (Office of Atoms for Peace) Thailand, APMP EC and its associated subcommittees newly proposed comparison programs and in the field of ionizing radiation, designated engaging with APLAC’s PT programs will CMC claims and workshops and symposia by NIMT Thailand – joined the APMP. The provide traceable reference values to those held during this period. Five economies from application from VNIIM Russia to become a programs and also consider the linking of the APMP region, Australia, China, Chinese new full member of APMP was approved by their formal comparison processes to relevant Taipei, Japan, and Korea, have CMC claims in APMP-GA. The 24th GA elected Dr. Kwang APLAC PT programs. the Appendix C and for the first time Hong Hwa Chung from KRISS as Chairperson for a Kong filed for CMC claims. TCQM encouraged second term of two years from the 25th GA to Recognizing the importance of global submissions from other economies using the the 27th GA, and Dr. Jia-Ruey Duann, Director consistency of Materials Metrology activities new template which can be obtained from the General of CMS/ITRI from Chinese Taipei and and noting the MoU between BIPM and VAMAS, JCRB document website (www.bipm.org/en/ Dr. Angela Samuel, Director of International APMP ad-hoc WGMM decided to contact BIPM committees/jc/jcrb/) and emphasized that all Cooperation Office of NMIA Australia as new whenever necessary. Participation of the claims should be made for services offered on EC members. The 25th APMP GA and related Institute of Materials Research & Energy in a reasonably regular basis and not just because meetings will be held in Kuala Lumpur, Malaysia APMP ad-hoc WGMM will be discussed in the EC. of participation in key comparisons. and hosted by SIRIM. Technical Committee on Amount of Reports on the APMP Workshop on Many recommendations and actions were taken Substance Meeting (TCQM) Metrology in Chemistry by the APMP GA, the main ones being: APMP The APMP TCQM held its 8th annual meeting will cooperate with the BIPM in the field of Dr. Laurie Besley presented the objective, on 3-4 November 2008 at the Mercure strategy and outcome of the APMP workshop nanometrology and provide BIPM with APMP’s Convention Centre, Jakarta, Indonesia. A total opinions and information on the priorities for on metrology in chemistry. The APMP guide, of 31 delegates from 17 member economies downloadable from the APMP website, was national and international activities when so attended the meeting (Fig. 1). The President requested. one of the outcomes of this workshop. Two of CCQM, Dr. Robert Kaarls, gave an update on workshops were conducted in 2008. The first CCQM working group activities during 2008. QMS review status could be improved through was held in May 2008 in Dhaka, Bangladesh He also announced that the coming CCQM while the second took place in Jakarta, enhanced communication between the TCQS working group meetings and workshops chair and the other TC chairs. For this purpose, Indonesia from 31 October – 1 November at BIPM Would take place from 17-24 April 2008. A number of economies participated and

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made presentations. There were suggestions run in parallel with CCQM-96 “Total arsenic Progress Reports on TCQM Key and to improve the APMP guide as well as and arsenobetaine in swordfish”, has been Supplementary Comparisons recommendations for APMP – TCQM, DEC, completed. 5 laboratories including 3 NMIs Dr. Jin Seog Kim reported about APMP. EC, mainly in 5 areas: training, RMs/CRMs, (NAM, NIST and UME), examining total arsenic QM-S1: Gravimetry, a supplementary study government support/awareness raising, new and 3 laboratories – all NMIs – examining designed for gravimetric comparison of gas APMP programs and national dissemination of arsenobetaine, participated. The results mixtures involving Helium in Nitrogen. Four capacity building. The discussion was intensive reported on total As measurement by the three organizations participated in the study. Dr. and showed a great depth of understanding. NMIs were in good agreement to the KCRV for Kenji Kato reported on APMP.QM-S2, a bilateral Organizers acknowledged the continuous total As in CCQM-K43.1. For arsenobetaine, the study between NMIJ and NMIT coordinated by financial support and technical input provided analytical results were in good agreement using NMIJ on O2 in N2 and Dr. Jin Seog Kim reported by PTB Germany in the region. NMIJ-AB as the calibration standard. Both NIM on APMP.QM-K1c, a bilateral comparison and NMIJ have observed a difference of 10% between NIM & KRISS. Dr. Kim announced 6th Workshop of APMP/TCQM Gas in analytical sensitivity between the BCR CRM that the report would include the degree of Analysis Working Group 626 arsenobetaine solution and the NMIJ CRM equivalence to show linkage to CCQM-K1c. The workshop on “Present Progress in Gas 7901-a one. An Investigation was conducted Metrology” was held in KRISS, Korea from 19- to determine the cause. The outcome of Reports from Member Economies 23 May 2008. It included a 2-day workshop, a the investigation was presented at the next Dr. Prabhat K. Gupta, NPLI, India, Dr. Laly tour to LCD company and a training session. workshop in April 2009. Samuel, MSL, New Zealand and Dr. Sumardi, There were 44 participants from 7 countries LIPI, Indonesia briefly shared their ideas on including participants from various NMIs, APMP.QM-P13: Metals in Polypropylene the development of metrology in chemistry government institutes and companies. The Dr. Feng Liuxing of NIM China presented as well as reporting on the activities relating 7th workshop was held in SIRIM, Malaysia in the results of the study on the determination to chemical metrology in their respective May 2009 and the 8th workshop will be held at of cadmium, mercury, chromium and lead economies. NMIJ, Japan in 2010. in polypropylene, which ran in parallel with a CCQM P-106 pilot study. This was the Forthcoming TCQM Key/ 8th ACRM Meeting in Lijiang China first comparison of polymers and plastics Supplementary/Bilateral and Tri-lateral The 8th ACRM meeting took place in Lijiang in response to the implementation of the Comparisons and Pilot Studies from 23-24 September 2008 and was attended RoHS’s directive. Cadmium and chromium Dr. Charun Yafa from NIMT, Thailand proposed by 26 participants from NIM, NMIJ and KRISS. represented the class of elements of minimum an inter-comparison study on preservatives in NIM reported the progress of the work of four challenge, lead of medium challenge and curry paste as there is a current lack of CRM working groups covering food, gas, RoHS and mercury of greatest challenge. There were in this matrix to support the testing need of biological analysis. a total of 22 participants; however only one the industry. In this pilot study, curry paste laboratory, DSS from Thailand participated in will be fortified with sorbic acid and sodium Progress Reports on TCQM Key APMP.QM-P13. benzoate. He gave an overview of the process Comparisons and Pilot Studies of production of this material as well as the APMP.QM-P10: “Cadmium and Lead in Herb” Overall it was a successful study with good stability and homogeneity data. He added that Dr. Cheung Tsz-chun of GLHK presented the agreement of results from most experienced further stability studies at -80˚C, -20˚C and technical data on the Herb (Herba Desmodii laboratories. The study showed that the +4˚C will be conducted and the samples would Styracifolii) as well as the performance of technique – INAA – is a potential primary be irradiated with gamma ray before they are participants. This study was conducted in method for the determination of mercury ice-packed and delivered to participants. A parallel with CCQM-97, and 12 laboratories and cadmium in this matrix. The study also number of economies have indicated interest from 8 economies participated in the pilot uncovered the potential use of XRF for the in participating in this study. study. The performance of APMP.QM-P10 determination of chromium, mercury and lead. was not as satisfactory as CCQM P-97. Better Future Meeting agreement between APMP.QM-P10 and CCQM APMP.QM-K24 (APMP.QM-P12): Cd in The General Assembly selected Thailand as the P-97 was achieved in the identification of Rice venue for the 26th GA and related meetings in outliers. Dr. Jin Seog Kim informed the meeting that 2010. the rice samples for the key comparison study APMP.QM-P11: Organo-arsenic in and pilot study were dispatched in July 2008 Swordfish and August 2008 respectively and reminded Dr. Laly Samuel Dr. Akiharu Hioki of NMIJ reported that this participants of the deadline for the submission MSL study, co-ordinated by NIM and NMIJ and of results. New Zealand

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Activities of the COOMET TC 1.8 “Physical Chemistry”

The Technical Committee 1.8 “Physical ● Rendering of metrological services in the A number of other studies, as well as PT schemes Chemistry” was established in the framework field of physico-chemical measurements. and industrial comparisons were run as well. of COOMET in 2002. Since this time, there have These projects’ objectives were of regional and been major efforts made actually on the choice TC 1.8 Projects international interest: aerosol particles, gene- of activity directions, involvement of National Only the NMIs of COOMET Member States as modified objects in food, standard gas mixtures Metrological Institutes (NMIs) of COOMET well as interested metrological centres and of ecological and technological purpose. Member States in the field of its activity, forging designated laboratories of other countries of relationships and participation in activities that have an appropriate basis of standard The Following New Key Comparisons of related committees and working groups of equipment can take part in the TC projects and Pilot Researches are Planned for other international organizations. on international comparisons and pilot 2010-2011: researches. ● COOMET No 483/RU/09 “Key comparison Whereas the information about activities of the of primary standards of components TC 1.8 is being published in CITAC News for The most significant projects of the TC during concentration in gas media - NO in Nitrogen the first time, this report is an attempt to show the last years were: (100 and 1000 μmol/mol)”; the main results as well as current activity of ● COOMET.QM-K3 “Automobile gases (CO, ● COOMET No 484/RU/09 “Key comparison TC 1.8. CO2, C3H8) in Nitrogen” of primary standards of components VNIIM (Russia), BelGIM (Belarus), BAM concentration in gas media - SO in Nitrogen General Information 2 (Germany), Ukrmetrteststandart (Ukraine) (100 and 1000 μmol/mol)”; Activities of the COOMET Technical Coordination: VNIIM (Russia); ● “Key/Pilot comparison of solutions with low Committee 1.8 “Physical Chemistry” covers ● COOMET.QM-K23.b “Certified reference nominal values of electric conductivity” (on those measurement services, which are materials - synthetic natural gas” a stage of registration); referred to “Metrology in chemistry” category. VNIIM (Russia), BelGIM (Belarus), BAM ● COOMET No 375/RU/06 Pilot comparison Twenty-two NMIs from 17 COOMET Member (Germany), SMI (Czech. Rep.), SMU “Determination of gene-modified objects in States are represented in TC 1.8 now. They are: (Slovakia), Ukrmetrteststandart (Ukraine) food”; AZSTANDART (Azerbaijan), NIM (Armenia), Coordination: VNIIM (Russia); ● COOMET No 435/RU/08 “Pilot comparison BelGIM (Belarus), BIM (Bulgaria), PTB and ● COOMET.QM-K1.a “Certified reference in the field of aerosol particles mass BAM (Germany), KazInMetr (Kazakhstan), materials - gas mixtures CO in nitrogen” concentration measurements”; NISM (Kyrgyzstan), CIM (KNDR), INIMET VNIIM (Russia), BelGIM (Belarus), BAM ● COOMET No 479/RU/09 “Supplementary (Cuba), VMT (Lithuania), INSM (Moldova), (Germany), Ukrmetrteststandart (Ukraine) comparison in the field of moisture INM (Romania), VNIIM, VNIIFTRI, UNIIM, Coordination: VNIIM (Russia); measurements in cereal grain and cereal VNIIOFI VNIIMS (Russia), SMU (Slovakia), o ● COOMET N 421/RU/08 “The products”; Ukrmetrteststandart (Ukraine) as well as CNS supplementary comparison of pH working ● COOMET No 362/RU/06 “Pilot comparison Uz (Uzbekistan) and GEOSTM (Georgia), who standards” in the field of measuring the aqueous joined the TC 1.8 in the last 2-3 years. VNIIFTRI, VNIIM, UNIIM, VNIIMS (Russia), glucose solutions”; NISM (Kyrgyzstan), BelGIM (Belarus), ● COOMET No 367/RU/06 “Pilot comparison The main directions of COOMET TC 1.8 Ukrmetrteststandart (Ukraine), KazInMetr in the field of blood elements”. activities are: (Kazakhstan) and Regional centers of ● Preparation of the NMI CMCs of the standardization and metrology (CSM) of Cooperation with CCQM COOMET Member States, to be placed in Russian Federation: CSM of Novosibirsk, Representatives of TC 1.8 have participated in the BIPM KCDB; CSM of Nizhniy Novgorod, CSM of Rostov, CCQM activity practically since its establishment ● Organization of an internal review of CMCs CSM of Ekaterinburg, CSM of Khabarovsk, and became members of the working groups of COOMET NMIs and carrying out of an Rostest-Moscow, Test-S.Petersburg, Ural- KCWG (Key Comparison working group), interregional review of CMCs of other Test OAWG (Organic Analysis working group), regional metrological organizations; Coordination: VNIIFTRI (Russia); GAWG (Gas Analysis working group), ● Planning and organizing international ● COOMET No 379/RU/06 “Pilot comparison IAWG (Inorganic Analysis working group), comparisons and interlaboratory in the field of moisture measurements in BAWG (Bio Analysis working group), EAWG researches; cereal grains and cereal products” (Electrochemical Analysis working group). ● Getting the TC 1.8 Members acquainted BelGIM (Belarus), Ukrmetrteststandart with the CCQM and COOMET documents (Ukraine), UNIIM (Russia), SP TRIS During 2008-2009, NMIs COOMET (VNIIM, concerning realization of the MRA and (Sweden), PTB (Germany) VNIIFTRI, UNIIM) participated in the following assurance of metrological traceability; Coordination: UNIIM (Russia). CCQM comparisons: ● Improvement of the TC 1.8 structure;

