Objectif
Specific Objectives
To ensure the supply of industrial CRMs (metals, physical/mechanical property CRMs, industrial raw materials) for the BCR programme, certifying both new and replacement CRMs, other samples (including accelerator targets) and administering both commercial and stock-keeping aspects of the BCR programme.
To ensure CRM stability through a continuous monitoring programme (70 CRMs).
Specific objectives for 2002 are:
- Drafting of TQM documentation according to ISO 34 ready for internal audit, including implementation of "project planning forms" for new CRMs;
- Development of ISO 35-compliant training guide for uncertainty calculations;
- Certification of CRMs BCR-692 (REMAST scratch test), IRMM-533 (Al-Ag), IRMM-
534 (Al-Sc), IRMM-521R (Ni), IRMM-540R, 541 (U-glasses);
- Certification of Charpy impact CRMs (8-10 batches), CRMs BCR-013-016, 415;
- Continuation of IRMM/NIST/NRLM Charpy inter-comparison (2 international master batch sets to be measured in 2002). Characterisation of 2 new castings of steel (5000kg in total) for Charpy production;
- Finalisation of new BCR guidelines for CRM production;
- Installation of NMR machine and certification of first batches of "plastic-in-oil" calibration sets for solid fat determinations;
- Characterisation of k0 multi-element standard. (3 types);
- Development of technical and administrative methods for taking over responsibility of BCR-CRM production from DG-RTD in the new Framework Programme.
Planned Deliverables
- Expected BCR CRMS sales (direct and via authorised distributors) of 10 000 units, value approximately 1.4M.
- TQM, ISO 35 and Guideline documentation as described above;
- Certifcation of new and replacement CRMs as described above.
Summary of deliverables made by: 31/12/2001
Certification procedures Continuous
Draft guidelines for "feasibility studies for CRMs" was prepared and discussed at BCR on 6.6.01 and the new ISO 35 philosophy is included. Discussion of BCR guideline revision took place at M&T. IRMM will work on relevant aspects (stability, packaging, labelling) and incorporate thinking from IRMM CRM "project planning". The BCR CRM review panel evaluated 9 reports. From IRMM, one was accepted 322R-325R (Zn), and 261T (Ta2O5) needs to be resubmitted. As part of the RTD study on future use of CRMs in Europe, an interactive website has been set up for users. The new draft ISO 35 (with major input by IRMM) has been discussed and accepted by ISO REMCO (Gaithersburg, USA) and should be issued in February 2002. Certification "Vademecum" has been produced, serving as a manual for administrative and technical procedures for CRM certification. Project Planning and Management Tools have been implemented and regular progress surveillance mechanism has been installed. A draft guideline on statistical principles to be applied for the proper evaluation of feasibility studies for CRMs has been developed and forwarded to DG RTD. Finally the communication channel between M&T and IRMM have been streamlined and enhanced.
Stability monitoring of BCR CRMs DG RTD
Quality of CRMs is a legal responsibility for IRMM. Furthermore ISO 31 and 34 require stability and shelf-life estimates for vulnerable CRMs.
Invitations to tender were sent out for 40 CRMs to 30 labs for the 2001 campaign. New digestion methods were developed and results were received from 6 labs on 10 CRMs (2000 campaign; no instabilities detected). Results for 14 CRMs from 8 laboratories received with no indication of instability. Three more laboratories were added to the list for Expression of Interest, bringing the number of accepted laboratories to 47. 21 orders were placed for 34 reference materials. Results for 26 CRMs from 14 different laboratories have been received and evaluated. No signs of instability were found. The preparation of 1 new EoI for veterinary drug analysis was initiated. Stability testing exercises for 29 CRMs was organised. A new software tool for the evaluation of isochronous stability measurements was developed and implemented for the determination of CRM-expiry dates.
Certification of Charpy CRMs EN 10045-2, ASTM E-23 DG RTD
EN standard specifically requires the use of BCR Charpys for machine verification so the Commission has an obligation to CEN to provide these. As there is no trace ability between different international standards, the long-term goal is harmonisation of ASTM and EN standards (important for trade).
Eight batches were delivered and certified, the first batch was tested for the inter-comparison and the results were sent to NIST, USA. A new Charpy supply contract was approved by CCAM and awarded to LNE, France (annual, renewable up to 5 years). The remaining steel (about 3000kg) was shipped to LNE. Two castings of steel and 2x1200 batches of Charpys (30+120J) were ordered from LNE. The second "international master batch" testing round was carried out providing a useful comparison with NIST and Japanese machines and the monitoring of IRMM machine performance.
