Evaluation of EC interlaboratory comparison on radionuclides in soil

A comparison was organised by the Institute for Reference Materials and Measurements among 73 environmental radioactivity monitoring laboratories for the determination of 15 radionuclides in soil. The reference material IAEA-375 Soil was reprocessed to provide the comparison material and reference values traceable to SI units and SIR were established at IRMM. The analytical procedures used by participating laboratories are described. A robust evaluation of the performance of laboratories is performed using three different approaches: relative deviations, En numbers and PomPlots. The performance of the participating laboratories varied depending on the radionuclide determined and method used. Gamma-ray spectrometry with respect to 137Cs and 40K is well controlled. The determination of 90Sr proved difficult for about two-thirds of the participants, which submitted results outside the acceptable range. Several laboratories need to improve their analytical procedures for the uranium isotopes and 226Ra. Moreover, the results for thorium isotopes are far from satisfactory mainly for the 230Th. The use of the En criterion revealed that the uncertainty estimation of many participants is poor.JRC.D.4-Standards for Nuclear Safety, Security and Safeguard

Evaluation of EC Measurement Comparison for 137Cs, 40K and 90Sr in Milk Powder

This report describes the full life cycle of the measurement comparison of 137Cs, 40K and 90Sr in milk powder among 60 European laboratories monitoring radioactivity in food and the environment. An available IAEA reference material was re-processed at IRMM into suitable intercomparison samples and the homogeneity of the distributed samples together with other quality parameters was determined. Reference values of the three radionuclides under study in this intercomparison were determined at IRMM using tracer techniques and standardised radionuclide solutions and are thus traceable to the SI units. The sample preparation and measurement processes applied in the participating laboratories are described and the results of the intercomparison are presented and discussed in detail. Whereas, in general, the measurement results for 137Cs and 40K show good agreement with the reference value, the results of this comparison point at problems of 90Sr determination in about one third of the laboratories. The corresponding participants should investigate and revise their analytical methods, next to many laboratories needing to improve their estimation of measurement uncertainty.JRC.D.4-Isotope measurement

Evaluation of EC Comparison on the Determination of 226Ra, 228Ra, 234U and 238U in Mineral Waters

This report describes all details of the comparison for the determination of 226Ra, 228Ra, 234U and 238U in mineral waters among 45 European laboratories monitoring radioactivity in food and the environment. Three commercially available mineral waters were provided as comparison samples. Reference values of the four radionuclides under study in this comparison were determined in collaborative work of IRMM and the Bundesamt für Strahlenschutz (BfS), using tracer techniques and standardised radionuclide solutions. The reference values are thus traceable to the SI units. The sample preparation and measurement processes applied in the participating laboratories are described and the results of the comparison are presented and discussed in detail. Whereas, in general, the measurement results for the uranium isotopes show a relatively favourable agreement with the reference value, the results of this comparison point at severe problems of 226Ra and 228Ra determination in about one fourth and more than one third of the laboratories, respectively. For radium, 19 results corresponding to 14 % of all are even off by a factor of two or more. By comparison, for uranium, this number amounts to 6 % (9 results out of 150). Nevertheless, also for the determination of uranium, 14 % to 23 % of the laboratories report results not compliant with the En evaluation criterion. The corresponding participants are urgently requested to investigate and revise their analytical methods.JRC.D.4-Nuclear physic

Results of a European interlaboratory comparison on gross alpha/beta activity determination in drinking water

An interlaboratory comparison was organised by the Institute for Reference Materials and Measurements (JRC-IRMM) among environmental radioactivity monitoring laboratories for the determination of gross alpha/beta activity concentration in drinking water. Four independent standard methods were used for the determination of the reference values of three different water samples. The performance of participating laboratories was evaluated with respect to the reference values using relative deviations. Sample preparation and measurement methods used by the participating laboratories are described in detail, in particular in the view of method-dependency of the results. Many of the participants’ results deviate by more than two orders of magnitude from the reference values regardless of the techniques used. This suggests that gross methods need revision.JRC.D.4-Standards for Nuclear Safety, Security and Safeguard

Feasibility study for the development of plutonium reference materials for age dating in nuclear forensics

Isotopic reference materials certified for the age of nuclear material (uranium, plutonium) are needed in the fields of nuclear forensics and environmental measurements. Therefore a feasibility study for the development of plutonium reference materials for age dating has been started recently at the Institute for Reference Materials and Measurements (EC-JRC-IRMM). The "age" of the material is defined as the time that has passed since the last chemical separation of the mother and daughter isotopes (e.g. 241Pu and 241Am). Assuming that the separation has been complete and all the daughter isotopes have been removed from the original material during this last separation, the age of the material can be determined by measuring the ratio of daughter and mother radio-nuclides, e.g. 241Am/241Pu. At a given time after the last separation and depending on the half lives of the radio-nuclides involved, a certain amount of the daughter radionuclide(s) will be present. For the determination of the unknown age of a material different "clocks" can be used; "clocks" are pairs of mother and daughter radio-nuclides, such as 241Am/241Pu, 238Pu/234U, 239Pu/235U, 240Pu/236U, and possibly 242Pu/238U. For the age estimation of a real sample, such as material seized in nuclear forensics investigations or dust samples in environmental measurements, it is advisable to use more than one clock in order to ensure the reliability of the results and to exclude the possibility that the sample under question is a mixture of two or more materials. Consequently, a future reference material certified for separation date should ideally be certified for more than one "clock" or several reference materials for different "clocks" should be developed. The first step of this study is to verify the known separation dates of different plutonium materials of different ages and isotopic compositions by measuring the mother (238Pu, 239Pu, 240Pu, 241Pu, 242Pu) and daughter (234U, 235U, 236U, 238U and 241Am) isotope abundances and to estimate the achievable uncertainties of the calculated ages. Thermal ionisation mass spectrometry (TIMS) is applied for the measurement of the plutonium and uranium isotope ratios after chemical separation of the plutonium and uranium fractions from the sample matrix, while 241Am is measured by gamma-ray spectrometry. In the course of this work the reference materials NBS SRM 946, 947 and 948 (NBL CRM 136, 137 and 138) will be investigated among others.JRC.E.7-Nuclear Safeguards and Forensic