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Gas Analysis consists mainly of participation in projects Table 1. Distribution of CMCs by NMIs CCQM-K79/P110 “Nitrogen dioxide 10 μmol/ of international comparisons. Particularly, and measurement fields mol”, VNIIM and Ukrmetrteststandart participated in CCQM-K51 “ CO in nitrogen (5 μmol/mol)”, EURAMET comparisons: NMI N CCQM-K65 “Mercaptans in methane” EUROMET. QM-K4 “Ethanol in air”, VNIIM 236 (coordination of VNIIM), EUROMET.QM-K1.c “NO in nitrogen”, VNIIFTRI 7 CCQM-K71 “Multi-component gas stack EUROMET 764 “NH3 in nitrogen”, emissions”, EUROMET 833 “PCB congeners in organic BelGIM 2 CCQM-K66 “ Purity analysis of methane”, solution”, Ukrmetrteststandart 7 CCQM-K68 “N2O at ambient levels”; EUROMET 621 “Key comparison(s) in humidity UNIIM 4 (dew-point temperature)”. Inorganic Analysis and Electrochemistry Measurement field N CCQM-K34.2 “Assay of Potassium hydrogen APEC, ANMET Gases 185 phthalate”, Cooperation of TC 1.8 with these organizations Organic solutions 21 CCQM-P111 “Seawater salinity”, in 2009 was realized through active Inorganic solutions 13 CCQM-P119 “Lead in solder”, workshops: CCQM-P100.3 “Determination of low levels of “Strengthening Chemical Metrology Metals and alloys 9 Hg in natural water”, Infrastracture”; Sediments, soils, ores and particulates 4 CCQM-P118 “Toxic metals in algae”; “Traceability in Material Testing to Reduce High purity chemicals 3 Technical Barriers to trade”. Food 5 Organic Analysis CCQM-K79 “Comparison of value assigned ISO TC Water 1 CRMs and PT materials for ethanol in aqueous Representatives of TC 1.8 participate in the Electrochemical analysis 15 matrix”, development of standards and carry out an CCQM-P109 “Determination of acrylamide expertise in the ISO TC 146 (Air Quality), TC Meetings and Events in cooked high-carbohydrate food (potato 158 (Gas Analysis), TC 190 (Soil Quality), TC ● 2nd All-Russian Conference “Certified chips)”, 193 (Natural Gas). Reference Materials in Measurements and CCQM-P91 “Pesticides in foods: pyrethroids in Technologies”, May 2008, St. Petersburg, apple juice”; OIML Russia; Representatives of VNIIM and VNIIFTRI are ● 3rd International Conference “Metrological Bio Analysis the Chairs of OIML TC 17 “Physico-chemical assurance of physico-chemical and optico- CCQM-P113 “Relative quantification of genomic measurements” and its sub-committees (SC) physical measurements”, November 2008, DNA fragments extracted from a biological SC2 “Saccharimetry”, SC3 “pH-metering”, Kiev, Ukraine; tissue”, SC4 “Conductometry”, SC5 “Viscosimetry”, ● International Scientific and Practical CCQM-P103 “Measurement of multiplexed SC6 “Gas Analysis”, and participate in the conference “Metrology – 2009”, April 14-15, biomarker panel of RNA transcripts”, development and expertise of standards. 2009, Minsk, Belarus; CCQM P94.1 “Quantification of DNA ● 3rd International Competition “The Best methylation”. Young Metrologist of COOMET 2009”, April Implementation of MRA 14-15, 2009, Minsk, Belarus; APMP In order to achieve comparability of ● International Seminar “Mathematics, Since 2008 VNIIM (Russia) has become a full measurements of national standards, COOMET statistics and computation to support member of APMP. KazInMetr (Kazakhstan) is an NMIs participated in more than 100 CCQM, measurement quality”, June 30, 2009 - July associated member of this Regional Metrology COOMET and EURAMET key and pilot 2, 2009, COOMET, St. Petersburg, Russia. Organization. comparisons. Numerous events devoted to celebration At present VNIIM participates in two projects of As a result of these activities, COOMET NMI of D.I. Mendeleyev’s 175th anniversary APMP in the field of Metrology in Chemistry: has included 256 CMCs into the international (08.02.2009) were organized in 2009. Many APMP.QM-P14 “Preservatives in a curry paste”, database (BIPM KCDB) in the field of Metrology Russian and foreign scientists, including in Chemistry. APMP.QM-K41 “H2S in nitrogen”. metrologists, took part in them. D.I. Mendeleyev is appreciated in Russia not only EURAMET Distribution of CMCs by NMIs and as the author of the Periodic Table of Elements VNIIM is an associated member of EURAMET. measurement fields is shown in Table 1, where but also as a founder of metrology as a science Cooperation with TC METCHEM EURAMET N is the number of CMCs. and of the first National Metrology Institute in

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Russia, which is named after him at present ● May 20, 2009 – International readings 1.8 representatives translated such important as D.I. Mendeleyev Institute for Metrology named after D. I. Mendeleyev, Saint- documents as: (VNIIM). Petersburg, VNIIM ● VIM3 “International Vocabulary of ● Jubilee exhibition in Polytechnical Museum Metrology - Basic and General Concepts Main Events in Celebration of (Moscow) devoted to D. I. Mendeleyev. and Associated Terms” (translation of Mendeleyev’s 175th Anniversary BelGIM and VNIIM, 2009) ● EURACHEM/CITAC Guide “Quantifying ● February 9, 2009 – Meeting of the Presidium Translation of International Documents of Saint-Petersburg Department of Russian Russian, as well as English, are the official Uncertainty in Analytical Measurement” Academy of Science languages of the COOMET Member States. For (translation of VNIIM, 2002); ● EURACHEM/CITAC Guide “Traceability in ● February 11, 2009 – Joint session of the the majority of specialists from countries of Presidium of Metrological Academy and CIS (Commonwealth of Independent States) Chemical Measurement” (translation of VNIIM Scientific Council Russian is the main language of international VNIIM, 2005). ● February 25, 2009 – Scientific conference communication and the scientific literature in “D. I. Mendeleyev heritage: historical Russian is in demand as before. Besides CIPM Dr. L.A. Konopelko aspects and modern view”, Moscow, and CCQM documents, at the initiative and Dr. Y.A. Kustikov Polytechnical Museum with the active participation of COOMET TC Dr. O.V. Efremova, VNIIM, Russia

Activities of the EURAMET Technical Committee for MiC in 2009

Second Phase of the European researcher grant schemes will be available results of the Conference were still pending Metrology Research Program to bring external expertise into the research at the time of writing. The start of successful The European Metrology Research Program projects and there will be opportunities for project proposals is anticipated in the course (EMRP) has been a crucial factor in the organizations to participate in the research of 2010. evolution of the European Association of projects with their own resources where it is National Metrology Institutes EURAMET e.V. mutually beneficial to do so. Good progress was also made in the running in recent years. EURAMET’s reorganization JRPs under the iMERA-plus initiative. The as a legal entity was required in order to The first call for potential metrology research current status of several projects was presented prepare for a research programe co-funded topics (PRTs, so called stage 1) was successfully at several occasions such as the International by the European Commission under article launched in May this year for a Targeted Metrology Congress in Paris in June 2009. 169 of the EC treaty. The first phase of EMRP Program in the energy sector with a budget of € is the currently running iMERA-Plus initiative approximately 34 M . The EMRP Committee has Further Activities in TC-MC launched in 2007 with a total value of 64.6 M€ subsequently selected sixteen research topics All EUROMET-bodies continue to work under under FP7 (ERA-NET Plus). iMERA-Plus projects (SRTs) from these PRTs submitted in stage 1. EURAMET including the chemistry sector, now started in May 2008. Many SRTs contain inputs from more than one called Technical Committee for Metrology PRT as similar ideas have been combined where in Chemistry (TC-MC) in line with the The second phase is the full European appropriate. Energy is considered to be one of nomenclature of the other TCs. The internal Metrology Research Program (EMRP) owned the “Grand challenges” of European Research structure of TC-MC remained unchanged and executed by EURAMET. Following and has a multidisciplinary character. This also with four Sub-Committees, Inorganic Analysis signature by the European Parliament and the applies to the SRTs – none of them is devoted (convenor: Christophe Quetel, IRMM), Council, the Co-decision process was finalized exclusively to chemistry for this reason but Organic Analysis (Gavin O’Connor, LGC), for the EMRP. The Decision (No 912/2009/EC) chemical topics are an integral part of several Electrochemical Analysis (Petra Spitzer, PTB) was published in the Official Journal of the SRTs. Those SRTs are the basis of the Joint and Gas Analysis (Rob Wessel, NMi). Gavin European Union on 30 September 2009. This Research Project Proposals which consortia are O’Connor (LGC) was introduced as the new second phase of the EMRP has a total value invited to submit. The second stage, the call for convenor of the Sub-Committee on Organic of 400 M€ over an approximately seven year Joint Research Projects (JRPs) was started in Analysis as the successor to Franz Ulberth period and is jointly funded by the European early September and ended 2 November 2009. (IRMM). Commission and 22 participating countries. The Consortia were formed and submitted project EMRP will provide the opportunity for the user proposals which were presented in a Review The second meeting of EURAMET TC-MC community and other stakeholders to directly Conference in Berlin on 25 & 26 November 2009 was conducted in Bucharest, Romania from suggest topics that the metrology community to a board of external referees from outside 3-6 February 2009. All Sub-Committees had should address with its resources. Additionally, the EURAMET metrological community. The separate meetings on the first two days of the

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conference and a TC- based spectroscopy MC plenary meeting (EUROMET 934), trace was held on 5-6 purity measurements February. There were (EUROMET 937), ultra 60 representatives from trace water vapor 30 institutions and 23 (EURAMET 1002) or countries attending the combustion particles meeting (Fig. 1). (EURAMET 1027). New project proposals were A EURAMET Workshop presented, for example dealing with the EMRP: on a comparison “Preparation for a on mixtures of Targeted Program ethanol in water Energy” was held on Fig. 1. Participants of the TC-MC meeting 2009, Bucharest, Romania saturated air (OIML 5 February. Following an recommendation). initial presentation by Jörn which is concerned with the analysis of Ni, Stenger, Member of the EMRP-Committee, on Cd and Pb. The final report for this part was EUROMET Project 886 is now finished. It “Recent developments of the EMRP Program”, presented in April 2009. Step 3 of the project was related to volatile organic compounds possible chemistry-related topics for a TP is concerned with the analysis of Hg, Ni, Cd (VOCs) at ambient concentrations in the Energy were presented. Several aspects related and Pb in natural water at a concentration level atmosphere. These play an important role to biofuels were addressed such as the analysis as required by the European Environmental in the photochemical generation of ozone. of impurities, electrochemical parameters, Quality Standard (EQS) and involves more than EU Directive 2002/3/EC mandates countries quality indicators and the calorific value, as well a hundred testing laboratories across Europe. within the EU to make measurements of the as methods to trace the regional and biological Regional comparison measurements organized specific set of VOC ozone precursors involved origin of biofuels. Other topics were related to by the reference institutes are made in order to in this comparison. 10 institutions from all alternative hydrocarbon fuels, such as Liquefied link these laboratories with the local monitoring over Europe and the United States and South (LNG) or Compressed Natural Gas (CNG) and laboratories. The reference values are provided Korea participated in this project. The World Liquefied Petroleum Gas (LPG). Measurands by the potential calibration laboratories. NMIs Calibration Centre for VOCs under the Global of interest are, e.g., the moisture content. also participate in these comparisons in order Atmospheric Watch Scheme in Garmisch- Other issues discussed were measurements to control the success of the validation. As a Partenkirchen in Germany also participated as for the hydrogen cycle (hydrogen purity) and result, a link between PCLs, NMIs and testing a non-NMI. During this exercise the stability measurements of salinity gradients for efficient laboratories should be established. This part trial of 1-10 nmol/mol VOC mixtures provided water power and drinking water production. was finished at the end of 2009. by NPL (UK) showed less than 0.6% drift for most species over 1 year. The accuracy of Although the European Metrology Research The purpose of EUROMET Project 843 in the these standards was further strengthened by Program is more and more an integral part Sub-Committee for Electrochemical Analysis the comparison results, which showed good of joint activities in the chemistry sector of was to produce new recommendations for agreement between participants. EURAMET, a wide range of further activities are the calibration and evaluation of pH on- ongoing and were also discussed in Bucharest. site measuring instruments in the field of A new proposal for comparison was made by A major activity in the Sub-Committee for water analysis. The resulting protocol is LNE in the Sub-Committee for Organic Analysis Inorganic Analysis is the EUROMET Project 924 intended for on-site measuring equipment and is concerned with herbicides in water as supporting the EU water framework directive. for the determination of pH in water. It gives a support to the EU WFD. LNE has developed The first step of the project linking NMIs and guidance to the end-user on how to estimate materials for the determination of herbicides in reference institutes as Potential Calibration the measurement uncertainty of the pH water stable for three years, namely pesticides Laboratories for priority metals has been value following standard procedures. The in acetonitrile (in vials), and pesticides completed. This step was divided into two vast majority of responses were very positive concentrated on a solid phase extraction. parts, covering the analysis of metals in pure and the document should be translated to LNE proposes to organize an inter-laboratory water and natural water, and was carried out make it available for end users. Possibly, a comparison campaign with these materials in in parallel with a CCQM pilot study which similar protocol shall be developed for multi- order to evaluate the intra and inter laboratory concentrated on mercury (CCQM-P100.1 and parameter instruments in a future project. In precision of this type of determination. P100.2). The final report for CCQM-P100 was total, 14 projects were discussed in the Sub- presented in March 2009. Another part of Committee for Gas Analysis. Five projects Dr. Bernd Güttler the EUROMET Project 924 is the EUROMET were finished, four projects started in 2008. Chair EURAMET TC-MC supplementary comparison, Euromet.QM.S2, They are concerned with issues like laser PTB, Germany

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Recent Activities of the SIM Chemical Metrology Working Group

Activities of the SIM Chemical Metrology agreed to serve as “deputy chair” for one year Friday of that same week. The purpose of this Working Group, implemented through a to assist with the transition. Forum was to provide a venue for dialogue cooperative arrangement between OAS/SIM among policy officials and national decision- and the German Government, provide: The SIM CMWG has organized itself into three makers within the Americas regarding the need ● chemical metrology awareness and strategic needs-based subgroups. Chairs are: and value of investing in national programs in planning seminars ● CMWG Subgroup I: Dr. Yoshito Mitani, chemical metrology to support: ● comparison studies Mexico ● International Trade ● workshops and training activities ● CMWG Subgroup II: Ms. Mónica Gualotuña, ● Food Safety and Nutrition for building capacity, facilitating improved Ecuador ● Sustainable Energy capabilities in Chemical Metrology and the ● CMWG Subgroup III: Ms. Saira Knox, ● Healthcare Decision-Making dissemination of internationally-recognized Trinidad and Tobago ● Consumer Protection measurement services within the Americas and ● Sustainable Economy throughout the world, all within the scope of Characteristics and Focus of Activities and participation in the CCQM and the CIPM within each Subgroup: Invitations for participation in this “Dialogue MRA. CMWG Subgroup - I Forum” were extended to NMI Directors and • NMIs and/or DI that currently have a Government Official with policy-making Most recently, the SIM Chemical Metrology Chemistry CMCs published in CIPM authority and decision-making responsibility for Working Group held events on 2 November MRA Appendix C metrology portfolios for economies within the and 5-6 November 2009 in Rio de Janeiro, ➥ Key and Supplementary Comparison ANDIMET, CAMET and SURAMET subregions Brazil. These events were held adjacent to the Studies to support CMCs of SIM that do not currently have government- CCQM Working Group meetings held in Rio supported programs in Chemical Metrology. A to facilitate the attendance of SIM members CMWG Subgroup - II second such Forum is planned for economies in the chemical metrology area at the CCQM • Economies that have existing within the CARIMET subregion as a part of the meetings, since it was the first time that all mandate for chemical metrology SIM General Assembly in October 2010. the CCQM WGs met in South America. The infrastructure, but currently have no meeting was attended by thirty-two SIM CMC’s published in MRA Database The Forum kicked off with a reception on members representing twelve Economies, two ➥ Awareness seminars: Differences in Thursday evening at Hotel Windsor Barra where Guests from AFRIMETS, one from APMP and expectations of NMI-like activities and Dr. Hratch Semerjian, Director of the U.S. CCQM President Robert Kaarls. those of a testing laboratory Council for Chemical Research, gave a Keynote ➥ Workshops on CMC Preparation and address entitled “Chemical Metrology: What it The Business Meeting featured presentations Review is and Why You should Invest in It”. This was of SIM.QM-K1, “Ethanol in Aqueous Matrix”, ➥ Key, Supplementary, and Subsequent followed by a poster session whose theme was: a review and summary of an activities needs studies to underpin CMCs to be “A National Program in Chemical Metrology: assessment workshop held in Paraguay in proposed Why It’s Needed and What are the Expected May, 2009, a proposal for a Key Comparison of ➥ Measurement Proficiency Assessment Impacts”. Several countries/economies that trace metals in drinking water and a strategic Studies currently have active “Metrology in Chemistry” planning session focused on determining participated. needs for Comparisons, Awareness Workshops CMWG Subgroup - III and other Training Activities for the next • No current NMI (central or Friday’s program featured presentations and a three years. SIM.QM-K1 was the SIM’s distributed) for Chemical Metrology roundtable discussion moderated by Willie E. Chemical Metrology Working Group’s first Key activities May, Chair; SIM Chemical Metrology Working Comparison after more than 20 pilot capability ➥ Need Assessment Seminars Group, which focused on “Chemical Metrology assessment studies that have taken place over ➥ Assistance in framing arguments for and Its Impact on Industry and Quality of Life: the past 10 years. obtaining sustainable government Testimonials and Dialogue” and dealt with the support rationale for and return on investment from It was announced that the SIM Council had ➥ Assistance in conducting Needs national programs in Chemical Metrology. The selected Ms. Gabriela Massiff of CMQ in Chile Assessments with relevant customer topics were discussed by: Prof. João Jornada, to assume Chairmanship of the Chemical sectors President, INMETRO Brazil; Ms. Gabriela Metrology Working Group effective 1 Jan 2010. Massiff, Director, Fundacionchile CMQ Chile; The previous chair, Dr. Willie E. May of NIST, A SIM Senior Policy Makers’ Dialogue Forum, Dr. Yoshito Mitani, Director for Materials sponsored by NIST, was held on Thursday and Metrology, CENAM Mexico; Dr. Wynand