Solid fat content reference materials AOCS
In response to the requirement by AOCS for an official European CRM for NMR calibration of solid fat measurements. Unilever did LThe NMR evaluation of the new primary standard samples. On a visit to Bruker, the secondary plastic-in-oil standards were discussed and instrument specifications for the planned purchase of an LR-NMR were obtained and the purchase procedure commenced. A second set of primary standard samples (SSS in OOO) was prepared and the results were discussed. The framework contract for plastic-in-oil standards was signed with Bruker and the first order for 50 plastic-in-oil calibration sets was placed for delivery at the end of 2001. An NMR machine was ordered for certification of the plastic-in-oil calibration sets by IRMM.
Production metallurgical BCR CRMs DG RTD
This forms an important part of CRM production for BCR.
As a first step to replace Cu CRMs 74 and 75, 50 units of 75B were remade. Furthermore Pb samples CRMs 286-288 were cleaned and repacked.
Certification 322R-325R (unalloyed Zn) DG RTD
BCR re-certification work.
Evaluations and calculations for the certification were finished, the certification report written and all samples were engraved and packed. The certification was approved by the BCR review panel (8.6.01) with minor changes to make to the report. Meanwhile the four CRMs were put on sale.
Courses on RM preparation DG RTD
Contribution to improved quality of CRMs Europe-wide.
The course held from 14-16.6.01 at the University Barcelona (25 participants). Practical part was processing of a soil reference material to be further processed by 7 laboratories for evaluation in 2002. The purpose was to disseminate information on the production of laboratory control samples (not CRMs) to southern and Candidate Countries.
Development of SMELS (Synthetic Multi Element Standards) DG RTD
This is a tool for the external quality control of k0-NAA labs.
The stability of prototypes under high flux was investigated and the final matrix preparation was performed. The analysis of the matrix for impurities was also done and the type II material (spiked with 10 elements) was precipitated. SMELS standards with three different compositions were prepared by spiking, drying, crushing, sieving and bottling (ca. 300 bottles per type) and a homogeneity study was performed. All results were presented at the international k0-users workshop in Brugge.
Certification IRMM 530R(Al-Au) EWGRD
This CRM is the most important CRM for k0 NAA labs (Au monitor).
In 2001, the data from the certification involving 5 labs was evaluated, the report was written, approved and submitted for printing.
Other neutron dosimetry CRMs EWGRD
These CRMs are requested by the Euratom Working Group on Reactor Dosimetry and their use is mainly for reactor safety surveillance.
Progress was achieved for the following neutron dosimeters:
Al-Ag: report finished.
Al-Co (three CRMs): the certification report was finished and is ready for evaluation in November.
Al-Sc: one additional set of data was requested.
Furthermore the rolling of IRMM-521R (Ni) got underway and the "restricted procedure" call for laboratories for the certification campaign was carried out. NpO2 was packed for shipment to AEA for sol-gel sphere preparation.
Certification IRMM 541(U in glass) DG RTD
CRM recertification. This is used for geological dating, eg for petrochemical exploration.
Samples for U analysis were sent out to three labs and IRMM will measure the U5/U8 ratio and the impurities. The samples were sent to INW/RUG for irradiation under certified flux, the irradiations were completed and the U mass fraction analyses got underway at 6 labs. Stability control cannot be completed because of fire damage at the University Gent.
Nuclear target preparation OECD, CEA, ILL
In support to the neutron data programme, IRMM is the only (European) nuclear target provider.
In the first quarter of 2001 the following samples were delivered: I-129 (2 samples: IRMM), Cr-52 (2 samples: IRMM), LiI (2 samples: IRMM), polyimide (5 samples: IRMM), B-10 (1 sample: IRMM), temp monitors (5 samples: Siemens), Pb (4 samples: IRMM). New test deposits of Pu-242 on Ni were made for the CEA.
In the second quarter samples delivered included: Ni-58 (1 sample: IRMM), Pu-242 (IRMM: 1 sample), Pu-242 (5 samples: CEA), Am-243 (5 samples: CEA), Al-Mn (1 sample: ITN, Portugal), Ni-61 (1 sample: IRMM). Ta layers were polished and sent to GSI for metal deposition (for IRMM). Polyimide and carbon substrates were sent to Russia and Univ. Mainz for Cf-252 deposition. Nine more glove boxes were catered for disposal (that makes a grand total of 25 since start of denuclearisation campaign).
