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At least 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Optical vibrational spectroscopic signatures related to U 3 O 8 production processes

Uranium ore concentrates are materials found early within the nuclear fuel cycle and contain high concentrations of uranium in an easily transported form, making the concentrates a likely target for illegal diversion. These concentrates are typically converted to U 3 O 8 for further processing and, therefore, may lose specific physicochemical characteristics in determining the materials’ source and processing history. In this work, we explore the Raman spectra of eight oxide samples produced from various uranium ore concentrates and processing pathways to examine the presence of spectroscopic signatures relating to each sample's process history. Samples produced from amine extraction and dialkylphosphoric acid extraction processes show unique characteristics due to high concentrations of α-UO 3 , whereas samples calcinated from metallic diuranates do not form pure α-U 3 O 8 because of metallic ion inclusions. Pure α-U 3 O 8 oxide samples are obtained through calcination of ammonium diuranate, ammonium uranyl carbonate, and metastudtite intermediates. The Raman spectra of these oxide samples show close agreement with pristine α-U 3 O 8 spectra. However, deviations from the pristine spectra are observed in the 300–460 cm -1 spectral range. In conclusion, these deviations are unique identifying signatures that were likely created by lasting effects from the process history. Spectral center of mass calculations indicate grouping of samples based on processing history.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

Effect of Plutonium on Uranium Oxide Microstructural Fingerprint

The analysis of particulates from environmental sampling is routinely performed for nuclear forensics applications. In order to increase the tools available for nuclear forensics applications, capability development materials (CDMs), or reference particulates, are necessary for developing and benchmarking new analytical methods. Historically, these CDM particulates have been produced with highly controlled and characterized isotopic and size parameters for applications in developing and benchmarking particle sizers and mass spectrometry analytical methods [1- 4]. However, the development of CDMs with highly characterized particle morphology and phase of the particles is vital for aiding in the development and benchmarking of particle analytical methods for those parameters. In many cases, key properties such as crystallographic phase, morphology, and microstructure, may be correlated to processing history of environmental sampling particulates [5]. To that end, this work investigates determining the structural fingerprint of produced Pu-doped uranium oxide CDMs using transmission electron microscopy (TEM). The particulates, one of which shown in Figure 1, were synthesized to Fig. 1. Single particulate of uranium oxide fabricated using the THESEUS technique. develop capabilities for environmental sampling investigations. These particles are monodisperse at diameter of 1 μm and a range of plutonium concentrations from 0- 1,000 ppm. Given their small diameter, TEM analysis was ideal for studying the particulate structural fingerprint in detail. Previous investigations confirmed the external homogeneity of the particulates at different plutonium concentrations, however this analysis focuses on determining the grain structure, phase distribution, and porosity of the particulates.