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Louw, Acting CEO, NMISA, South Africa; Dr. SIM Chemical Metrology Working Group • NMI’s from six countries (Argentina, Chainarong Cherdchu, Director for Chemical Summary: Brazil, Canada, Chile, Mexico, U.S.) Metrology and Biometry, NIMT, Thailand; and • 20 countries participate in SIM CMWG have chemistry CMCs in the BIPM Key Dr. Robert Kaarls, CIPM Secretary and CCQM meetings Comparison Database. President, The Netherlands. • 15 NMI’s or their designated labs • Uruguay plans to submit CMCs in the next are now regular participants in SIM few years. Copies of these presentations are provided on intercomparison studies: up from three the SIM Chemical Metrology Working Group in 2002. webpage http://www.nist.gov/cstl/sim_forum. • Six countries are now participating in cfm. Prof. Humberto Brandi, SIM President CCQM meetings and various activities: up Dr. Willie May and Director for Metrology at INMETRO also from three (Canada, Mexico and U.S.) in NIST joined in the panel discussions. 2002. USA

Update on ISO/REMCO

ISO/REMCO is structured as shown on 20 November 2009. Guide 34 in Fig. 1. The committee consists of describes the requirements for the Working Groups (WG) and Ad-hoc quality management system and the Groups (AHG) set up to implement technical competences of reference a specific task under two Steering material producers (RMP). This Groups (SG1 and SG2). The 3rd revision aligns the document Chairman’s Advisory Group (CAG) with ISO/IEC 17025:2005 and has provides input to the Chair from undergone wide consultation the group convenors. with stakeholders, including accreditation organizations. ISO One of the main tasks of ISO/ Guide 34 has become the worldwide REMCO is preparing guides for standard for RMP accreditation the preparation, characterization, and was included into the Mutual certification and use of reference Recognition Arrangement (MRA) materials and the competence of National Metrology Institutes assessment of reference material (NMIs) and other signatories of this producers. A new information MRA. booklet has been published (in English and French) on the The 32nd meeting of ISO/REMCO ISO/REMCO website (www.iso. was held in Teddington (UK) from org/remco) about the role of this 3-6 July 2009 and was hosted by LGC ISO committee, its members, on behalf of the British Standards stakeholders, deliverables and Institute (BSI). ISO/REMCO now working structure. has a membership of 70 members of the International Organization for The main public output from Standardization (ISO) and liaisons ISO/REMCO in 2009 was the third with 18 international organizations edition of ISO Guide 34 “General and 6 ISO-internal committees. The requirements for the competence liaisons are very important for the of reference material producers”, design and implementation of ISO/ which was unanimously approved REMCO’s work program. Most of by ISO members and was published Fig. 1. ISO/REMCO structure the documents from ISO/REMCO

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directly affect work in other (international) extensive consultation with other liaison The Technical Report on RM classification organizations. It is important to avoid organizations; (ISO/TR 10989:2009) has been published. A duplication of efforts and, where possible, to ● complete revision of the guide on first draft of ISO/TR 11773 on RM transportation share resources, especially the limited number accompanying documentation (ISO issues was discussed at the meeting, and it is of experts. For this reason, ISO/REMCO has Guide 31, 2000), expanded to cover all envisaged that a voting draft will be available given a strong mandate to its Steering Group documentation for reference materials; for review at the next meeting. SG1 convener to ensure good communication. ● complete revision of the guide on the use of Moreover, the current extensive and broadly reference materials (ISO Guide 33, 2000); The next ISO/REMCO meeting will be held in scoped work program has prompted ISO/ ● development of a new guide for the Hangzhou, China on 3-7 May 2010. REMCO to request assistance from additional in-house production of in-house used contributors which can provide special reference materials for quality control (ISO experiences from their own field of activities. Guide 80); ● development of a guidance document Prof. Hendrik Emons ISO/REMCO updated its work program during for the production of RMs for “qualitative EC-JRC-IRMM, Chair of ISO/REMCO the meeting in Teddington. Main activities for analysis” (testing of nominal properties); Belgium 2009 and beyond include: ● further studies into the matter of ● complete revision of the vocabulary ‘metrological traceability’, in particular how Dr. John P. Hammond related to reference materials (ISO Guide to express the concept on CRM certificates Convenor of ISO/REMCO WG 6 30, 1992/Amd 1:2008), supported by and related documentation. Starna Scientific Ltd., UK IImportantmportant PPapersapers oonn MiCMiC iinn 20092009

Comparison of Calibration Curves Using the Lp Norm

Luca Callegaro Francesca Pennecchi Pier Giorgio Spazzini

Introduction There are several situations in which point wise specified points. Hence, the data sets realized Interlaboratory comparisons are a fundamental analysis is a loose tool, for instance when the by different laboratories are usually made task in metrology, as they are the main tool to traveling standard is not a realization of the equivalent by comparing “approximately check and maintain the compatibility between quantity of interest but a measuring instrument. coincident” points, but this method appears the various national measurement standards, Examples of such comparisons include those quite questionable. Since the measurement and make them traceable to an international concerning mass flow rate, airspeed, ionizing instruments’ response, although not always standard [1]. Statistical methods for the point radiation, photometry and so on. strictly linear, is usually smooth, one possible wise analysis of such comparisons have been solution could be to determine their calibration extensively studied, and several publications In such cases it might be inconvenient or curves to recompute the expected instrument and guidelines are available on the subject impossible for the laboratories to calibrate responses at the cardinal points and then to (see, e.g., [2]). the instrument on the very same set of compare such results. The logical evolution

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of this approach is to compare the curves as is the (normalized) Lp norm of f(x) on [a, b] that <|| g|| p while, when increasing p, the a whole. [4]. If f(x) describes a dimensional physical higher peak of f(x) becomes more important

quantity, its Lp norm is defined to have the same and the order between norms is inverted. Rationale dimension as f(x). If f(x) = k, for k constant, Comparing calibration curves would provide then || f|| p = |k|, irrespectively of the interval several advantages: first, it would make possible [a, b] and the parameter p. to globally assess the compatibility of the measurement sets; second, it would allow to Three special cases are particularly interesting; obtain, through the global evaluation, at least for p = 1, the norm is proportional to the some indicative results even at those cardinal area of the region bounded by the function points at which an outlier is measured. graph (the shaded area in Fig. 1a) and is the mean value of f(x) on the interval; for p = 2, This approach, although initially studied for it is proportional to the inertia moment of the interlaboratory comparisons, could be useful function graph with respect to the x axis; for p also in other situations, e.g., for analyzing tending to infinity, || f|| ∞ is the supremum of the time drift of the calibration curve of an |f(x)| (if the function is continuous on [a, b], instrument. Possible applications in chemical its supremum coincides with its maximum) on analytical laboratories include development the interval (indicated by the arrow in Fig. 1a). and validation of new methods, quality control and spectroscopic analysis. Presently, the comparison of absorption spectra of unknown compounds to reference spectra is performed Fig. 2. (a) Two functions and (b) the using distance-to-model methods [3]. The evolution of their Lp norm as a function of p method proposed here is an alternative, allowing to directly compute the distance Distance Between Curves between the measured and the reference In order to evaluate the distance between two spectra. functions f(x) and g(x) defined over the same domain [a, b], we propose to consider the Lp Calibration curves should be compared norm (2) of the difference between the two irrespectively of their mathematical curves: formulation, and in a quantitative and objective (3) way. To this aim, we will introduce a distance between two generic analytical curves based on Obviously, this distance has the same properties the Least Power Lp norm of their difference. as the Lp norm of a single function treated in the previous section. In particular, if the curves Lp Norms differ one from the other only by an additive In this context, we restrict the definition of the Fig. 1. (a) A generic function and (b) the term k (simple translation), then DP =|k|, evolution of its Lp norm as a function of p Lp norm (with p ≥ 1) of a function f(x) to the always. If the two curves coincide everywhere case of bounded functions which are defined on [a, b], then DP=0. If g(x) = 0 all over [a, b], on the interval [a, b], having length ∆ = b - a. Fig. 1b) depicts the dependence of on then DP = . If the Lebesgue integral of the p-power of the p. The monotonic increase of the norm absolute value of f for increasing p is a general property [4]. It can The same functions plotted in Fig. 2a) are been seen, as expected, that tends, for plotted again in Fig. 3a), while Fig. 3b) reports (1) increasing p, to the maximum value of f(x). their distance DP ; two special cases of this distance are also graphically represented in is defined and finite, then Figs 2a) and 2b) show function f(x) Fig. 3a), namely p = 1 (the shaded area) and together with another function g(x) and the p tending to infinity (the maximum distance corresponding Lp norms. It is clear that the between the curves, indicated by the arrow). ordering of and | | g| | p is dependent on The distance provides a global evaluation of (2) the value of p. Since the mean value of g(x) is the difference between the curves. For small larger than that of f(x), for low p values one has

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values of p the distance takes into account the Calibration Curves vs a Conclusions and Future overall similarity of the curves, while for large Reference Curve: an Example Developments values of p it highlights the maximum local We show here a specific application example, The distance (3) can be employed to rank differences between them. but many others can be conceived. Assume calibration curves with respect to a reference that the calibration curve of an instrument has one. If the interest is focused on the overall the form of a second order hyperbola f(x) = differences between the curves, a small p value 2 a0 + a1/x + a2/x , and that the instrument is is appropriate, for example, when dealing with calibrated at five different laboratories. The a global assessment of a calibration laboratory result of each calibration is the estimate of the in an audit. Otherwise, if large (although local) parameters a0, a1, a2, whose corresponding differences are important for the context, a curves are plotted in Fig. 4a) together with a large p value should be used, for example, to reference curve REF, the red one, which is here identify the presence of outliers. considered as given. Two major problems are currently subjects of a work in progress: • the determination of a reference curve, which will be addressed by considering, as the reference curve, the function minimizing the norm of the vector of the distances between the calibration curves and the function itself; • the evaluation of the uncertainty associated Fig. 3. (a): The same curves as in Fig. to the distance between a calibration 2a) and graphical representation of curve and the reference one, which will be two special cases of their distance; (b) undertaken by considering the calibration Relative distance as a function of p curves as random functions.

A small variation of the distance all over the This article is a summary and update range of p will indicate that the curves can be of the CITAC Award winning paper considered similar in shape, although shifted published by the authors in Accreditation and Quality Assurance (2009) 14:587-592. with respect to each other. In this case, the Fig. 4. (a) Diagrams of five pseudo- question is whether such (almost) constant calibration curves (thin lines) and of a References distance represents a small or a significant reference curve (thick red line); in the [1] CIPM, Mutual recognition of national amount with respect to the actual context. On box, a zoom of the region with the highest measurement standards and of calibration and the other hand, a small value of the distance for slope. (b) Distances of the five curves measurement certificates issued by national small p values followed by a strong increase for from the reference curve; in the box, a metrology institutes, BIPM, Sèvres, France, 1999. large p values will indicate that the curves are zoom of the region close to origin [2] M. G. Cox, The evaluation of key relatively close to each other except in some comparison data, Metrologia, 39(6), 2002, reduced regions where large differences may Fig. 4b) shows distances (3) of the calibration pp. 589–595 exist. In this case, one should decide which of curves from REF, as functions of p. For low [3]http://www.thermo.com/com/cda/ the two aspects is more important for the aim of values of p, curves 1 and 3 have the smallest resources/resources_detail/1,,13229,00.html the actual analysis: the good overall agreement distance. Actually, from Fig. 4a), curves 1 and [4] S. Y. Hwang, On Monotonicity of Lp and lp between the curves or their few but high 3 seem on the average closer to REF than the Norms, IEEE Trans. Acoust., Speech, and discrepancies. Moreover, if a maximum value others. On the other hand, the distance of Signal Processing, ASSP-f 3, 1975, pp. 593–594 (e.g., a prescribed tolerance) for the distance curve 3 from REF rises quickly and becomes between two curves is set, it is possible to check the largest, for large p. In fact, curve 3 has which range of p satisfies such condition; this Dr. Luca Callegaro the largest local distance from REF among all result would allow to check whether the curves Dr. Francesca Pennecchi curves, as can be seen by carefully observing are within tolerance only in a global sense or Dr. Pier Giorgio Spazzini the zoom in the box of Fig. 4a). also locally. INRIM, Italy

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Metrological Aspects of Glucose Measurements by Biosensors

Samuel Wunderli Hanspeter Andres

Introduction Self-monitoring and point-of-care testing devices In this work we present a calibration method National regulations and the European use direct reading biosensors that do not need for glucose measurements without the Directive on In Vitro Diagnostic Medical prior dilution of the test sample. They respond need of prior dilution of the specimen. Devices (IVD Directive, 98/97/EC) [1] demand to (active) glucose molality, the amount of Chronoamperometric measurement signals that traceability of values assigned to calibrators glucose per unit mass of water. The quantity of a glucose sensitive biosensor based on and/or control materials must be assured molality is identical in whole blood, plasma or Glucose-Oxidase and a mediator that prevents through available reference measurement aqueous solutions. But, for concordance with the formation of hydrogen-peroxide are used procedures and/or available reference materials traditional methods, the results are converted as the direct measure of the active glucose of a higher order. The Joint Committee on to concentration. This quantity now depends molality. This work focuses on the metrological Traceability in Laboratory Medicine (JCTLM) on the water content, which is different for aspects of such a quantitative electroanalytical provides a worldwide platform to promote and whole blood, plasma and aqueous solutions. measurement method. Up to now, neither give guidance on internationally recognized The International Federation of Clinical a thorough uncertainty evaluation of and accepted equivalence of measurements Chemistry and Laboratory Medicine (IFCC) chronoamperometric measurements results in laboratory medicine and traceability to therefore recommends reporting result for of glucose contents has been done nor has appropriate measurement standards. Based blood glucose always as concentration of their traceability to internationally recognized on its legal mandate the Federal Office glucose in plasma. [2] For each calibration standards been established. of Metrology METAS (the Swiss national solution the factor varies. False conversion metrology institute) is building up a laboratory factors in the calibration of glucose monitors Experimental infrastructure for electro-analytical chemistry with concentration standards can thus lead to The amperometric sensor is a three-electrode to provide a valuable contribution to the false positive or false negative measurement device mounted in the fully automated flow traceability of glucose content measurements results. [3] system depicted in Fig. 1. The working by biosensors and ion activity measurements.

