Development of Metrology of Chemical Measurements in Estonia Ivo Leito University of Tartu Estonia

May 2003 Palanga Scope of the Lecture Metrology system in General –Present –Future Metrology in Chemistry –A Recent Survey –Situation at Field Labs –Accreditation –Teaching/Training –International Collaboration

May 2003 Palanga The Metrology System in Estonia: the Current Structure The NMI National standards: Mass, Length Other: Pressure, Force, Density Temperature Electrical quantities Flow etc. Metrology council MoEAC Central Office of Metrology (Metrosert Ltd)

May 2003 Palanga Planning the Future PHARE Projects: –ES National Metrology and Accreditation Centre Aim: Strategy planning –ES Development of Conformity Assessment Infrastructure in the field of metrology Aim: Investments

May 2003 Palanga Strategy Planning Project Donor: PHARE Foreign experts: NMi VSL (Netherlands) Estonian contractor: Ministry of Economic Affairs (MoEA) Start: Jan 2002 End: Dec 2002 Initially metrology in chemistry was not included at all!

May 2003 Palanga Strategy Planning Project Extensive visits of Dutch experts Two questionnaires targeted specifically to the needs and expectations of laboratories, incl industrial Workshop at MoEA involving as many stakeholders as possible Survey: Chemical Analyses and Measurements: the Needs of Estonia

May 2003 Palanga The Main Problems Identified In several fields no traceable calibration possibility is available Status of the NMI is somewhat unclear Poor International visibility. No membership in: –Metre convention, CIPM MRA –EUROMET, Eurachem Low financing of metrology: –In Estonia % of the GDP –Average in EU 0.005% of the GDP Chemistry is split between ministries

May 2003 Palanga The Metrology System in Estonia: Planned Structure The NMI National standards: Mass, Length, Temperature Other: Pressure, Force, Density Electrical quantities Time Luminous intensity etc. MiC - Chromatography-mass- spectrometry - pH metry - Spectrophotometry Air Humidity Air Flow Velocity MiC - Atomic Spectroscopy - Ion Chromatography Surface Hardness Surface Roughness Metrology council Technical University of Tallinn University of Tartu MoEAC Central Office of Metrology (Metrosert Ltd)

May 2003 Palanga Spearheads Distributed metrology system: –Metrosert Ltd + UT + TTU = NMI Metrology system tuned to the needs of the country CIPM MRA: –membership –registration of CMC-s International and regional co-operation –EUROMET, Eurachem –Baltic collaboration

May 2003 Palanga Investments Project Donor: PHARE Foreign experts: MIKES (Finland) Estonian contractor: Ministry of Economic Affairs (MoEA) Start: May 2003 Planned End: Dec 2004 Investments: 2 MEUR –equipment for chemistry: 0.5 MEUR

May 2003 Palanga Functions of the MiC Centres at Universities Providing traceability to field labs Developing, maintaining and disseminating competence in MiC Organising/mediating interlaboratory comparison measurements Applied research tuned to the needs of the country Supporting Governmental institutions Supporting Accreditation

May 2003 Palanga Survey: Chemical Measure- ments, the Needs of Estonia There is ample general information that chemical measurements are highly important in Estonia There is a lack of specific information –about the present volumes of chemical measurements –about the present and future needs in terms of types and volumes of chemical measurements A Survey was conducted in 2002

May 2003 Palanga Survey: Results The full report (in English) is available at:

May 2003 Palanga Survey: Results, Industry Selected sectors: Food, Chemical, Water The annual number of chemical measurements in the selected sectors of industry: –performed by the enterprises: 1.5 ± 0.3 M –ordered from Estonian laboratories: ± 0.01 M –ordered from outside of Estonia: 500 ± 300

May 2003 Palanga Survey: Results The estimated annual volume of chemical measurements: the whole Estonian industry: 1.9 ± 0.6 M dedicated laboratories: 4.9 ± 1.0 M the medical sector: 5.7 ± 2.0 M

May 2003 Palanga Survey: Results The estimated total annual volume of chemical measurements in Estonia is 12.5 ± 2.3 millions

May 2003 Palanga Survey Results: Trends

May 2003 Palanga Survey Results: Types of Chemical Measurements

May 2003 Palanga Survey: Results Strong need for: –more different ILCs –more different CRMs –more training only 6% of the industry and 0% of the dedicated laboratories’ respondents indicated that the competence is sufficient –a competence centre in chemical analysis

May 2003 Palanga Survey: Results Fields of chemical measurements that are currently uncovered were identified: –Contaminants: some pesticides, veterinary drugs, dioxins,... –Food quality: selenium, dietary fibre, iodine,...

