Sample Preparation Method for Analysis of Swipe Samples by Inductively Coupled Plasma Mass Spectrometry

International nuclear safeguards have been applied for over 30 years to control nuclear activities. Following the recon of undeclared nuclear activities in Iraq in 1991, strengthening of the safeguards system became necessary (1995). From 1996 the detection of undeclared nuclear activities using sensitive and precise analysis of swipe samples became one of the most important parts of IAEA inspections. The aim of this study was the development of a fast and easy sample preparation and analysis method for the bulk uranium and plutonium analysis of swipe samples. For the sample preparation low power microwave-assisted digestion followed by extraction chromatography using TRU resin was applied. The concentration of analytes of interest and their isotopic composition were determined by inductively coupled plasma sector field mass spectrometry (ICP-SFMS). The analytical performance of the method is in good agreement with the requirements (accuracy, precision, repeatability) of the International Atomic Energy Agency¿Network for Analytical Laboratories (IAEA¿NWAL) and can be applied for routine analysis. The low detection limits achieved enable the determination of the isotope ratios and isotope concentrations of U and Pu (234U, 235U, 236U, 238U and 239Pu, 240Pu, 241Pu) present in ultratrace concentration levels in swipe samples. The method was tested with real swipe samples collected at Hungarian radioactive source producing facilities.JRC.E.7-Nuclear Safeguards and Forensic

Determination of Rare-earth Elements in Uranium-bearing Materials by Inductively Coupled Plasma Mass Spectrometry

A novel and simple analytical procedure has been developed for the trace-level determination of lanthanides (rare-earth elements) in uranium-bearing materials by inductively coupled plasma sector-field mass spectrometry (ICP-SFMS). The method involves a selective extraction chromatographic separation of lanthanides using TRUTM resin followed by ICPSFMS analysis. The limits of detection of the method proposed is in the low pg g-1 range, which are approximately two orders of magnitude better than that of without chemical separation. The method was validated by the measurement of reference material and applied for the analysis of uranium ore concentrates (yellow cakes) for nuclear forensic purposes, as a potential application of the methodology.JRC.E.7-Nuclear Safeguards and Forensic

Report on the Workshop on Direct Analysis of Solid Samples Using Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS)

The ESARDA Working Group on Standards and Techniques for Destructive Analysis (WG DA), in close collaboration with the Hungarian Atomic Energy Authority (HAEA) and the University of Natural Resources and Life Sciences (BOKU), organized a dedicated workshop on 'Direct Analysis of Solid Samples Using Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS)'. The workshop was held in conjunction with the ESARDA Symposium, on 16 May 2011 at the Helia Conference Hotel in Budapest, Hungary. The workshop aimed to explore the potential of LA-ICP-MS for safeguards, non-proliferation, nuclear forensics and other applications. Safeguard authorities, fuel manufactures, analytical laboratories and experts in the field of LA-ICP-MS were invited to participate in this workshop, to exchange views and information on the challenges and limitations of LA-ICP-MS in these areas. Forty representatives from the main European and International nuclear safeguards organizations, nuclear measurement laboratories, nuclear industry and manufacturers, but also experts from geochemistry and environmental sciences institutes participated in this workshop. The plenary lecture was given by Dr. Joachim Koch from the ETH Zürich on 'Recent Trends and Advancements in LA-ICP-MS' followed by a session focussing on the application of LA-ICP-MS in nuclear safeguards and nuclear forensics. The second session of this workshop was entirely dedicated to particle analysis with LA-ICP-MS and quality control. The findings and points of discussions from these sessions were further discussed in a working group using the 'world café' approach around 4 selected topics enabling that all workshop participants could benefit from the 'collective intelligence'. This report is a summary of the findings and points of discussions raised during the sessions and in the working group, including recommandations for research, instrumental development and quality control, reference materials and data interpretation, emphasizing also different fields of application. Like in previous workshops organized by the ESARDA WGDA, all participants recognized once more the need and the benefit of intensifying the cooperation between the nuclear safeguards, nuclear forensics community on the one hand, the nuclear industry and the instrument manufacturers on the other hand with environmental institutes. This report is an attempt to share the outcome of this workshop with a broader community.JRC.D.2-Reference material

Determination of trace elements in lithium niobate crystals by solid sampling and solution-based spectrometry methods

Solid sampling (SS) graphite furnace atomic absorption spectrometry (GFAAS) and solution-based (SB) methods of GFAAS, flame atomic absorption spectrometry (FAAS), inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) were elaborated and/or optimized for the determination of Cr, Fe and Mn trace elements used as dopants in lithium niobate optical crystals. The calibration of the SS-GFAAS analysis was possible with the application of the three-point-estimation standard addition method, while the SB methods were mostly calibrated against matrix-matched and/or acidic standards. Spectral and non-spectral interferences were studied in SB-GFAAS after digestion of the samples. The SS-GFAAS method required the use of less sensitive spectral lines of the analytes and a higher internal furnace gas (Ar) flow rate to decrease the sensitivity for crystal samples of higher (doped) analyte content. The chemical forms of the matrix produced at various stages of the graphite furnace heating cycle, dispensed either as a solid sample or a solution (after digestion), were studied by means of the X-ray near-edge absorption structure (XANES). These results revealed that the solid matrix vaporized/deposited in the graphite furnace is mostly present in the metallic form, while the dry residue from the solution form mostly vaporized/deposited as the oxide of niobium