The measurement of blood glucose levels is one of the most common tasks of a clinical chemical laboratory. Various types of instruments detect and report fundamentally different glucose quantities. In the clinical chemistry laboratory routine glucose measurements are primarily performed by photometry based on the absorbance of molecules involved in the enzymatic conversion of glucose in diluted samples. Results are reported as glucose concentration, amount of glucose per volume of specimen. Glucose concentration standards are available either as pure materials or frozen human serum with concentration in the Fig. 1. Amperometric flow system at METAS equipped with flow cell and electrodes: WE = -1 -1 physiological range (2 mmol·L to 20 mmol·L ). working electrode, RE = reference electrode, CE = counter electrode and DB = database

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Table 1. pH, ionic strength I and glucose molality m of the buffered glucose standards and test samples n is the number of released electrons, A is the name buffer type pH ionic glucose uncertainty um, strength I, molality m, geometric surface of the planar electrode, F mmol·kg-1 mmol·kg-1 mmol·kg-1 % is the Faraday constant, DS is the diffusion coefficient of the substrate glucose and δN is I1 imidazole 7.2 156.788 2.761 0.015 0.53 the thickness of the Nernst diffusion layer. In I2 imidazole 7.2 157.216 11.324 0.028 0.25 this work eq. 1 is extended by a dynamic term I3 imidazole 7.2 156.795 5.650 0.022 0.38 k(t) and a drift term D(t) as shown below: I4 imidazole 7.2 156.794 8.446 0.025 0.29 I6 imidazole 7.7 148.623 5.465 0.018 0.33 I7 imidazole 6.7 166.738 5.372 0.018 0.34 (2) The quantification of the uncertainty is done I9 imidazole 7.2 238.290 ~ 5.5 according to the principles outlined in GUM P1 phosphate 7.2 130.611 2.747 0.015 0.53 [6]. The combined uncertainty of the potential P2 phosphate 7.2 130.611 11.271 0.028 0.25 signal result from eq. (2) is equal to the positive square root of the combined variance , P3 phosphate 7.2 130.611 5.497 0.021 0.39 which is given by: P4 phosphate 7.2 130.611 8.298 0.025 0.30 P6 phosphate 7.5 128.021 5.479 0.018 0.33 (3) P7 phosphate 6.5 132.473 5.459 0.018 0.33

P9 phosphate 7.2 211.035 ~ 5.5 Covariances are not considered in our approach at present. The standard uncertainties electrode is composed of platinum prevented by adding sodium azide. The purity of each influence xi are either of the A- or B- contacted glucose sensing paste. The paste of the glucose used was 99.7 ± 0.4 % (k = 2. 95 % type. A-type uncertainties can be evaluated from consists of glucose oxidase (GOD), the confidence interval). The gravimetric data of statistical distribution of the results of a series mediator system Tetrathiafulvalene - p- all imidazole buffered glucose standards and a of measurements, while B-type uncertainties Tetracyanochinodimethane (TTF - TCNQ) test sample used in this study are summarized are evaluated from assumed a priori probability and graphite suspended in silicone-oil. [4] To in Table 1. The uncertainty calculation for distributions based on experience, and from prevent depletion of the water soluble GOD the glucose molality includes uncertainty other information originating from separate during operation the paste is protected by a 20 contributions of the weighing data and experimental results. - 50 μm cellulose cut open tubular membrane. environment as well as of the glucose purity. The reference electrode is a closed system Ag/ AgCl gel-type reference electrode. The counter Theory Results and Discussion electrode is simply a platinum wire. The current Glucose oxidase is often used in direct reading In Fig. 2 the chronoamperometric response between the working and counter electrode biosensors to determine glucose enzymatically, signal I of a glucose sensitive electrode after applying a constant voltage between the a process during which the chemically active during the course of a fifty hour experiment is working and reference electrode is measured form of ß-D-glucose is transformed highly depicted. The measuring system was calibrated with a potentiostat. The electroanalytical signal selectively into 5-gluconolactone. Two by alternating the glucose standards I1, I2, I3, together with the environmental and flow electrons are released for each converted I4, I1 and P1, P2, P3, P4, P1, respectively. For system control parameters are recorded in a glucose molecule and mediated to the each buffer type two independent calibrations database. Platinum electrode at a constant potential. This were performed. The samples I9 and P9 were electron stream is the evaluable measuring treated as unknown test samples and measured A standard for glucose measurements is signal in chronoamperometry and is directly in between the respective system calibration. a buffered and sterilized aqueous glucose proportional to the glucose content of the After each solution change the system was solution of known molality. In this work sample under test. [5] The limiting current Il at flushed with the subsequent solution for two aqueous imidazole or phosphate buffers in the a planar electrode with strong radial diffusion is minutes. The measurement interval is two pH range 6.7 - 7.7 were used. Where necessary, directly proportional to the substrate activity aS: hour per sample. The observed current varies lithium chloride was added to adjust the ionic in the range of 100 nA to 500 nA, depending strength to the physiological range. Fouling (1) on the glucose content of the sample under of the buffered aqueous stock solutions is test. As depicted in Fig. 2 only a very small

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with typical values xi for all influences xi of the model eq. (2). Table 3 also lists the measured

limiting current Il and calculated combined uncertainty .

Whereas for =0.000 all three

uncertainties u(aS), and u(D) contribute to the combined uncertainty, for =

0.005 the uncertainty of Il is dominated by the uncertainty of the dynamic term k.

The glucose activity for the test samples I9 and P9, respectively, is determined as follows. From the glucose molalities of the standards I1, I2, I3, I4, P1, P2, P3 and P4 in Table 1 and the measured limiting current values of the standards and the two test samples I9 and P9 in Tables 2 and 3, respectively, the glucose molality can be determined using the Fig. 2. A fifty hour chronoamperometric experiment is shown: a) measured applied bracketing technique with a linear regression voltage U between working and reference electrode, b) measured resulting current I according to ISO standard 6143 [7]. In this type between working and counter electrode. The limiting current value for the standard of linear regression both the uncertainty in the I3 in the imidazole cycle 2 is marked. The broken line visualizes a small linear signal glucose molalities as well as the uncertainty in drift D(t) for the standard I1. Part c) is measured flow displaying the sample changes the measured currents are taken into account. within the two measurement cycles of the imidazole and phosphate buffer system, The calibration and analysis functions are respectively depicted in Fig. 3 assuming no uncertainty in the dynamic term k . The resulting values for linear drift of approx. 2 nA / 24 h is observed. latter time than for the test sample I9. For glucose activity of the samples I9 and P9 are Typically the signal reaches a steady state after the subsequent signal analysis the last 100 s summarized in Table 4. an hour of measurement of a new sample. For before a sample change are used to determine the samples I9 and P9 the response behaviour the limiting current I . The mean experimental l The values determined are concordant is different; after a decrease of the signal within values of I for all cycles are summarized in l between the two measurement cycles and the first hour the current increases again Table 2. buffer systems, as can be seen from Fig. 3 towards the end. This behavior is attributed and Table 4. Concordance is already achieved to the reference electrode, which stabilizes The uncertainty budget for the response signal assuming zero uncertainty in the dynamic much later due to the different ionic strength I of the sample I2 and P2, respectively, is listed l term for both buffer types. For the imidazole of the samples (see Table 1). Clearly, for the in Table 3. The mathematical expressions of buffered test sample I9 the glucose activity test sample P9 the steady state is reached at a the derivatives in eq. (2) are given together can thus be determined with a combined uncertainty of 0.5 % rel. For the phosphate Table 2. Mean experimental values of current Il are summarized of measurement cycle 1 of the imidazole and phosphate buffer system, respectively. The respective standard buffered test sample P9 the combined deviations s(Il) are given in brackets uncertainty is 0.8 % rel.

sample imidazole sample phosphate Conclusions cycle 1 cycle 1 Based on the model equation for the current Il (nA) current Il (nA) measurand, all significant sources of I2 503.1(4) P2 460.3(3) uncertainty of the analyte result are identified, their magnitude estimated from published and I3 224.9(2) P3 199.2(2) experimental data and finally mathematically I9 217.3(4) P9 201.0(9) combined to give the combined uncertainty in the reported value of the glucose molality. It I4 357.1(5) P4 327.3(1) is found, that the combined uncertainty of the I1 81.2(2) P1 65.4(1) glucose molality comprises mainly uncertainty contributions from the non-ideal behavior, the

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chronoamperometric measurement setup and from the used glucose purity. The expanded uncertainty is below 2 % rel. (k = 2, 95 % confidence interval) of the glucose content determined by bio-electrochemical measurements, thus competes well with today’s considered most accurate reference method IDMS [8]. The advantage of the presented calibration method is its directness, the glucose content is determined without prior dilution of the sample. Furthermore, by restriction to the quantity molality no conversion factors for different specimens are needed as it is the case for concentration measurements.

This article is a summary and update of the CITAC Award winning paper published by the authors in Electroanalysis (2009) Fig. 3. Calibration functions with four glucose standards (open symbols) and 21: 1984 – 1991. one test sample (full symbols) are depicted; a and inset a) standards I1, I2, I3, I4, test sample: I9; b and inset b) standards P1, P2, P3, P4, test sample: P9. The analysis function is the inverse of the calibration function. From the depicted References [1] Directive 98/79/EC of the European analysis function (full lines) with 95 % confidence interval (dotted lines) the Parliament and the council on in vitro unknown glucose activity of the test samples and their respective uncertainties diagnostic medical devices (p.36), Official can be mathematically determined Journal of the European Communities 1998, L331, 1-37 Table 3. Uncertainty budget and resulting limiting current and combined [2] P. D’Orazio, R. W. Burnett, N. Fogh- uncertainty of the standards I2 (imidazole buffer) and P2 (phosphate buffer) Andersen, E. Jacobs, K. Kuwa, W.R. in cycle 1 are listed Külpmann, L. Larsson, A. Lewenstamm, A.H.J. Maas, G. Mager, J.W. Naskalski, A.O. Okorodudu, Clin. Chem. Lab. Med. 2006, 44, 1486 – 1490 [3] J. Mahony, J. Ellison, Clinical Chemistry 2007, 53, 1122 – 1128 [4] a) A. Chaubey, B.D. Malhorta, Biosensors & Bioelectronics 2002, 17, 441 – 456. b) J. P. Müller, Dissertation ETHZ Nr. 13743, 2000 [5] F.G. Cottrell, Z. Physik. Chem. 1902, 42, 385 [6] ISO/IEC Guide 98, Guide to the expression of uncertainty in measurement (GUM), 1995 [7] ISO 6143, Gas analysis – Comparison methods for determining and checking the composition of calibration gas Table 4. Glucose activities a and uncertainty u(a) of the test samples I9 and P9 mixtures, 2001 for uncertainties in the dynamic term k of 0.000 and 0.005 are listed [8] a) D. Stöckl, H. Reinauer, Clin. Chem. 1993, 39, 993-1000, b) L. Thienpont, A.P. Leenheer, D. Stöckl, H. Reinauer, Clin. Chem. 1993, 39, 1001-1006

Dr. Samuel Wunderli Dr. Hanspeter Andres METAS, Switzerland

● 29 / CITAC NEWS ● FEBRUARY 2008 CITAC NEWS FEBRUARY 2010 / 29 IImportantmportant PPapersapers oonn MMiCiC iinn 22009009 A Convenient and Economic Approach to Achieve SI-traceable Reference Values to be Used in Interlaboratory Comparisons Concerned with Water Analysis

Olaf Rienitz Detlef Schiel Bernd Güttler Michael Koch Ulrich Borchers

Introduction To obtain metrologically traceable reference taken advantage of by regarding and evaluating Within the scope of European harmonization, values the usual way using so-called primary the comparison as a standard addition. The gap for example the Drinking Water Directive methods is often demanding with respect to between the measured values and the added 98/83/EC [1] and the Water Framework time and cost. concentration arises from the matrix content. Directive 2000/60/EC [2] are demanding Therefore the measurement results of the the comparability of measurement results. Two interlaboratory comparisons addressing participants themselves provide the missing Comparability can be achieved by implementing heavy metals in drinking water are discussed piece needed to complete the reference value a traceability chain to the SI units via national in detail taking lead as an example to show a without any additional measurements. standards. National standards are developed convenient way to generate metrologically and provided by National Metrology Institutes traceable reference values solely based on Refusing the straightforward use of consensus (NMIs) [3]. data collected during these comparisons. values as metrologically traceable ones, but PT providers usually prepare their samples applying them to introduce a minor correction In the field of analytical chemistry proficiency by adding appropriate amounts of the to the beforehand incomplete reference values testing (PT) rounds play an important role in analyte elements to natural drinking water seems to be a contradiction. The special verifying measurement results even though (matrix). Doing this addition volumetrically properties of standard addition are able to reference materials (RMs) or even certified or gravimetrically, the added amount is well- smooth this out. For example: the result of a reference materials (CRMs) are used for known, especially if certified reference materials standard addition experiment remains totally calibration purposes. Therefore, in Germany, are used. Even though the matrix content of the unaffected by recovery problems, because all laboratories responsible for drinking-water analyte elements is low, reference values have the slope and the y-intercept are changed monitoring regularly have to participate in to include these matrix contents along with by exactly the same factor. However there interlaboratory comparisons. The German their measurement uncertainties to become may exist any constant biases misleading the drinking water directive [4] establishes the traceable. Therefore, the matrix contents have standard addition. To rule this out and to prove corresponding legal basis in conjunction with to be measured and their uncertainties have to the whole approach experimentally, IDMS as a recommendation issued by the German be estimated. a primary method was applied to determine Federal Environment Agency (UBA) [5]. reference values that are independent of the Measuring these matrix contents directly sample preparation. In the last consequence only interlaboratory is often a challenging task and yields poor comparisons providing metrologically traceable uncertainties. The experimental design of Two different ways of sample preparation reference values instead of consensus values the discussed comparisons, however, offers (volumetric and gravimetric) were scrutinized can help to establish national and international a totally different way to obtain the matrix with respect to the metrological traceability comparability. As an additional benefit such contents. To avoid cheating and to check their of the added analyte contents. The crucial reference values enable the participating measurement capabilities over a certain range, point was to set up an equation describing laboratories to check their results for accuracy the participants are provided with randomly the particular sample preparation procedure. on a reliable and unbiased basis. selected samples out of a pool of up to 12 This so-called mathematical model of the concentration levels covering nearly two orders measurement (model equation) was used of magnitude. This complex design can be to estimate the measurement uncertainty