Mayer, Jack [Univ. of Florida, Gainesville, FL (Un↗
NASA NTRS2008

Hyperspectral Fluorescence and Reflectance Imaging Instrument

The system is a single hyperspectral imaging instrument that has the unique capability to acquire both fluorescence and reflectance high-spatial-resolution data that is inherently spatially and spectrally registered. Potential uses of this instrument include plant stress monitoring, counterfeit document detection, biomedical imaging, forensic imaging, and general materials identification. Until now, reflectance and fluorescence spectral imaging have been performed by separate instruments. Neither a reflectance spectral image nor a fluorescence spectral image alone yields as much information about a target surface as does a combination of the two modalities. Before this system was developed, to benefit from this combination, analysts needed to perform time-consuming post-processing efforts to co-register the reflective and fluorescence information. With this instrument, the inherent spatial and spectral registration of the reflectance and fluorescence images minimizes the need for this post-processing step. The main challenge for this technology is to detect the fluorescence signal in the presence of a much stronger reflectance signal. To meet this challenge, the instrument modulates artificial light sources from ultraviolet through the visible to the near-infrared part of the spectrum; in this way, both the reflective and fluorescence signals can be measured through differencing processes to optimize fluorescence and reflectance spectra as needed. The main functional components of the instrument are a hyperspectral imager, an illumination system, and an image-plane scanner. The hyperspectral imager is a one-dimensional (line) imaging spectrometer that includes a spectrally dispersive element and a two-dimensional focal plane detector array. The spectral range of the current imaging spectrometer is between 400 to 1,000 nm, and the wavelength resolution is approximately 3 nm. The illumination system consists of narrowband blue, ultraviolet, and other discrete wavelength light-emitting-diode (LED) sources and white-light LED sources designed to produce consistently spatially stable light. White LEDs provide illumination for the measurement of reflectance spectra, while narrowband blue and UV LEDs are used to excite fluorescence. Each spectral type of LED can be turned on or off depending on the specific remote-sensing process being performed. Uniformity of illumination is achieved by using an array of LEDs and/or an integrating sphere or other diffusing surface. The image plane scanner uses a fore optic with a field of view large enough to provide an entire scan line on the image plane. It builds up a two-dimensional image in pushbroom fashion as the target is scanned across the image plane either by moving the object or moving the fore optic. For fluorescence detection, spectral filtering of a narrowband light illumination source is sometimes necessary to minimize the interference of the source spectrum wings with the fluorescence signal. Spectral filtering is achieved with optical interference filters and absorption glasses. This dual spectral imaging capability will enable the optimization of reflective, fluorescence, and fused datasets as well as a cost-effective design for multispectral imaging solutions. This system has been used in plant stress detection studies and in currency analysis.

Ryan, Robert E.↗
NASA NTRS2008

Nondestructive Testing As a Tool in the Space Shuttle Columbia Accident Investigation

Nondestructive testing (NDT) played a crucial role in determining the Columbia tragedy's cause. Over 84,000 pieces of debris were recovered; hundreds were subsequently subjected to NDT and materials analysis. Visual NDT of the debris revealed localized areas of damage such as erosion, excessive heating, knife edging and mechanical damage. Three-dimensional reconstructions were made of the left wing leading edge, utilizing a tripod-mounted laser scanning head and focused laser beam, and an advanced topometric optical scanner (ATOS) with digital white light to scan complex-shaped debris, producing monochrome 3-D models. Texture mapping provided a means to capture true colors of the debris and superimpose them on the scanned images. Uniform deposits were found over large portions of debris, obscuring underlying materials. To determine what was beneath, inverse radiography was enlisted. The radiographs guided investigators to where samples should be taken. To ascertain compositions, these samples were subjected to analytical testing, including energy dispersive X-ray spectroscopy and electron microprobe analysis. This combination of visual evidence, radiography, virtual reconstruction, and materials analysis allowed the forensic scientists to verify that a breach occurred in the leading edge of the left wing, the path the plasma followed, and the sequence of events that led to the loss.

McDanels, Steve↗
DOE OSTI2016

Nuclear Forensics at Los Alamos National Laboratory

Nuclear forensics assists in responding to any event where nuclear material is found outside of regulatory control; a response plan is presented and a nuclear forensics program is undergoing further development so that smugglers are sufficiently deterred.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗
DOE OSTI2022

Trace Impurities Identified as Forensic Signatures in CMX-5 Fuel Pellets Using X-ray Spectroscopic Techniques

We report that small-particle analysis is a highly promising emerging forensic tool for analysis of interdicted special nuclear materials. Integration of microstructural, morphological, compositional, and molecular impurity signatures could provide significant advancements in forensic capabilities. We have applied rapid, high-sensitivity, hard X-ray synchrotron chemical imaging to analyze impurity signatures in two differently fabricated fuel pellets from the 5th Collaborative Materials Exercise (CMX5) of the IAEA Nuclear Forensics International Working Group. The spatial distributions, chemical compositions, and morphological and molecular characteristics of impurities were evaluated using X-ray absorption near-edge structure (XANES) and X-ray fluorescence chemical imaging to discover principal impurities, their granularity, particle sizes, modes of occurrence (distinct grains vs incorporation in the UO 2 lattice), and sources and mechanisms of incorporation. Differences in UO 2+x stoichiometry were detected at the microscale in nominally identical UO 2 ceramics (CMX5-A and CMX5-B), implying the presence of multiple UO 2 host phases with characteristic microstructures and feedstock compositions. Al, Fe, Ni, W, and Zr impurities and integrated impurity signature analysis identified distinctly different pellet synthesis and processing methods. For example, two different Al, W, and Zr populations in the CMX5-B sample indicated a more complex processing history than the CMX5-A sample. K-edge XANES measurements reveal both metallic and oxide forms of Fe and Ni but with different proportions between each sample. Altogether, these observations suggest multiple sources of impurities, including fabrication (e.g., force-sieving) and feedstock (mineral oxides). This study demonstrates the potential of synchrotron techniques to integrate different signatures across length scales (angstrom to micrometer) to detect and differentiate between contrasting UO 2 fuel fabrication techniques.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

