Fusion Bead Procedure for Nuclear Forensics Employing Synthetic Enstatite to Dissolve Uraniferous and Other Challenging Materials Prior to Laser Ablation Inductively Coupled Plasma Mass Spectrometry

Abstract

There is an increasing demand for rapid and effective analytical tools to support nuclear forensic investigations of seized or suspect materials. Some methods are simply adapted from other scientific disciplines and can effectively be used to rapidly prepare complex materials for subsequent analysis. A novel sample fusion method is developed, tested, and validated to produce homogeneous, flux-free glass beads of geochemical reference materials (GRMs), uranium ores, and uranium ore concentrates (UOC) prior to the analysis of 14 rare earth elements (REE) via laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The novelty of the procedure is the production of glass beads using 9 parts high purity synthetic enstatite (MgSiO) as the glass former with 1 part of sample (sample mass ∼1.5 mg). The beads are rapidly prepared (∼10 min overall time) by fusing the blended mixture on an iridium strip resistance heater in an argon-purged chamber. Many elements can be measured in the glass bead, but the rare earth group in particular is a valuable series in nuclear forensic studies and is well-determined using LA-ICP-MS. The REE data obtained from the GRMs, presented as chondrite normalized patterns, are in very good agreement with consensus patterns. The UOCs have comparable patterns to solution ICP-MS methods and published data. The attractions of the current development are its conservation of sample, speed of preparation, and suitability for microbeam analysis, all of which are favorable for nuclear forensics practitioners and geochemists requiring REE patterns from scarce or valuable samples.

Rapid Determination of Trace Element Compositions in Peridotites by LA‐ICP‐MS Using an Albite Fusion Method

“…, Reading et al . ) and migration of transition elements (e.g., Ni and Cr) into capsules (Kurosawa et al . , He et al .…”

Recent Advances in Nuclear Forensic Chemistry

“…This is demonstrated by Reading and co-workers for custom-made, UOC-containing glassy beads, which are designed to model glassy fallout in a postdetonation scenario. 95 This study is noteworthy not only because it showcases the microanalytical capabilities of LA-ICP-MS for nuclear materials but also because it introduces a new synthetic process that can be used to model nuclear weapon debris in a controlled laboratory setting.…”

Atomic Spectrometry Update – a review of advances in environmental analysis

“…An alternative approach for bulk analysis by LA-ICP-MS is the preparation of fused beads. In a fusion procedure developed 254 for the analysis of U ore concentrates and uraniferous ores with low silica contents, highly pure synthetic enstatite (MgSiO 3 ) was added to ~1.5 mg of sample powder in the proportion of 9+1 (enstatite + sample) to improve the fusion properties of these materials. The blended mixture was fused on an iridium strip resistance heater in an argon-purged chamber to form glass beads.…”