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of the added amount of analyte according to the matrix content β0 and the concentration relative uncertainties of the means are more the Guide to the Expression of Uncertainty in arising from the added amount of the analyte than 10 times larger than the uncertainties of Measurement (GUM) [6]. (added mass concentration βadd). Eq. 1 shows the added mass concentration it is reasonable the corresponding relation with lead as an to determine the parameters a0 and a1 by Combining the added concentration of analyte example. an ordinary least square fitting (ODF). The βadd and the concentration β0 arising from the uncertainty associated with the matrix content matrix resulted in the desired reference value (1) was calculated according to an equation E rcm Pb Eadd Pb  E0 Pb β (Fig. 1). The corresponding model equation published in [9]. needed in the uncertainty budget reflects also This equation can be regarded as a linear the traceability chain by linking the reference equation with a slope of 1 and a y-intercept Reference Values value directly to the purity of the applied equal to β0(Pb). Unfortunately, the slopes were The reference values were calculated as the certified reference material (standard). not very close to one. For lead, for example, sum of the added mass concentration and a slope of approximately 0.95 was found. the matrix content obtained by the described standard addition-like method:

E Pb Eadd Pb  E0 Pb (3)

Despite of the different relative expanded uncertainties associated with the gravimetric and volumetric sample preparation (< 0.4 % and < 1 %, resp.), eq. 3 as the mathematical model, yielded relative expanded uncertainties of 2 to 20 % associated with reference lead concentrations of 5 to 50 μg/L regardless of the preparation procedure. These calculated reference values were compared to the reference values determined by the IDMS measurements (dashed red line, Fig. 2). Unlike the consensus values (dashed yellow line, Fig. 2), they were in very good agreement with the Fig. 1. The SI traceable reference value β(Pb) can be obtained on several different IDMS values. Their uncertainties and deviations ways. Solid line: An example using the added content β (Pb) from a gravimetric add from the IDMS values increased all the more, the preparation, combined with the content β (Pb) arising from the matrix calculated 0 closer the reference values got to the matrix using the consensus values and the preparation. concentration. This behavior is reasonable because larger concentrations should be Results and Discussion Therefore it was necessary to rearrange eq. 1 measurable with smaller uncertainties. to yield a more general form (eq. 2). Providing Therefore, the added mass concentrations Matrix Content that the means recover a certain fraction a1 of completed by the matrix concentration The content arising from the matrix β (matrix 0 the true lead concentration β(Pb) leads to: derived from the consensus values were content) was determined equally to a standard suited for use as the reference values. By addition experiment. This requires the analyte contrast, the deviations and the uncertainties already present in the matrix and the added E ˜ E ˜ E  ˜ E rcm Pb a1 Pb a1 add Pb a1 0 Pb of the consensus values themselves showed analyte to behave in the same way, which a0 no dependency on the concentration (Fig. 2). is a reasonable assumption considering the E Pb a ˜ E Pb  a rcm 1 add 0 While the deviations were more than twice as analyte element(s) and the drinking water a E Pb 0 large, the uncertainties were smaller. A few matrix. The results of the participants of the 0 a 1 values were in good or acceptable agreement interlaboratory comparisons 3/2004 TW A2 with the IDMS measurements, but they were and 1/2006 TW A2, respectively, were used to (2) scattered randomly over the concentration calculate the robust consensus means β of rcm This linear function shows that the matrix range. Therefore, the use of consensus values all samples [7, 8] along with their uncertainties. content β (Pb) is equal to the x-intercept of as the reference values seems questionable. These means should represent the sum of 0 the plot βrcm(Pb) vs. βadd(Pb). Given that the Furthermore, there would be no proper

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Conclusions It was demonstrated that SI-traceable reference values to be used in drinking- water interlaboratory comparisons can be achieved without any additional efforts. These reference values were obtained by combining already existing data coming from the sample preparation and the consensus values. As expected, the gravimetric sample preparation yielded a slightly smaller uncertainty than the volumetric, but the uncertainty associated with the reference value was virtually not affected by the contribution of the sample preparation procedure.

To improve the reliability of the calculation of the matrix content and its uncertainty in the meantime the ordinary least square fitting was Fig. 2. Relative deviations of the reference values (∆1, red) and relative replaced by a generalized least square fitting, deviations of the consensus values (∆2, yellow) from the IDMS values βIDMS(Pb). The deviations of the consensus values are larger (< 10 %) and in several cases taking into account the uncertainties of the not or in poor agreement with the values determined by the IDMS measurements, added amount of analyte as well as of the even considering their uncertainties (not shown in the figure for the sake of robust consensus means [10]. clarity) There is only one additional effort the PT provider has to face: Setting up a proper way to show the traceability to the SI. Very experimentally by IDMS measurements for uncertainty budget describing the sample similar results were also found for cadmium, cadmium, chromium, copper, lead, and nickel preparation. This concept shows a way to chromium, copper and nickel, regardless in the concentration ranges usually found provide SI-traceable reference values without of the preparation method (volumetric or in German drinking-water interlaboratory the regular participation of an NMI applying gravimetric). comparisons. At least for these elements and primary methods being necessary. The role concentration ranges, the reference values of the NMI is focused on the validation of the obtained by combining the volumetrically or application of the described concept. This Traceability to the SI gravimetrically added amount and the matrix task may include guidance and support in the The added mass concentration βadd(Pb) is content calculated with the described standard uncertainty calculation, but may include just traceable to the SI by linking it to the certified addition-like method using the consensus as well the participation in interlaboratory mass concentration of the reference solution values have proven to be traceable to the SI. But comparisons, i.e. from time to time or if the βref and the purity of the certified reference there are limitations that need further research: concept shall be applied to problematic material wpur, respectively, provided that elements or other analytes that are volatile or analytes or analytes other than the discussed βref and wpur, respectively, are traceable not stable and therefore tend to change their ones, and to changed matrices. themselves. Unfortunately the matrix content concentration in an unpredictable way after derived from the consensus values at first does the preparation, which causes the value of not seem to be traceable to the SI. But the the added mass concentration to be useless. Outlook uncertainty associated with the matrix content Under these circumstances, contributions have At the moment a European interlaboratory calculated using the consensus values is large to be added taking stability, adsorption and/or comparison (Euromet 924 part 3) and a enough to cover its true value. Furthermore, volatility problems into account. Another closely connected international comparison the matrix is just a small contribution to the problem is caused by matrix concentrations in (CCQM-P100.3) organized by PTB, BAM, LNE, reference value, except for those close to the the order of the reference values themselves. IWW and EC-JRC-IRMM are in progress. These matrix content. But even in these cases, the The resulting large uncertainties associated comparisons are aiming at the determination uncertainty associated with the reference value with the reference values may limit their use as of the mercury mass concentration in a natural (now dominated by the contribution of the reference values. water matrix on a concentration level below matrix content) increases sufficiently to include 100 ng/L (as required by the WFD, [2] and the true value (Fig. 2). This was demonstrated [11]). All participants received not only the

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sample itself but also one or more additional consumption, Official Journal of the [8] ISO 13528:2005 Statistical methods for use sample(s) adjusted at well-known higher European Communities, L 330/32, 1998 in proficiency testing by interlaboratory concentrations. This is going to be the first [2] Directive 2000/60/EC of the European comparisons time that in the case of very low concentrations parliament and of the council establishing [9] O. Rienitz, K. Röhker, D. Schiel, J. Han, D. (only 10-20 times above the matrix content) a framework for Community action in the Oeter, New Equation for the Evaluation of and with a volatile analyte (Hg) the approach field of water policy, L 327, 2000 Standard Addition Experiments Applied described has to prove its applicability even [3] H. Kipphardt, R. Matschat, O. Rienitz, D. to Ion Chromatography, Microchim. Acta under these demanding circumstances. Schiel, W. Gernand, D. Oeter, Traceability 154, 21-25 (2006) system for elemental analysis, Accred Qual [10] M. Koch, F. Baumeister, Traceable The method described is routinely applied in Assur (2006) 10: 633–639 reference values for routine drinking water one of the German water PT schemes (AQS [4] Verordnung über die Qualität von proficiency testing: first experiences, Baden-Württemberg) since 2007. To proof Wasser für den menschlichen Gebrauch Accred Qual Assur (2008) 13:77-82 the absence of unrecognized uncertainty (Trinkwasserverordnung – TrinkwV 2001), [11] Directive of the European parliament and sources and to fill the lack of traceability of the Bundesgesetzblatt, Teil I Nr. 24, 2001 of the council on environmental quality reference materials used for the fortification [5] Umweltbundesamt, Empfehlung für standards in the field of water policy and of the samples more reference measurements die Durchführung von Ringversuchen amending Directive 2000/60/EC, 2006/ will be needed. zur Messung chemischer Parameter 0129 (COD) und Indikatorparameter zur externen This article is a summary and update Qualitätskontrolle von Trinkwasserunter of the CITAC Award winning paper suchungsstellen, Bundesgesundheitsbl – Gesundheitsforsch – Gesundheitsschutz, published by the authors in Accred. 2003, 46:1094-1095 Dr. Olaf Rienitz, PTB Qual. Assur (2007) 12:615-622. [6] Guide to the Expression of Uncertainty in Dr. Detlef Schiel, PTB Measurement, ISO, Geneva (1993) Dr. Bernd Güttler, PTB References [7] DIN 38402-45:2003 Ringversuche Dr. Michael Koch, ISWA, University of Stuttgart [1] Council Directive 98/83/EC on the zur externen Qualitätskontrolle von Dr. Ulrich Borchers, IWW quality of water intended for human Laboratorien Germany

DDiscussioni s c u s s i o n PPapersa p e r s

Should We Look More Closely at the Measurement Results We Compare?

In a chapter contributed to a recent book [1], attempt was made to give the readers of the a scientific debate is needed, followed by a we took a closer look at a number of graphs book some “food for thought”. A mere look suitable dissemination of its conclusions. in which measurement results are compared. at the examples given in the graphs in Fig. 1 The chapter was written at the insistence of and 2 presenting comparisons of measurement When looking at these graphs, one of the most the book’s editors, who indeed wanted a closer results, raises a number of questions, to which striking observations is the absence of “normal look at comparisons of measurement results answers have either not (yet) been given, distribution” of the results. Yet, the assumption sampled from practice, regardless of how they or not made properly known to the users of “normal distribution” around a most likely would look. In retrospect, the contrast with concerned, or the answers are unsatisfactory, ‘reference quantity value’ is encountered the other chapters of the book provides a rare or they unveil a variety of opinions, if not many times in the chemical literature on comparison of theory and practice in matters outright controversy. Thus the very reason comparisons and used as basis for conclusions: of comparing measurement results. Thus an for this chapter in this book simply is that “On the assumption that the data are normally

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Fig. 1.

Fig. 2.

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distributed, ...” or “Assuming a normal Thus a number of questions are formulated result a priori, cannot use the calculated distribution of the data ,...”. Thus the question in the chapter and attempts are made to give average (or median or mean) as a(n other) is discussed whether “normal distribution” of them a preliminary answer: metrological reference a posteriori? measurement results can be “assumed” if clear 1. Must an organizer of an ILC, who is going 14. Isn’t the basic product of an ILC to establish proof is presented of absence of it. Wouldn’t it to compare the participants’ measurement some sort of “degree-of-equivalence” of be indicated to only build any conclusion on results, not verify whether they are any specified pair of results of participants, normal distribution after such a distribution “comparable” in principle? rather than comparing and possibly has been shown in an unambiguous picture 2. Must the organizer of an ILC not request combining measurement results? to apply in the particular case of measurement metrological traceability from each 15. Is a “consensus value” for the certified concerned? participant for his measurement result? quantity value(s) carried by a calibrator 3. Doesn’t an ILC organizer need to require (CRM) (average, median, mean of selected A large majority of relevant literature assumes a statement of measurement uncertainty values) metrologically traceable? normal distribution as a matter of course, from any participant? 16. Isn’t measurement uncertainty sometimes sometimes even in the case of absence of it. 4. Is the establishment of metrological (instinctively) made larger to encompass a Isn’t this matter for debate? Thus the chapter traceability not a prerequisite for the perceived uncertainty in the statement of a of the book asks some 18 questions to generate evaluation of measurement uncertainty? metrological traceability? that debate. 5. Can we combine two measurement results 17. Is it possible to state or establish a (non- which are not metrologically comparable? metrological) form of traceability for a Another feature of the chapter is that a 6. Must each participant of an ILC establish “consensus value” of an ILC? distinction is made between comparison of himself the metrological traceability of his 18. Is the measurement uncertainty claimed two measurement results and comparison of own measurement result before measuring for a ”certified measurement result” many measurement results. In practice, many the measurand concerned in an ILC? which is generated from the combination cases of comparing measurement results 7. Can measurement results in chemistry in of several measurement results with are involving only two parties: buyer-seller, an ILC automatically be expected to be full (GUM) measurement uncertainties, inspector-inspected, regulating-regulated. Yet, normally distributed around a reference obtained by, for example, a few National an enormous interest goes to the comparison quantity value? Metrology Institutes, smaller or larger than of many measurement results, thus establishing 8. Can general conclusions which are based the individual measurement uncertainty of a multi-party context with the ensuing complex on the assumption of a normal distribution either of the two individual measurement statistical treatments of these results. around a reference quantity value be drawn results? when experimental evidence does not Why? substantiate such a distribution? A good debate is suggested. 9. Do the different measurement results of an To have a general background view of the state ILC belong to a same population? References of the practice in which the two parties are 10. If the average, or mean, or “cleaned” mean [1] Paul De Bièvre, Comparing results of active? Maybe. of the participants’ results derived from an chemical measurements: time to raise some Do they need this general overview in case they ILC, where metrologically traceable and basic questions from practice. Chapter 8 might need an umpire to settle a dispute? non-metrologically traceable measurement in F Pavese and A B Forbes (Eds): “Data Maybe. results are sometimes mixed (“combined”), Modelling for Metrology and Testing in Do they need that to settle a dispute over a can that lead to a “reference quantity value”? Measurement Science”, Birkhauser, Boston difference – or reach agreement – about their 11. To which extent is a subsequent calibration 2009, 255-273; DOI 10-1007/978-0-8176- measurement results? of measurement procedures, using such a 4804-6_8 Not really. reference quantity value, a circular process [2] BIPM, IEC, IFCC, ILAC, ISO, IUPAC, IUPAP, if the same measurement procedures were OIML: The International Vocabulary of Mostly, their problem is whether their used in the establishment of the reference Metrology, Basic and General Concepts and measurement results are compatible [2] quantity value? Associated Terms - VIM, JCGM 200-2008, or equivalent, regardless of what other 12. Who is then guarding orthodoxy in this http://www.bipm.org/en/publications/ laboratories achieve. process? guides/vim.html End of story. 13. Does the very fact of participating in So, why requiring a multi-inter laboratory an ILC not have as logical consequence Prof. Paul De Bièvre comparison (ILC) to enable two parties to that the participant who offered a non- Independent Consultant on settle their compatibility problem? metrologically traceable measurement Metrology in Chemistry, Belgium