May 2003 Palanga MiC at Field Laboratories Metrological principles form the basis of every measurement –Validated measurement procedures –Measurement uncertainty –Traceability –Independent assessment of performance Their application is the responsibility of every laboratory

May 2003 Palanga MiC at Field Laboratories Validation is in general well established Measurement uncertainty –most laboratories do at least something –the quality is often insufficient Traceability –in many cases remains a mystery –most of the labs use CRM-s –price and availability are often obstacles

May 2003 Palanga Interlaboratory Comparisons Organised in Estonia: –Surface water –Ground water –Wastewater From abroad: FAPAS/FEPAS, Aquacheck, etc. IMEP There is quite a wide range of measurements for which no ILCs are available

May 2003 Palanga Accreditation of Field Laboratories Accreditation is required by a number of legislative acts (around 50) 115 testing laboratories are accredited ( ) Out of them ca 50% perform chemical measurements MiC is Important! Source:

May 2003 Palanga Accreditation of Field Laboratories Estonian Accreditation Centre has applied for the membership of the EA MLA –Preliminary assessment: March 2002 –Full assessment: March 2003 –Report on dealing with non-conformities: June 2003 –Possible acceptance to EA MLA: October 2003

May 2003 Palanga Teaching and Training University level teaching of chemistry: –University of Tartu (UT) –Tallinn Technical University (TTU)

May 2003 Palanga Teaching and Training Teaching MiC Teaching of MiC at UT started in 1999 –MiC is now well established in the curricula of chemistry and materials science students –The course at present is voluntary, with the commencement of the 3+2 scheme it becomes obligatory Teaching of MiC is also carried out at TTU

May 2003 Palanga Teaching MiC There is a dilemma: –On one hand: It is desirable to make it clear for the students from the very beginning that Metrological aspects, and MU in particular, are an integral part of any measurement, not just a fancy add-on. –On the other hand: Explaining the topics of MiC in full rigor before starting with analytical chemistry has low efficiency, because the concepts of MiC do not link to anything in the student's knowledge and will therefore be only partially understood and forgotten very quickly.

May 2003 Palanga Teaching MiC at UT: 2 Stages The First stage –The basics of MiC have now been introduced into the general analytical chemistry curriculum –Students get: the very basis in lectures (measurement, measurement results, their comparability and traceability, measurement uncertainty, the ISO method of uncertainty estimation…) practical training in laboratory classes: estimation of measurement uncertainty of real analyses performed by the students

May 2003 Palanga Teaching MiC at UT: 2 Stages The second stage: Special Course on MiC –In addition to the basics in the general analytical chemistry curriculum there is a dedicated course on MiC –Topics covered: –Metrology, measurement, measurement unit, the SI system, measurement result, measurement uncertainty, comparability and traceability of measurement results, error and uncertainty, estimation of measurement uncertainty, the ISO procedure of uncertainty estimation, other procedures, possible uncertainty sources, uncertainty components, quantifying uncertainty components, metrology in chemistry, method validation, primary methods (gravimetry, titrimetry, coulometry, isotope-dilution mass- spectrometry), reference materials, certified reference materials, interlaboratory comparisons (ILCs), types of ILCs, proficiency testing schemes (PTSs), data treatment of results of PTSs, metrology system in Estonia, the metrology act, metrology in Europe and the World, standards, ISO standards, quality, quality management, quality systems, ISO 17025, accreditation, accreditation in Estonia

May 2003 Palanga Teaching MiC at UT The “Current Status” of teaching MiC at UT has been published: Accreditation and Quality Assurance (2002) 7:

May 2003 Palanga Teaching MiC: Joint Activities of the Universities There is a preliminary agreement to join forces between UT and TTU Student Teaching Material on MiC will be published jointly

May 2003 Palanga Training University of Tartu offers training to laboratories –MiC –Experimental techniques (GC, HPLC, …), incl their MiC aspects –Practical aspects of work in laboratory –Efficient use of computers in laboratories Education is if not the most important then at least one of the most important things in this field

May 2003 Palanga International Collaboration Still limited, but getting better EUROMET EC-JRC IRMM The Baltic Countries. Plans: –joint projects and events –joint ILC-s –joint database of laboratories