A new thorium-229 reference material

A new reference material was characterized for 229 Th molality and thorium isotope amount ratios. This reference material is intended for use in nuclear forensic analyses as an isotope dilution mass spectrometry spike. The reference material value and expanded uncertainty (k = 2) for the 229 Th molality is (1.1498 ± 0.0016)×10 -10 mol g -1 solution. The value and expanded uncertainty (k = 2) for the n( 230 Th)/n( 229 Th) ratio is (5.18 ± 0.26)×10 -5 and the n( 232 Th)/n( 229 Th) ratio is (3.815 ± 0.092)×10 -4 .

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2023

Actinide Science for Post Detonation Nuclear Forensic Analyses

Actinide and fission product separations, analyses, and solid material syntheses are key to supporting the development and testing of new nuclear forensic science technologies and for training nuclear emergency responders to effectively respond to nuclear emergency events. In this presentation, nuclear forensic scientist Dr. Mathew Snow will discuss a variety of technologies developed at Idaho National Laboratory (INL) and around the world for these applications. The presentation will include discussions of new approaches to rapid, high-efficiency chemical separations, sample preparation and analysis techniques for field-deployable actinide analyses, and techniques recently developed at INL for producing solid nuclear fallout simulant materials. An overview of the challenges confronting researchers in these area, along with possible opportunities, will also be provided.

Nuclear Forensics↗
DOE OSTI2025

Utilization of traceable standards to validate plutonium isotopic purification and separation of plutonium progeny using AG MP-1M resin for nuclear forensic investigations

Radio-chronometric studies on plutonium (Pu) materials require independent measurement of the Pu (parent) content and isotopic distribution as well as concentration and isotopic distribution of the plutonium isotopic decay products. We performed a series of experiments to demonstrate the consistency of separations using the Lewatit MP 800 macroporous anion exchange resin and the AG MP-1M resin with traceable Pu isotopic certified reference material (CRM) standards 136, 137, 138, and 126-A. Two different mesh-sizes of the AG MP-1M resin were tested and the 50–100 mesh size resin was found to work more efficiently for the separation task. Both Lewatit and AG MP-1M resins were found to perform satisfactorily for quantitatively extracting the americium (Am) and uranium (U) progeny as well as gallium (Ga) present as a tracer in the Pu material. Both resins were effective in removing isobaric interferences from the Pu fraction used in isotopic measurements by thermal ionization mass spectrometry (TIMS). To address the co-elution of uranium and gallium, Alizarin red S (ARS) was used as a colorimetric dye to determine the behavior of UO 2 2+ and Ga 3+ on AG MP-1M resin with various acidic solutions as eluents using UV–vis spectra. Poor resolution of these peaks complicated quantitative analysis by UV–vis spectroscopy, but these results were informative in planning automated separation experiments by HPLC. LA-UR-24-28919.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2018