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1. National Metrology Institutes procedures (e.g. traditional AOAC approach) basic requirement for establishing sustainable National Metrology Institutes (NMIs) are → measurement procedures for a specific approaches for ensuring the integrity of the guardians of quality measurements measurand → to routine bulk assay procedures; analytical results in several F&N areas. for a given country. They are the primary and (ii) the other, that reflects a decreasing interface between internationally recognized traceability link by using primary standards → Importantly, a change of this magnitude calls measurement systems and national primary (natural matrix) reference materials for bold, swift and decisive efforts by the NMIs measurement requirements, related to → secondary reference materials → tertiary and the policy makers in the food, nutrition traceability and accuracy, among others. As reference materials → to in-house reference and health sectors. custodians for national metrology systems, materials or control materials. Importantly, the NMIs facilitate international comparability a clear picture of uncertainty and traceability 2. Food and Nutritional Metrology as a for quality systems, and permit calibration of is critical to establish a basis for credible Part of Biological Metrology standards at the national level, that extends comparability, when results are generated in Dealing with the F&N measurements involves through various measurement linkages down different geographical locations under differing handling of complex chemical and biological to the measuring equipment at the user level. laboratory conditions [1]. matrices for numerous assays. The food as a Simultaneously, they establish traceability natural matrix in its many forms, presents a for the field equipment through → working 1.2. Extending out-reach to every-day variety of problems in achieving a meaningful standard → secondary standard → and thus Measurement Communities analytical result. e.g. food composition providing a link to the national standard, as As the torch-bearers for strengthening the and food safety areas. Further, dealing a part of the required validation process. The usefulness of measurements, the role played with nutritional investigations extends the NMI infrastructure generally includes extensive by the NMIs is rather unique. In addition to measurement process into the physiological laboratory set-up, scientific and technical the pivotal functions outlined above, they have and metabolic domains, leading us to the capabilities and expertise, and is generally well other responsibilities: e.g. (i) strengthening the complexity of metrology in biology [2]. There equipped to meet the needs of various statutory metrological basis of various measurements, are several issues surrounding these concepts responsibilities; e.g. meeting regulatory and (ii) imparting these metrological concepts that need to be carefully evaluated to enhance requirements in chemical and physical for strengthening awareness in the minds of the reliability of F&N analytical results and to measurements, ensuring harmonization for the analytical professionals. It is recognized ensure sustainability to the QA process [3,4]. units and setting standards for measurements, that experts from the NMIs interact with QA These steps are crucial for infusing authority among others. professionals from the private and other to analytical results in the F&N areas and for sectors. These professionals in turn extend making sound public health decisions. 1.1 Uncertainty, Traceability and their services as requested by different sectors in the user community. Further, NMIs interact Comparability 3. Interfacing F&N Investigators with The quality assurance (QA) path outlined above, with groups from industries who request for Metrological Concepts percolates through a hierarchical pattern: specific type of QA training (e.g. metrology There is a crying need for an extended NMIs → to networks of national (or regional related to manufacturing processes, sometimes outreach by NMIs for strengthening where applicable) reference laboratories referred to as productive-metrology). However, the metrological awareness and capacity → accredited reference laboratories → it would be timely for the NMIs to support other developmental needs, in several analytical manufacturer’s standardization laboratories → disciplines that have limited opportunity to communities. I wish to single out the F&N hospital, pharmaceutical and other user-type communicate with such national laboratories. investigators who are not sufficiently exposed state and privately run (e.g. food composition to metrological concepts in their day to day and food safety) laboratories → routine service A daunting task for the NMIs is to put in place work. In fact, the word metrology is practically laboratories (officially recognized facilities functional metrological traceability systems that unknown to traditional F&N professionals. analyzing scores of samples on a daily basis). are suitable for numerous user groups. Taking the example of the food and nutrition (F&N) Therefore, getting to know metrology for daily applications assumes a life-changing situation The processes that take place at different community, the implication of this effort is as for them, with all the apprehensions that go parts of this hierarchical system are governed significant as a movement taking place at the with such thinking. by two components: (i) taking the example population level. If successful, it precipitates of chemical metrology, one that reflects an substantial changes at the grass root level, For a long time, the measurement philosophy increasing uncertainty level from step to step, as a result of improved awareness in this of a typical F&N investigator has been to apply i.e. → a well defined reference measurement segment of the analytical community. Infusing a single chosen method for analyzing two or system traceable to SI Units (e.g. definitive such a new culture into the overall thinking more sets of different samples and evaluate measurements), → reference measurement process of the F&N analytical community is a

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the differences (between them), if any, based chemical metrology. Several other physiological (25% - 30%) of health-related measurements on the measurement results. This line of measurements are carried out under complex is performed for non-diagnostic reasons thinking is open for the following deficiencies: conditions and are frequently assessed by (re-tests, error prevention and detection). (i) suitability of the chosen technique; (ii) indirect means. These include, among others, Even modest improvements in measurement sensitivity of the chosen method (which measurements for body composition and accuracy and QA will result in multi-billion can greatly influence the cost and even the dietary energy intake and energy expenditure dollar savings in healthcare costs. Project planning of an investigation); (iii) failure by traditional methods (e.g. balance technique drivers are, therefore, measurement reliability to validate the method against a certified for intake and out-flow) that lack evidence of (as it impacts healthcare costs and medical reference material or comparing the results a proven traceability link. These deficiencies decision-making), regulatory requirements, obtained by another independent method to are amenable for metrological improvements and international trade and competitiveness- identify the sources of errors; (iv) impact of not using stable isotope techniques based on related issues [6]. using direct (definitive methods) vs indirect single or double-labeled water and utilizing methods (e.g. skin-fold thickness to assay mass spectrometry for ratio measurements. Economic impact of food safety is two fold: body fat) that lack traceability aspects; and, However, it should be noted that even with (i) intrinsic confidence in the safety of the (v) doubtful qualification of studies pooled for stable isotopic investigations, systematic food as a commodity and the resulting trade meta-analysis (meta-analysis assumes that the studies designed to examine the metrological benefits in the international market; and (ii) studies chosen are compatible in all respects aspects to estimate uncertainties are lacking. the health safety related to consumption of including analytical accuracy and precision, With increased attention being focused on such foods. The food safety issue has become a and method validation). Also, it is important obesity and associated chronic disorders, there global concern and demonstrates the need for to note that outcomes of prescriptive type of is a need to strengthen the validity of these concerted efforts to integrate the metrological methods (e.g. based on the AOAC philosophy) types of measurements. concepts into the measurement processes. may be dependent on the analyst, and It should be noted that in some parts of the therefore, independently validated methods 5. Economic Impact of Quality world, movement of foods has assumed the should be used [5]. The latter practice would Assurance status of borderless-trade; foods in many enable a realistic assessment of uncertainties The statement by the Commission of the forms as commodities cross national borders associated with a given measurement process European Union in 2006 “There is no science on a daily basis. Reliable F&N measurement is and make the results more meaningful and without measurements, no quality without indispensable here. therefore, reliable. testing, and no global markets without standards” aptly summarizes the impact of 6. Capacity Developmental Issues 4. Status of F&N Measurements QA on measurements and economy. This Integration of metrology into F&N The food and nutritional (F&N) measurements sentiment is further accentuated in the trade measurements strengthens the very base represent a combination of physical, chemical circles as reflected by the notion that analytical of nutrition education, a nearly forgotten and biological metrology: quantity, density chemistry is the language of commerce. The agenda in our current academic practices. An and size (physical metrology), composition and Australian NMI website (www.measurement. observation by de Bievre [7] is appropriate in speciation (chemical metrology), and energy gov.au) states that the NMI adds value to that this context: “Unfortunately, in many parts metabolism and bioavailability (biological country’s economy by providing a reliable of the world, teaching such basics of the metrology). Certain clinical (e.g. cholesterol foundation for measurements, thus providing process called measurement is almost absent and glucose in blood) and a few others (e.g. certainty to measurements used in legal in the educational system”. The International enzymes, hair and urinalysis) overlap with transactions and in trade. The added value of Food Policy Research Institute [8], World chemical metrology. Similarly, in-vitro assays measurement in a developed economy has Bank [9,10] and a few other United Nations for body composition, bone density and been estimated to account for between 3% and Agencies are now embarking on human nutrient intake and excretion closely resemble 6% of GDP. Even the lower figure of 3% would capacity building as a critical focal point in the chemical measurements (e.g. traditional translate into about $15 billion in the Australian context of national development. The United methods), while in-vivo approaches (e.g. economy. This added value is underpinned Nations Standing Committee on Nutrition, the isotopic techniques) fall under physiological or by the NMI activities in the form of advice, International Union of Nutritional Sciences, metabolic measurements. assistance, training and transfer of technology the International Atomic Energy Agency, to industry and the science community. the World Health Organization, and the Further, measurements carried out to assess Food and Agricultural Organization among the impact of foods (e.g. cholesterol and The NIST (USA) website documents that several other organizations, have supported glucose levels in blood) and certain types of measurements are responsible for 10% - 15% capacity development efforts through task bio-analytical measurements (e.g. enzymes, of the $1.7 trillion annual costs of healthcare force deliberations, co-ordinated research hair and urinalysis) overlap closely with in the United States. A significant portion projects [11], development of internationally

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applicable quality systems and training courses education. However, the leadership here rests Measurements, Extended Abstracts, ISBN [12-15]. However, these efforts are just drops on the dynamism of the academic community. 978-963-9319-83-7, IMEKO, Hungary, pp. 68- in a bucket since the need for revamping the 69, 2008 capacity developmental issue is global, and The purpose is to disseminate the benefits [6] S.A. Wise et al., NIST contributions only national initiatives can bring sustainable of integrating metrological concepts into the to strengthen food and nutrition progress in QA and developments at the level daily laboratory work carried out by the F&N measurements, Ref, 5, pp. 88-92, 2008 it is needed. professionals. Universities on their part should [7] P. de Bievre, Traceability and comparability strive to teach metrology to analytical chemistry of results in food measurements, Ref. 1, 7. Resources for Enhancing students, at least at the graduate level. This is pp. 521-522, 2004 part of the capacity development drive that Metrological Awareness Programs [8] S. Gillespie, Strengthening capacity to carries long-term benefits. Generally, the NMIs are adequately funded improve nutrition, FCND paper 106, IFPRI, Washington D.C., pp. 1-102, 2001 because of their exceptional importance The NMIs have an indispensable role in to the national development programs. In [9] Repositioning nutrition as central to disseminating the QA message. In the national development: Strategy for large-scale action. contrast, the F&N community that stems from context, the NMIs are the torch-bearing the academic circles, is often dependent on World Bank Report, Washington D.C. 2006 leaders expected to proactively interact with [10] R.Haver, Strengthening country project funding for any additional activities. It various groups such as the F&N community, is here, that the extended outreach by the commitment to human development for preserving the integrity of the quality of lessons from nutrition, World Bank, NMIs would be most useful since they have the measurements. institutional capacity to design and teach basic Washington D.C. 2005 [11] G.V. Iyengar and R.M. Parr, IAEA’s metrological concepts to young investigators Building a sound metrological base for F&N and from universities and F&N institutions. contributions to advances in nutritional health-care measurements is a movement by and environmental metrology, Accred. This would be a long-term investment in itself, and requires a sound policy (facilitating the country’s quest for excellence in QA. Qual. Assur., Vol. 10, pp. 393–402, 2005. capacity development) to attain sustainable QA [12] FAO, (/http://www.fao.org/infoods/ The NMIs should note that this process is at the national level. This is a shared responsibility not merely a small change in the currently data2_en.stm), Rome, 2004 between the academic community, policy makers [13] B. Burlingame, Measuring nutrients in existing perceptions (or practices) in the F&N and leaders of NMIs. community. It is essential for introducing foods: the importance of international standards and the needs of diverse user sustainable approaches for preserving quality The hardball question for the academic groups, Ref, 5, pp. 70-72, 2008 systems (16). community, NMI leaders and policy makers [14] I. Castanheira and P. Finglas, Implementing is, – are they ready to take up this timely quality systems and metrological Among the food industry professionals, challenge? mobilizing funding may not be critical but principles in food composition data bases in Europe, Ref, 5, pp. 93-95, 2008 the metrological needs are numerous and References [15] G.V. Iyengar, Food and nutritional rather specific, since each product has its own [1] R. Kaarls, The CCQM and comparability measurements: capacity developmental profile. Hence, there may be understandable and traceability in food analysis, Accred. issues, Ref, 5, pp. 65-67, 2008 limitations as to what extent the NMIs can help Qual. Assur., Vol. 9, pp. 530-532 [16] G.V. Iyengar, Applied metrology for in such situations. [2] G.V. Iyengar, Editorial: Metrological concepts strengthening food and nutritional for enhancing the reliability of food and measurements: ways, means and 8. Conclusions nutritional measurements, J. Food Comp. outcomes, Invited Lecture at the F&N metrology is an emerging discipline Anal., Vol. 20, No. 6, pp. 449-450, 2007 International Conference of Nutrition, and it should be embedded as a culture in the [3] G.V. Iyengar, Presampling factors in the Bangkok, Thailand. Annals of Nutrition minds of our young analytical chemists aspiring elemental composition of biological systems, and Metabolism, Vol. 55 (supplement), to become F&N investigators. Anal. Chem., Vol. 54, pp. 554A-558A, 1982 pp. 626, 2009 [4] G.V. Iyengar, Autopsy sampling and

