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Chemical reference methods and measurements for normalisation and certification

Objective

Specific Objectives
- Support in the certification of environmental, biological and food reference materials in organic analysis for trace metals;
- Method development for the reliable analysis of compounds in environmental, biological and food (e.g. pesticides in oranges, trace metals in honey) matrices;
- Method development for the reliable analysis of traces of metals and/or radionuclides in food and environmental matrices;
- Provide metrological support to all units of the institute.
Planned Deliverables

Specific Deliverables to DGs
- To deliver reference values for actinoids, radium and strontium for IAEA milk powder and soil (DG RELEX);
- Th in workplace materials: Results of feasibility and research studies on relevant materials, available standards and suitable determination procedures
(DG RTD).

Deliverables as a result of the research
- Certified reference methods and materials needed for the implementation of EU legislation;
- International proficiency testing exercises and advice on reference measurements;
- Provide expertise in the separation and quantification of radio nuclides and/or trace metals in complex matrices.

Summary of deliverables made by: 31/12/2001

Radionuclides DGs RELEX, TRADE and RTD
The Thorium Network. This purpose of this network is to implement the directive (EURATOM 96/29) laying down the basic safety standards for health protection of the general public and workers. It states that all environmental and workplace materials above 100Bq/g must be reported;
The results of the 3rd inter-comparison samples were received and the final evaluation report is presently being drafted. The 2001 workshop was successfully organised in collaboration with the Belgian Nuclear Centre (SCK/CEN) and 72 participants attended it from 17 countries. The project is now principally completed and an Expression of Interest for a dedicated call was submitted to the GROWTH Programme, on the subject Feasibility study for the preparation of Certified reference materials for the Analysis of Thorium in Workplace Materials in the Non-Nuclear Industry.

Pu-2000;
inter-comparison for the external quality control of Safeguards and NMC laboratories;
The results were received and transferred to the DAMRI for evaluation. The IAEA are now also interested to use the samples for validation of new detection systems and are expected to send an official request.

De-nuclearisation
The decontamination and clearance of the whole Chemistry Building is finished. Refurbishment will almost be finished by the end of the year. The first new laboratories have been taken back into operation.

Support to Certification (of Reference Materials)
The air filters task was completed and the results were submitted to the customer. The stability measurements of Li, Ca and Mg in serum (BCR 304) were also completed and the evaluation of data is presently in progress.
Stability measurements of Mg, Ca and Mn in two water reference materials (BCR 616 and 617) were completed and the final report was submitted to the customer. Measurements of Na and K in the same reference materials are foreseen for the near future.
The homogeneity tests for BCR 804 and soy flour were completed and the reports were submitted to the customers rendering these tasks completed. Evaluation of a request (including literature research) commenced for the certification of 2 honey reference materials and stability measurements of Mg, Ca, Zn, Mn by ICP-OES have started for BCR 129. Finally for the request for stability tests on BCR 281 were evaluated and accepted.

Metrological Support
Forming the backbone of IRMMs measurements, the calibration of weight sets including the checking and calibration of balances was performed twice and maintained at the highest level.
Metrological measurements were carried out in direct support to the following tasks:
- IRMM-1027f (dried spikes)
- IRMM-058 (233U)
- MP2-solution (239Pu);
- IMEP-12 (serum): density measurements were carried out on serum samples and 3 water samples;
- IMEP-17 (IDMS for Cl: 6 spikings + IA; IDMS for Fe: 6 spiking + 4 blanks; IDMS for Ca: 6 spiking + 4 blanks);
- IMEP-19 (rice powder): 6 spikings with 111Ca, 65Cu, 206Pb and evaporation control;
- Alignment work was carried out on the 150MeV linear accelerator;
- 10B measurements on Inox backings
- For IM-6009 and IM-6008, isotope dilution mass spectrometry for Ca required 12 spikings + 6 blanks. That entailed the weighing of Ca, Li and Mg standards + dilution for atomic absorption;
- For SSS-OOO BCR standards measurements were performed for 15% SSS, 45% SSS, 60% SSS and 75% SSS;
- For 1027f gravimetric distribution, 600 measurements were performed and about "b 400 still need to be done;
- Micro reference material length measurements were performed on 5 samples;
- 13 mixtures + 5 blanks were prepared for the sulphur mixtures;
- For JRC project 72, mass determinations of Nb was performed on 42 strips;
- Weightings were performed for 44Ca and natCa reference solutions and for a range of sediments (RMs 277, 280 and 320: 12 samples for atomic absorption) and serum 9RM stability: 3 samples for atomic absorption);
- Finally for the 1027f solution: 6 spikings with IRMM-046b for JNC method were performed.

Output Indicators and Impact

The focus is on the development of chemical separations and determinations of (low-level) radio nuclides in environmental and food matrices for which substantial know-how has been accumulated and on (non-nuclear) trace analysis of elements (like heavy metals) in the frame of certification of CRMs and PTMs for which a substantial in-house capacity is needed (service for Reference Materials Unit at IRMM).Analytical support in the frame of the certification, homogeneity and stability control of CRMs is expanding. For reference measurements of radionuclides, the development and application of high performance analytical methods aiming to support the protection of workers and the citizen (e.g. Ra in ground and drinking water, Th in work place materials) will be continued.
Summary of the project

High performance and reliable reference methods and analytical measurement procedures are indispensable for the execution of Commission policies on normalisation and standardisation. In summary this project entails:
- Developing analytical methods to very high standards and to adapt chemical measurement procedures to the specific requirements imposed by the implementation of directives and the needs in monitoring of EU policies as well as the characterisation of reference materials;
- Establishing, improving and validating a pool of complementary analytical techniques for trace element analysis and radio nuclide determination in all kinds of sample matrices, for speciation of chemical elements and for analysis of organic micro-constituents in various matrices.

Rationale:
Reference analytical measurements are required to ensure a harmonisation and equivalence of chemical data in many areas, like securing industrial standards, food and environmental quality, health at the work place ¡V to name but a few. With globalisation, EU enlargement and an increased importance attached to world trade issues, more scientific reference methods are needed to enact EU policies and provide hands-on scientific support towards EU harmonisation and interaction with the EU's trading partners, particularly future Member States.

Funding Scheme

JRC - Joint Research Centre research

Coordinator

Institute for Reference Materials and Measurements
Address
Retieseweg
B-2440 Geel
Belgium