Evaluation of EC Measurement Comparison on Simulated Airborne Particulates - 137Cs in Air Filters

This report describes the full life cycle of the measurement comparison of 137Cs in air filters among 43 European laboratories monitoring radioactivity in the environment. Gravimetrically pipetting droplets of a gravimetrically diluted standardised 137Cs solution onto real air filters, SI-traceable reference values were established for intercomparison filters carrying a large range of activity close to the routine measurement conditions of the corresponding laboratory. The sample preparation and measurement processes applied in the participating laboratories are described and the results of the intercomparison are presented and discussed in detail. The results point at some problems of radioactivity measurement in air filters which need to be improved by several laboratories. Overall, with 41 out of 48 reported measurement results lying within +/- 33 % of the IRMM reference value, this comparison renders a rather fair result.JRC.D.4-Isotope measurement

Preparation and certification of 243Am spike reference material: IRMM-0243 : Certified reference material for the amount content of 243Am and n(241Am)7n(243Am) isotope amount ratio

This report describes the preparation and certification of IRMM-0243, a 243Am spike reference material. It is certified for the amount content of 243Am and the isotope amount ratios of n(241Am)/n(243Am) and n(242mAm)/n(243Am). Furthermore, the material is certified for the amount contents of 241Am and total Am, the mass fractions of 243Am, 241Am and total Am, the isotope amount and mass fractions (e.g. isotopic composition) and the molar mass of Am. The material was produced in compliance with ISO/IEC 17034:2016 and certified in accordance with ISO Guide 35:2006. The material was prepared by dilution of an americium starting solution in nitric acid and dispensing of the solution into glass ampoules. In total 587 units were produced. Between-unit homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2006. The characterisation of the amount content of 243Am was performed by Isotope Dilution Mass Spectrometry (IDMS) using a 241Am spike, produced from highly enriched 241Pu material. The isotope amount ratios of n(241Am)/n(243Am) and n(242mAm)/n(243Am) were measured by Thermal Ionisation Mass Spectrometry (TIMS). The certified values were verified by alpha particle spectrometry, alpha particle counting at a defined solid angle (DSA) and high-resolution gamma-ray spectrometry as independent verification methods. The uncertainties of the certified values were estimated in compliance with the Guide to the Expression of Uncertainty in Measurement (GUM) [ ] and include uncertainties related to possible inhomogeneity, instability and characterisation. The main purpose of this material is for use as a spike isotopic reference material for the quantification of americium by IDMS in unknown samples. A unit of IRMM-0243 consists of a glass ampoule with a screw cap containing about 3.5 mL nitric acid solution (c = 1 mol/L) with an americium mass fraction of about 1.5 μg/g solution. The material is a true solution; therefore there is no recommended minimum sample intake to be taken into account.JRC.G.2-Standards for Nuclear Safety, Security and Safeguard

The certification of the activity concentration of the radionuclides 137Cs, 90Sr and 40K in wild berries: IRMM-426

This report describes the production of CRM IRMM-426, a dried bilberry material certified for the radionuclide activity concentrations of 137Cs, 90Sr and 40K. The material was produced following ISO Guide 34:2009. Bilberry samples were collected in a woodland region of so-called “strontium hot spots” close to the Chernobyl reactor site. The samples were air-dried at the sampling site before transport to IRMM, where the raw material was oven-dried, cryo-milled, sieved, homogenised and bottled. The bottled material was sterilised by gamma-irradiation. Between-unit homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2006. The material was characterised by an intercomparison among laboratories of demonstrated competence and adhering to ISO/IEC 17025. Technically invalid results were removed but no outlier was eliminated on statistical grounds only. Uncertainties of the certified values were calculated in compliance with the Guide to the Expression of Uncertainty in Measurement (GUM) and include uncertainties related to possible inhomogeneity and instability and to characterisation. The material is intended for the assessment of method performance and quality control. As any reference material, it can also be used for control charts or validation studies. The CRM is available in amber glass jars containing about 100 g of dried bilberry powder. The minimum amount of sample to be used for analysis is 50 g for 90Sr and 18 g for 137Cs and 40K.JRC.D.2-Standards for Innovation and sustainable Developmen