Integration of metrology into F&N elemental analysis: Errors arising from measurements is helpful also for improving the post-mortem changes, J. Path., Vol. 134, measurement infrastructure of an institution. pp. 173-180, 1981 Educating the future F&N investigators [5] W.R. Wolf, Reference materials for food Prof. Venkatesh Iyengar with knowledge of metrology is pivotal for and nutrition metrology: past present and Tufts University strengthening the very base of nutrition future”, International Conf. on Metrology Biomineral Sciences International of Environment, Food and Nutritional USA

38 / CITAC NEWS ● FEBRUARY 2010 DDiscussioni s c u s s i o n PPapersa p e r s Simple Basic Principles for Chemical Measurement: Identifying and Counting

There should be renewed attention for establish that matter had a “particulate” measured by the performance of two operations counting as form of measurement such as in structure. Hence it was exceedingly logical (identification and counting), the results of microbiology or when counting “active sites” – and exceedingly simple – to arrive at an which may be communicated with two items on protein molecules where measurements appropriate unit for counting a number of of information (their name and the number and their results should not be described in particles (generic name: entities): one entity. A of entities). We distinguish nominal, ordinal, terms of the quantity ‘mass’ and its units – be fixed (because defined) multiple of the natural interval and ratio scales of measurement it kg or g or mg – but in ‘number of things’ unit “one entity” can then be established and and apply these to counting, referring to with ‘one thing’ as a unit. Thus it is a good time given a name: one mole (symbol mol). The fact ordinal and cardinal numbers and Helmholtz’ to remind ourselves of the “particulate” or that a mole of entities is a very large number analysis of measurement. Counting may be “granular” structure of matter with the ensuing of entities, does not constitute a problem since by direct serial numeration, direct parallel usefulness and ensuing desirability of – indeed we can replace counting of very large number numeration, or comparative numeration. We – counting of particles: atoms, molecules, ions, by measuring ratios of very large numbers. It discuss the limitations of serial numeration, microbes, active sites i.e. “entities”. reduces the problem of measuring very large the possibilities of parallel numeration, and the ratios back to simple ratio numbers. That is advantages of comparative numeration where On the macroscopic scale that must surely what we do in a titration. The zero point tells a unit for counting in multiples (such as the have been the earliest – and easiest – form of us when a large but unknown number of ions analyst’s mole) may be used to define a scale measurement: counting cattle, soldiers, horses, is equal to a large but known number of other on which equal numbers of objects correspond apples, or coconuts, which determined the ions, yielding the simplest ratio number of all: to equal values of some other physical quantity. degree of richness or power. A more modern 1 (1:1). In isotope dilution mass spectrometry We conclude that the numeration of very large application of counting occurs in banks daily IDMS, we do something similar: we compare numbers of objects is readily achieved but with and on a massive scale: counting currency a large but unknown number of atoms of one unavoidable uncertainty, using operations units. Also, in a set of persons, it makes more isotope of an element to a known number of which compare numbers of entities either to sense to think of an average height per person atoms of another isotope of the same element numbers of other entities or to some other (unit for measuring a number of persons: (called a “spike”). In this case we also have an quantity which accurately models numbers of one person) rather than of an average height “equivalence point” indicator of equality of entities.” per mass of person (unit for measuring mass large numbers: we have even measurement of persons: one kg of person). Similarly, it is instrumentation which is reasonably linear Comments can be sent to the author, to the more useful to talk about an average salary enabling us to measure ratios of large numbers editor of the CITAC Newsletter, or to the per person (unit for measuring a number of (of isotopic atoms) when the “equivalence Discussion Forum of ACQUAL. persons: one person) rather than of an average point” is different from a number ratio 1. It can salary per mass of person (unit for measuring even differ from that number ratio 1 by several mass of persons: one kg of person). orders of magnitude e.g. 10-2 (1/99) and still be References measured easily. Thus, ‘numerosity’ or ‘numerousness’ is a very [1] G Price and P De Bièvre, Simple principles basic property of matter and an extremely The fundamental thinking touched above for metrology in chemistry: identifying and useful tool to measure a “number of things”. is underpinned in [1], the abstract of which counting, Accred Qual Assur 14(2009)295- It took a long time before that was recognized. follows hereafter: 305 For centuries, matter was looked upon as “We examine the problem of quantitative something being “continuous”. Although chemical measurement for well-identified Demokritos in ancient Hellas implied already substances, discuss the quantity called ‘amount Prof. Paul De Bièvre the “particulate” nature of matter, it took of substance’, the means of expressing it, and Independent Consultant on Dalton, Berzelius, Lavoisier and others, almost its physical SI unit the mole. The everyday Metrology in Chemistry two thousand years later, to definitively quantity which is a number of entities may be Belgium

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V METROCHEM - Brazil

The Brazilian analytical community Fifty posters presented were also witnessed the successful realization focused on topics such as method of the “V METROCHEM - International and procedure validation, uncertainty Congress on Traceability in Laboratory in measurements, calibration, Measurements and Productive Chains”, accreditation and formal recognition, 11 to 13 November 2009 in São Paulo, reference materials – production and Brazil. São Paulo, South America’s use, and interlaboratory comparison largest city, with a population of 20 programs/proficiency testing, million people and a GNP of about 500 laboratory techniques and analytical billion U.S. dollars, is also Brazil’s most methods. industrialized center. The realization of the Congress in this city benefited The Conference opened with several a wide range of industrial sectors musical selections from the University and their customers, regulators of São Paulo Choral Group. This was and suppliers, as well as academic Fig. 1. Dr. Willie May delivers to Dr. Robert Kaarls a followed by an Awards Session where institutions and government. Certificate of Recognition of Professional Excellence: "Man's Drs Robert Kaarls, José Carlos de Castro mind, once stretched by a new idea, never regains its Waeny and Vera Maria Lopes Ponçano The primary focus areas of the Congress original dimensions" received Certificates of Recognitions were: (i) metrological traceability of Professional Excellence in their for laboratory measurements with organizations, exporters, research and respective fields. emphasis on reference methods, certified development institutions and universities. reference materials, and methods and protocols Focusing on the participation of CITAC for providing reliable laboratory results that The main themes of the forty two oral members and associated international can be compared over both time and space, presentations were: metrological traceability, organizations, the Congress started with the and (ii) traceability of the production chain, product technical specifications and presentation of Dr. Robert Kaarls (CCQM focusing on the food, beverage, fishing and regulations, food and safety chain, wood chain President), who highlighted the impact of chemical industries. of custody, hazard analysis and critical control metrology in the global economy and the points, quality in laboratory measurements, demands of metrological traceability in brand The Congress was co-sponsored by the calibration hierarchy, VIM, technical translation, new scientific areas. Then Dr. Willie May (NIST- Metrology Network of São Paulo State traceability related to analytical equipment, USA) called the audience’s attention on the (REMESP), the Instituto de Pesquisas traceability in industrial gases, meat and fishery impact of chemical metrology on the industrial Energéticas e Nucleares (IPEN-SP) and the chain, certified reference materials production competitiveness and quality of life. Finally, Dr. Cooperation on International Traceability in and consumer protection, among others. Ilya Kuselman (INPL-Israel) described the role Analytical Chemistry (CITAC). The of CITAC in developing metrological event was attended by more than one traceability worldwide. hundred and fifty professionals eager to update their technical knowledge, In a very conceptual and therefore including fifty metrology experts from dense session, Prof. Paul De around the world. Bièvre explained how the concept of metrological traceability of The interaction between invited experts measurement results must be and congress participants provided implemented in chemistry. This talk a positive contribution to higher allowed several Brazilian experts learning institutions, industry, service to describe their experiences organizations and exporters. the target in establishing metrological audience was composed of participants traceability in fields like agriculture, from the technical and managerial staff biological materials, clinical analysis, of testing and calibration laboratories, environmental monitoring, minerals clinical laboratories, regulatory Fig. 2. Prof. Paul De Bièvre, Dr. Ilya Kuselman and Prof. and metals, pharmaceuticals, gas and agencies, certification and quality Maria Filomena Camoes during a coffee break oil.

40 / CITAC NEWS ● FEBRUARY 2010 MMeetinge e t i n g RReportse p o r t s

The metrological system management session Education and training was deemed essential this event, where traceability under different was a very important one. Dr. Maria Fernandes for disseminating knowledge in metrology in perspectives were the key words. Whaley (NMISA-South Africa) presented the a thorough and consistent way. Following this example of AFRIMET in the African context route, Dr. Philip Taylor shared his experience The final activity was an award session which was connected with some Brazilian with the very successful European platforms recognizing the five best papers presented presentations on how traceability was TraiNmiC and MSC Euromaster. Then, according to the rules established by the implemented in practice for food and feed Brazilian professors from public and private scientific committee. The event finished with products in Brazil. The highlight was the universities reported their experiences in the an open evaluation session that led to several lecture of Dr. Nineta Majcen (NMI-Slovenia), implementation of metrology in chemistry into interesting suggestions promising to continue who described the strategy for building a the university’s curriculum. the friendly scientific atmosphere we all distributed metrology infrastructure to face her experienced in São Paulo. country’s most pressing demands. The presentations related to productivity chain traceability were the occasion to verify how Another interesting topic was the new VIM. the Brazilian meat, fish, poultry and wood Although it is now largely accepted as the official industries are organizing their quality control technical language in metrology, problems systems to demonstrate to the consumer Dr. Marina Beatriz Vasconcelos Agostini of translation to Portuguese were raised by the traceability from farm to fork. This topic Dr. Olívio Pereira de Oliveira Júnior Prof. Maria Filomena Camões, Universidade is highly important for Brazil because the Scientific Committee Presidents, IPEN de Lisboa. After a cheerful discussion it was country is of the world’s largest commodities concluded that metrological concepts must be producer. Dr. Vera Maria Lopes Ponçano thoroughly understood before the translation The presence and active participation of CITAC Congress President, REMESP work actually start. members and colleagues added real value to Brazil

ISRANALYTICA 2010 and the CITAC Workshop in Israel

The Conference participated in the conference and exhibition, mass spectrometry, pharmaceutical analysis, bridging between technology developments proteomics and bioanalysis, water and ISRANALYTICA 2010, the 13rd Annual Meeting and end users. In fact, ISRANALYTICA combines environmental analysis, separation methods, of the Israel Analytical Chemistry Society and the largest chemistry convention in Israel with nano-analytics, analytical spectroscopy. On the accompanying Exhibition took place the largest analytical chemistry exhibition in the second day metabolomics and bioanalysis, according to tradition, January 19-20, 2010, one location. forensic and legal analysis, electrochemistry at the David Intercontinental Hotel, Tel-Aviv, and spectroscopy applications, food analysis, Israel. ISRANALYTICA has been recognized by the metrology and quality, education and Analytical Chemistry Division of the European intellectual properties were the session The annual meetings of the Israel Analytical Association for Chemical and Molecular topics. Distributions of the lecturers and Chemical Society have become one of the Sciences (DAC EuCheMS), the International poster presenters by economies are shown in largest annual conferences in analytical Society of Electrochemistry (ISE), and the Fig.1 and Fig. 2, respectively. However, the chemistry in the World. About 3000 participants Cooperation for International Traceability in problem was that only about 25% of the 3000 from academia, the pharmaceutical and Analytical Chemistry (CITAC). participants were attracted by the lectures and chemical industries, petrochemistry and food posters, while the others were busy at the industry, biochemistry and biology, water The scientific program consisted of 4 plenary exhibition. The Organizing Committee will experts, engineers, quality managers and lectures and 14 keynote lectures delivered by study this phenomenon to decide what can be metrologists from major laboratories and international top scientists, oral presentations improved. companies from Israel and about 20 other (in 14 parallel sessions) of featuring speakers countries attended. As well, about 60 leading from Israel and abroad, and a poster session. Three prestigious poster awards were granted analytical equipment companies successfully On the first day there were sessions on by the Conference Organizing Committee

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to the outstanding posters during ● “A practical guide to chemical the general assembly of the Israel metrology and pharmaceutical Analytical Chemistry Society. quality” by Dr. William Koch, USP, USA. In Fig. 3 and Fig. 4 one can see two pictures from the Isranalytica 2010. Every lecture was planned for 45 min, Hundreds of other pictures are while the next 15 minutes were used available in http://www.isranalytica. for questions and discussions. org.il/Isranalytica2010/Gallery. It was an exciting, very fruitful meeting. This workshop was intended for: ● Laboratory personnel in analytical The CITAC Workshop (quality control) and R&D A CITAC one-day workshop was laboratories; presented on 21 January 2010 as a Fig. 1. Lecturer distribution by economies ● Quality assurance personnel post conference event titled “What involved in reviewing analytical should you know about metrology data and validation studies; & quality requirements to analytical ● Projects coordinators and results?” The workshop program analytical laboratory managers; included the following lectures: ● Metrologists specialized in chemistry. ● “Introduction to metrology and quality in chemistry” by Dr. Ilya Since the lecturers were already Kuselman, INPL, Israel; familiar to the audience from the conference, the interactions ● “Different approaches to estimation of measurement between them were simple, helpful uncertainty in analytical and creative. The workshop chemistry” by Prof. Ivo Leito, participants were very satisfied by Fig. 2. Distribution of poster presenters by economies University of Tartu, Estonia; the possibility to learn, ask and receive answers directly from the leading ● “Exploiting the potential implementation” by Prof. Paul De Bievre, specialists in metrology in chemistry – the of reference materials and accompanying Consultant, Belgium; CITAC members. information by different laboratories” by ● “Metrological traceability in analytical Prof. Hendrik Emons, IRMM, European spectrophotometric instrument Dr. Ilya Kuselman Union; qualification” by Dr. Jerry D. Messman, INPL ● “Metrological traceability of measurement Stranaska Scientific LLC, USA; and results in chemistry: concepts and Israel

Fig. 3. Prof. Hendrik Emons delivers his plenary lecture Fig. 4. Dr. William Koch (from the left) and Dr. Raphy Bar in “Towards the “chemical kilogram”: development and use the special session on US Pharmacopeia and USP reference of references for chemical and bioanalysis” standards

42 / CITAC NEWS ● FEBRUARY 2010 MMeetinge e t i n g RReportse p o r t s

14th International Metrology Congress 22-25 June 2009 - Paris: A Glimmer of Hope Before Summer!