In the third quarter samples delivered include: Pu-240 (1 sample: IRMM), Eu (1 sample: IRMM), Th-232 (1 sample: IRMM), Nb, Ni, Co deposits on Ta (12 samples: IRMM), I-129 (2 samples: IRMM), Zr (1 sample CCEN, Brazil), In, Zr (2 samples: Tajura, Libya). Evaporation installations were modified for Se-77, Sm-147 evaporations, U-235 test deposits made by electro-deposition, Pb-206 was reduced with hydrogen and rolled to foil. Encapsulation of Nb flux monitors for CERCA (France) also got underway.
Thin film reference samples DG RTD
Making use of IRMM's unique equipment and know how for the deposition of surface layers traceable to the SI, provision of reference samples for the improvement and trace ability of surface and interface analytical measurements performed in research labs and high-tech industry.
The evaluations and calculations for certification of IRMM-302 Sb in Si were completed with GUM compliant uncertainty estimates.The certification report and certificate were reviewed at IRMM and BAM and the certification of the material was accepted. Since new measurements of IRMM-302 with synchrotron radiation induced XRF proved a better homogeneity than previously assessed, the certification report and certificate were revised resulting in an unsurpassed certified value having only 1.2% relative expanded uncertainty.
Output Indicators and Impact
Indicators are: sales volume, new CRM certifications, samples produced (including nuclear targets) and publications.
Impact is in the area of support to European (and world) metrology, particularly support to CEN (through CRMs needed for application of EN standards). The BCR programme already has major international recognition and will be further enhanced by the incorporation of DG RTD responsibilities into the DG JRC programme.
Summary of the project
Certified Reference Materials (CRMs) are required to support international trade, the mutual acceptance of measurements and goods as well as underpinning international standardisation.
This project is directly connected with the Programme "Measurement and Testing" (M&T, formerly BCR) of the Research DG which finances research for the development and production of BCR(r)-CRMs. Once certified these materials are transferred to the IRMM who has the responsibility for storage, stability control, distribution and renewal when the material is exhausted. Presently 500 different BCR CRMs are available at IRMM with a storage load of some 500.000 units.
Rationale
Certified Reference Materials (CRM) are required to achieve comparability of measurements in all areas where technical measurements are performed. In the field of chemistry CRMs are the most important means to achieve "trace ability to stated references" as required in a structured measurement system, which should provide a reliable underpinning of trade and industry. Correct assessment of the composition and quality of virtually all products is of primary importance in promoting international trade, detecting fraud and providing correct information to consumers. IRMM provides a unique high-technology support to the production and certification of BCR reference materials, which rank second in the world after NIST Standard Reference Materials (USA). The laboratory itself is considered one of the world leaders and hosts a unique multi-functional and flexible production laboratory, clean chambers, cryo grinding, freeze drying, high purity milling, ultra fine classification and levitation melting. This highly flexible laboratory can quickly adapt its production facilities to cater for urgent requests that stem from the policy makers and has a modern adjoining analytical laboratory fully equipped to monitor and control the production process. Dosimetry CRMs, for example, are increasingly required for the safe and efficient operation of power plants, improved accuracy in pressure vessel lifetime assessments and the fulfilment of quality assurance obligations. IRMM provides the only certified stock of neutron dosimetry CRMs worldwide.
Champ scientifique (EuroSciVoc)
CORDIS classe les projets avec EuroSciVoc, une taxonomie multilingue des domaines scientifiques, grâce à un processus semi-automatique basé sur des techniques TLN. Voir: Le vocabulaire scientifique européen.
CORDIS classe les projets avec EuroSciVoc, une taxonomie multilingue des domaines scientifiques, grâce à un processus semi-automatique basé sur des techniques TLN. Voir: Le vocabulaire scientifique européen.
- sciences naturelles informatique et science de l'information logiciel
- ingénierie et technologie ingénierie des materiaux revêtement et films
- ingénierie et technologie ingénierie des materiaux solides amorphes
- sciences sociales économie et affaires entreprise et gestion commerce
- lettres philosophie, éthique et religion philosophie
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Coordinateur
B-2440 Geel
Belgique
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