The application of scanning electron microscopy (SEM) and secondary ion mass spectrometry (SIMS) for characterization of mixed plutonium and uranium particles from nuclear weapons material is presented. The particles originated from the so-called Thule accident in Greenland in 1968. Morphological properties have been studied by SEM and two groups were identified: a "popcorn" structure and a spongy structure. The same technique, coupled with an energy-dispersive X-ray (EDX) spectrometer, showed a heterogeneous composition of Pu and U in the surface layers of the particles. The SIMS depth profiles revealed a varying isotopic composition indicating a heterogeneous mixture of Pu and U in the original nuclear weapons material itself. The depth distributions agree with synchrotron-radiation-based mu-XRF (X-ray fluorescence microprobe) measurements on the particle (Eriksson, M., Wegryzynek, D., Simon, R., & Chinea-Cano, E., in prep.) when a SIMS relative sensitivity factor for Pu to U of 6 is assumed. Different SIMS identified isotopic ratio groups are presented, and the influence of interferences in the Pu and U mass range are estimated. The study found that the materials are a mixture of highly enriched 235U (235U:238U ratio from 0.96 to 1.4) and so-called weapons grade Pu (240Pu:239Pu ratio from 0.028 to 0.059) and confirms earlier work reported in the literature.
In order to prevent nuclear proliferation, the isotopic analysis of uranium and plutonium microparticles has strengthened the means in international safeguards for detecting undeclared nuclear activities. In order to ensure accuracy and precision in the analytical methodologies used, the instrumental techniques need to be calibrated. The objective of this study was to produce and characterize particles consisting of U, Pu, and mixed U-Pu, suitable for such reliability verifications. A TSI vibrating orifice aerosol generator in connection with a furnace system was used to produce micrometer sized, monodispersed particles from reference U and Pu materials in solution. The particle masses (in the range of 3-6 pg) and sizes (approximately 1.5 microm) were controlled by the experimental conditions and the parameters for the aerosol generator. Size distributions were obtained from scanning electron microscopy, and energy-dispersive X-ray analysis confirmed that the particle composition agreed with the starting material used. A secondary ion mass spectrometer (SIMS) was used to characterize the isotopic composition of the particles. Isobaric and polyatomic interference in the SIMS spectra was identified. In order to obtain accurate estimates of the interference, a batch of Pu particles were produced of mainly (242)Pu. These were used for SIMS analysis to characterize the relative ionization of Pu and U hydride ions and to determine the SIMS useful yields of U and Pu. It was found that U had a higher propensity to form the hydride than Pu. Useful yields were determined at a mass resolution of 450 for U-Pu particles: (1.71 +/- 0.15) % for Pu and (0.72 +/- 0.06) % for U. For Pu particles: (1.65 +/- 0.14) % for Pu. This gave a relative sensitivity factor between U and Pu (RSF(U:Pu)) of 2.4 +/- 0.2. However, the RSF(U:Pu) showed large fluctuations during the sputtering time for each analyses of the mixed U-Pu particles, in the range of 1.9-3.4.
Balkan endemic nephropathy (BEN), a kidney disease that occurs in rural villages in Bosnia, Bulgaria, Croatia, Romania, and Serbia, is thought to be linked to an environmental toxin. The authors review literature on proposed environmental exposure agents, report the results of field sampling and analysis studies to evaluate potentials for exposure to proposed agents, and propose criteria for future testing. They used these criteria to evaluate the evidence for suggested hypotheses, concluding that several proposed agents can be eliminated or considered unlikely based on apparent inconsistencies between clinical or epidemiologic evidence related to BEN and toxicologic or exposure evidence related to the agents. Mycotoxins and aristolochic acid are the primary targets of current toxicologic investigations, and while the evidence on exposures for both is potentially consistent, it is insufficient.
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