Rapid Microanalysis-Based Process for Nuclear Material Characterization for Nuclear Forensics

Conventional nuclear forensics workflows rely on complete dissolution and radiochemical separations of bulk samples, providing robust measurements but potentially obscuring microscale heterogeneity and requiring lengthy processing. A complementary microanalysis-based workflow is presented for rapid characterization of nuclear material for nuclear forensics. For post-detonation nuclear forensics samples, the approach integrates radiological particle localization, targeted microsample extraction and gamma spectrometric analysis, automated microdissolution, reduced-volume separations, mass spectrometry, and data-driven process optimization. In two demonstrations, ionizing-radiation quantum imaging detectors identified regions of interest in surrogate post-detonation particulate samples, which were processed by automated microdissolution, custom microcolumns, and multicollector ICP-MS. The experiments demonstrate how uranium, plutonium and neptunium isotopics can be rapidly quantified along with fission products on single particulate samples. The single particulate subsamples showed distinct isotopic compositions, demonstrating heterogeneity that bulk analysis would obscure. These results establish a targeted microanalysis pathway that complements established bulk methods and supports adaptive processing and streamlined reporting.