The color of the fitted carpet in stands was Conference Poster Prize awarded to Mrs. The organization committee also had some orange, which was a good sign! The general Goyon of BIPM, tough challenges to face this year, including impression and the first reactions expressed by ● Business sessions providing live discussions keeping registration fees unchanged (at the participants were also very positive. As one of in the conference room between service 2007 price level), which involved making some them put it: “It was a glimmer of hope in the providers, manufacturers and participants, difficult decisions in organizational matters. current gloomy outlook!” ● Lunches in the form of a standing buffet But it showed real maturity and management allowed easy interaction and discussion skill, building on experience with previous 750 participants registered for full access to the among participants, although some were a events. In fact, its goal was to make the event event, a 15% increase over previous congress’ bit nostalgic for the classic sitting format! available to the widest audience, in spite of the attendance! 200 additional non-registered ● Thursday’s event was very much current budget restrictions prevailing in most participants visited the exhibition. 30% of the appreciated, and exhibitors stayed until companies. participants were foreigners from 48 different the end and attended the 4.00 pm closing countries, mainly European, but also from party. The International Metrology Congress is now North and South America, Africa, the Middle held in high esteem by our European partners. East and Asia (Fig. 1). For the first time, we may also have found the Many prospects and opportunities for new proper balance in contents. Indeed, at closing developments are now open, both in France The Congress proved to be of great interest to time, “scientists” said they had found this and abroad. those participating: event too “industrial”; and on the other hand, ● 59% among them were industrial: “manufacturers” said that the event was too The Collège Français de Métrologie, as the main measurement tools users of all sectors, “science” oriented! In regard to the selection of operator, is aware of the high expectations analysis laboratories, metrology topics discussed, generally participants found such an event has raised, and will spend the laboratories or materials manufacturers ... that the Program was quite exhaustive, varied needed time and effort to study such new ● 26% were from big national and and “very attractive”, although some topics opportunities. A warm thank you to all the international institutions: national were missing – as is inevitably the case! organizations and partners for supporting the laboratories of European countries, Congress: Government Officials, accreditation institutions, international organizations... ● The Organization Committee members: ● 10% were from the university or research Acac, BEA Metrologie, BIPM, CETIAT, fields, CETIM, EA, EURAMET, EUROCOPTER- ● 5% from other sectors (hospitals, training Group EADS, IMQ, INSA of Lyon, LNE, NPL, organization, free lance, press..) OIML and RENAULT, ● The Premium Sponsors: Stork Intermes This year, the Congress offered many new and Hexagon Metrology, features, including: ● The Technical Partners: Endress & Hauser ● 6 round tables running over the full and Trescal, course of the congress with current hot ● The Institutions: the French Ministry for topics discussed in the field of business Industry, Economy and Finance, the French management, environmental and health Ministry for Culture and the Ile-de-France issues, and future prospects for wireless Region. equipment, ● Best Conference Prize awarded to Ms. Sandrine Gazal Mr. Lübbehüsen of GE Sensing and Best Fig. 1. Bag "Métrologie" of a participant Collège Français de Métrologie, France

● 43 / CITAC NEWS ● FEBRUARY 2008 CITAC NEWS FEBRUARY 2010 / 43 AAnnouncementsn n o u n c e m e n t s International Summer School Euromaster Measurement Science in Chemistry 18 July-2 August 2010, Tartu, Estonia

Measurement Science in Chemistry For 2010, a limited number of places are (MSC) Euromaster is a consortium of 9 available to persons who are not enrolled at European universities that conduct a Master’s one of these universities. They will be able to Degree Program offering education in the participate in all learning activities, including measurement science which is needed to follow-up assignments and learning evaluation obtain reliable results for chemical and bio- and will obtain a certificate of attendance. analytical measurements. The consortium The minimum requirement for enrolment is was awarded the ECTNA (European a bachelor’s degree in chemistry. Chemistry Thematic Network Association) Euromaster® quality label in 2008, Fig. 1. Practicalities See http://www.msc-euromaster.eu/ for The summer school will take place at the more info. University of Tartu, Estonia. The fee for the Fig. 1. Awarding Ceremony of the The Euromaster® summer school is €1900, which includes label to the MSC concortium EUROMASTER Summer Schools full board accommodation for the entire An important activity of the MSC is the period, all teaching materials and certificate. common social activity. Students get follow- summer school – intensive training course Details of the event will become available up assignments and their learning is evaluated of the advanced topics of measurement at the consortium website http://www.msc- afterwards by scoring and by description of science (metrology) in chemistry: validation euromaster.eu/ their strong and weak points. Summer schools of chemical analysis procedures, traceability have been organized in 2008 (Celje, Slovenia) in chemistry, statistics and statistical basis of and 2009 (Blagoevgrad, Bulgaria). How to Register calibration, quantification of measurement Contact Prof. Ivo Leito (e-mail: ivo.leito@ut. uncertainty, ISO 17025 quality systems and The next summer school will take place from ee; phone: +372-5 184 176), coordinator laboratory assessment and sampling and 18 July to 2 August 2010 in Tartu (Estonia). of the EUROMASTER MSC sending a letter sample preparation. of motivation, including a CV stating your educational qualifications. The volume of the summer school is 30 ECTS Who can participate? points and the teaching methods range from The summer schools are attended by master classical lectures to case studies and role students of the MSC consortium partner Prof. Ivo Leito playing. The summer school is conducted universities. University of Tartu during two weeks, with a one day break of Estonia

Teaching Analytical Chemistry at the Beginning of the 21st Century 8-10 September 2010, Radovljica, Slovenia In a time period when those teaching at and self-learning. They will present their university are under pressure to excel various teaching approaches and share their in their research, search for funding and successes and problems. This will be done perform a multitude of administrative tasks, via a series of lectures, poster sessions and there is often too little time left to face focused discussion groups. This workshop the challenge of how to best teach today’s aims at providing you with some ideas to try students, who are quite different from those out at home. of the previous decade. This conference is organized by the joint This multi-disciplinary conference brings consortium of Euromaster Measurement together people from all across the world Science in Chemistry (www.euromaster- interested in finding effective and novel msc.eu), which is a master’s degree program ways of teaching analytical sciences so as to jointly delivered by a group of 9 European attract students and teach in a more effective universities. This conference takes place 5 Fig. 1. The Southern Alps and up to date format, stressing interactivity years after the first summer school for analytical

44 / CITAC NEWS ● FEBRUARY 2010 AAnnouncementsn n o u n c e m e n t s

chemistry lecturers which was held in Rogaška Registration fee: €300, which includes an ice- Ph. Taylor (Institute Reference Materials and Slatina (Slovenia), and which led to the Rogaška breaker, coffee breaks, conference dinner, Measurements, JRC, European Commission), Declaration (http://dx.doi.org/10.1007/s00216- conference materials and a visit to a local 006-0548-5). industrial archaeology site. How to Register Contact: [email protected] Contact [email protected] to receive Venue Accommodation: www.radovljica.si further information and be updated on the Radovljica is a medieval market town in event. Registration will be set up at www.msc- Slovenia, about 25 km from Ljubljana airport, Organising Committee euromaster.eu in due course. and is surrounded by the magnificent scenery M. Islamčević Razboršek, M. Kolar, N. Majcen, D. of the Southern Alps (Fig. 1). Brodnjak-Voncina (University of Maribor, Slovenia)

Practical Info Scientific Committee Prof. Ivo Leito 8-10 September 2010 in the Radovljica Mansion E. Bulska (University of Warsaw, Poland), J. University of Tartu Randon (University Claude Bernard Lyon 1), Estonia

International Symposium “The Future of Reference Materials – Science and Innovation” 23-25 November 2010, Geel, Belgium

The Institute for Reference Materials and Measurements (IRMM) of the European Commission’s Joint Research Centre is organizing this scientific symposium within the frame of the IRMM 50th anniversary. The symposium aims at mapping out the current and upcoming measurement and testing needs for which challenging demands on reference materials are envisaged. Forward-looking contributions are invited on the scientific and technological demands and developments for the design, preparation and certification of such measurement standards for: • clinical/laboratory medicine • biotechnology/molecular biology • pathogens/microbiology Important dates Further information • food safety http://irmm.jrc.ec.europa.eu/future-rm • nutrition 30 June 2010 Deadline for abstracts • environment 15 September 2010 Confirmation for selected E-mail: • calibration and purity presentations [email protected] assessment in chemical analysis 30 September 2010 Second announcement • nanotechnologies 22 October 2010 Deadline for registration Prof. Hendrik Emons • nuclear safeguards EC-JRC-IRMM 23-25 November 2010 Symposium • material science Belgium

● 45 / CITAC NEWS ● FEBRUARY 2008 CITAC NEWS FEBRUARY 2010 / 45 AAnnouncementsn n o u n c e m e n t s 7th Workshop on Proficiency Testing in Analytical Chemistry, Microbiology and Laboratory Medicine 3-6 October 2011, Istanbul, Turkey

The EURACHEM Proficiency Testing Working Social & Cultural Program Group (www.eurachem.org), in cooperation Social events which reflect the rich and with CITAC (www.citac.cc) and EQALM diverse culture of Turkey will be provided (www.eqalm.org), is organizing the 7th event for workshop delegates and accompanying of a series of workshops addressing current persons. A welcome cocktail party and practice and future directions of proficiency workshop dinner will be organized. Daily testing (PT) and external quality assessment trips to local tourist sites of Istanbul during (EQA) in analytical chemistry, microbiology the workshop are being planned for and laboratory medicine. accompanying persons.

Venue Registration The workshop will be held in Istanbul, 2010 Fig. 1. Maiden's Tower The first circular, registration and hotel European capital of culture and a historic city booking forms will shortly be available where east meets west (Fig. 1). The month of October is a pleasant time of the year to presentations, discussions in working groups Workshop Secretariat enjoy scenery and historic sites, some of which and poster sessions, to enable interactive Phone: +90 312 210 4889 date back 8000 years. There are good airline participation and cross-fertilization of ideas. Fax: +90 312 210 5668 connections from most major international Two training sessions will precede the Website: www.labkar.org.tr/EURACHEM2011 cities to Atatürk Airport, in the European side Workshop. of the city. There is also a second international airport, Sabiha Gökçen Airport, which is in the Dr. Ender Okandan Chair of Local Organising Committee Anatolian side of Istanbul. The workshop will Who Should Attend? be held in the Polat Renaissance Hotel, close to Petroleum Research Centre, Ankara The Workshop will provide an excellent Turkey Atatürk Airport (www.polatrenaissance.com). opportunity for PT/EQA scheme organizers and end-users of PT/EQA (laboratories, Dr. Brian Brookman Technical Program accreditation bodies, regulators and the Chair of Scientific Committee The workshop will be structured to include laboratories’ customers) to come together and LGC Standards Proficiency Testing, Bury keynote lectures along with a number of short share their views. UK

Visit CITAC Website: www.citac.cc

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46 / CITAC NEWS ● FEBRUARY 2010 CCITACI T A C MMembers’e m b e r s ’ LListi s t

Dr Celia Puglisi Prof Dr Hendrik Emons Prof Ivo Leito INTI Institute for Reference Materials and University of Tartu CC 157, San Martin Measurements (IRMM) Institute of Chemistry Buenos Aires (1650) Joint Research Centre European Commission 14a Ravila Str. ARGENTINA Retieseweg 111 Tartu 50411 Tel + 54 11 4754 5151 2440 Geel ESTONIA Fax + 54 11 4713 5311 BELGIUM Tel +372-518-4176 Email [email protected] Tel + 32 14 571 722 Email [email protected] Fax + 32 14 571 548 Email [email protected] Prof Timo Hirvi Dr Laurie Besley Center for Metrology and Accreditation National Metrology Institute Dr Olívio Pereira de Oliveira Junior P.O. Box 9 1 Suakin Street Instituto de Pesquisas Energeticas e Nucleares FL-02151 Espoo Pymble NSW 2073 (IPEN) FINLAND AUSTRALIA Av. Lineu Prestes 2242, Cidade Universitaria Tel + 358 9 616 74 50 Tel + 61 2 9449 0159 05508-000 Sao Paulo – SP Fax + 358 9 616 74 67 Fax + 61 2 9983 1398 BRAZIL Email timo.hirvi@mikes.fi Email [email protected] Tel + 55 11 3817 7180 Fax + 55 11 3814 4695 Dr Philippe Charlet (CITAC Secretary) Email [email protected] Laboratoire National de Métrologie et d`Essais Mr Alan Squirrell (LNE) ILAC Secretariat Dr Vera Ponçano (CITAC Past-Chair) 29, avenue Roger Hennequin 7 Leeds Street Technical Director of the Metrology Network 78197 Trappes Cedex Rhodes, NSW 2138 of Sao Paulo State (REMESP) FRANCE AUSTRALIA Rua Padre Olavo Pereira da Silva, 28 Tel + 33 1 30 69 21 95 Tel + 61 2 9736 8374 Cid. Sao Francisco Fax + 33 1 30 69 12 34 Fax + 61 2 9736 8373 São Paulo - SP Email [email protected] Email [email protected] CEP: 05353 100 BRAZIL Dr Ioannis Papadakis Tel + 55 11 8458 3715 Consultant Dr Ales Fajgelj Fax + 55 11 3283 1073 Megistis 25 International Atomic Energy Agency Email [email protected] 17455 Alimos, Athens Wagramer Strasse 5, P.O. Box 100 GREECE A-1400 Vienna Mrs Gabriela Massiff Tel + 30 6977 190905 AUSTRIA Fundación Chile Fax + 30 2107 212909 Tel + 43 1 2600 28233 Av. El Condor 844, Ciudad Empresarial Email [email protected] Fax + 43 1 2600 28222 Huechuraba, Santiago Email [email protected] CHILE Dr Tai Lun Ting Tel + 56 2 242 8180 Government Laboratory Fax + 56 2 242 8182 7/F Ho Man Tin Government Offices Prof Dr Wolfhard Wegscheider Email [email protected] 88 Chung Hau Street, Kowloon (CITAC Treasurer) HONG KONG, CHINA Dept. of General & Analytical Chemistry Prof Yu Yadong Tel + 852 2 762 3701 University of Leoben National Research Centre for CRMs Fax + 852 2 714 4083 Franz-Josef Strasse 18 18, Bei San Huan Dong Lu, Chaoyangqu Email [email protected] A-8700 Leoben 100013 Beijing AUSTRIA CHINA Mr Prabhat K. Gupta Tel + 43 3842 402 7000 Tel + 86 10 6427 1638 Head, Chemical Metrology Section Fax + 43 3842 402 7012 Fax + 86 10 6422 8404 National Physical Laboratory Email [email protected] Email [email protected] Dr. K.S. Krishnan Road New Delhi-110012 Prof Dr Miloslav Suchanek INDIA Prof Dr Paul De Bièvre EURACHEM-CZ Tel +91-11-45608232 Accreditation and Quality Assurance Department of Analytical Chemistry Fax +91-11-25726938 Duineneind 9 Institute of Chemical Technology (ICT) Email [email protected] B 2460 Kasterlee 166 28 Prague 6 Dr Máire Walsh BELGIUM CZECH REPUBLIC Newton, Celbridge, Co Tel + 32 14 851 338 Tel + 420 22044 3685 Kildare Fax + 32 14 853 908 Fax + 420 22044 3685 IRELAND Email [email protected] Email [email protected] Tel +353 1 6271522 Email [email protected]

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48 / CITAC NEWS ● FEBRUARY 2010