The Development of National Nuclear Forensics Capability in ROK - 18562

According to the IAEA, each state has to build a national nuclear forensics system to determine the origin of radioactive or nuclear materials related to nuclear terrors. Based on this, the system in ROK was proposed by the Korea Institute of Nuclear Nonproliferation and Control (KINAC). The strategy for it consists of 4 TIER; legal framework, field response, library, and analysis. The legal framework for anti-terror has been systemizing and planned to extend to the nuclear respond with reflection of nuclear threat. It does not include the role and responsibility for each TIER, which impedes the progression of lower TIER. The government makes it materialized shortly with a strong will. The field of sampling and library had many progress. These were not completed, since unexplored before. However, it is possible to expect the outcome in years by active cooperation of license holders. The field of analysis has no major progress. KINAC expects rapid progress after roles are confirmed by law, because there are research laboratories specialized in nuclear material analysis. Meanwhile, the interface with the traditional forensics is in a barren land. KINAC expects there would be ignition for the traditional forensic experts by raising awareness of the nuclear forensics, such as cooperation in the council. Through these efforts, KINAC hopes to build regulatory system without loophole. In this process, the NSSC and KINAC are aware that this process is not possible with a single agency's effort, and will strive to elicit cooperation. (authors)

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗
DOE OSTI2016

Chemical and Sr isotopic characterization of North America uranium ores: Nuclear forensic applications

This study reports major, minor, and trace element data and Sr isotope ratios for 11 uranium ore (uraninite, UO 2+x ) samples and one processed uranium ore concentrate (UOC) from various U.S. deposits. The uraninite investigated represent ores formed via different modes of mineralization (e.g., high- and low-temperature) and within various geological contexts, which include magmatic pegmatites, metamorphic rocks, sandstone-hosted, and roll front deposits. In situ trace element data obtained by laser ablation-ICP-MS and bulk sample Sr isotopic ratios for uraninite samples investigated here indicate distinct signatures that are highly dependent on the mode of mineralization and host rock geology. Relative to their high-temperature counterparts, low-temperature uranium ores record high U/Th ratios (>1000), low total rare earth element (REE) abundances (<1 wt%), high contents (>300 ppm) of first row transition metals (Sc, Ti, V, Cr, Mn, Co, Ni), and radiogenic 87 Sr/ 86 Sr ratios (>0.7200). Comparison of chondrite normalized REE patterns between uraninite and corresponding processed UOC from the same locality indicates identical patterns at different absolute concentrations. Lastly, this result ultimately confirms the importance of establishing geochemical signatures of raw, uranium ore materials for attribution purposes in the forensic analysis of intercepted nuclear materials.

07 ISOTOPE AND RADIATION SOURCES↗
NASA NTRS2008

Portable Device Analyzes Rocks and Minerals

inXitu Inc., of Mountain View, California, entered into a Phase II SBIR contract with Ames Research Center to develop technologies for the next generation of scientific instruments for materials analysis. The work resulted in a sample handling system that could find a wide range of applications in research and industrial laboratories as a means to load powdered samples for analysis or process control. Potential industries include chemical, cement, inks, pharmaceutical, ceramics, and forensics. Additional applications include characterizing materials that cannot be ground to a fine size, such as explosives and research pharmaceuticals.

Source record↗
DOE OSTI2025

RIMS analysis of isotopically tagged uranium particles with application to Intentional Forensics

Traditional nuclear forensics approaches leverage isotopic measurements for characterizing nuclear forensics signatures in fuel cycle materials. To aid in provenance assessment, isotopically perturbed transition metal taggants can be added to fuel cycle materials. We present a case study for examining natural uranium oxide powder that was tagged with isotopically perturbed Mo before and after irradiation using resonance ionization mass spectrometry. In conclusion, this method accurately and precisely measures taggant and uranium compositions, rapidly enabling the ability to clearly discriminate between tagged particles and other material with application for robust assessment of material provenance.

Forensic Anthropology↗
DOE OSTI2020

Radiation-Induced Modifications in Copper Oxide Growth

Radiation-induced effects and their influence on oxidation processes were evaluated for their use as a forensic tool for special nuclear material (SNM). A beam of 10 MeV Au³⁺ ions was used to mimic the accumulation of microstructural damage from self-irradiation through the decay of radionuclides. Several copper samples were irradiated as suitable surrogate materials at 200 °C with a flux of 1x10¹² ions/cm·s to damage levels of 5, 10, and 15 displacements per atom (dpa). This corresponds to about 50, 100, and 150 years, respectively, of accumulated α-decay damage in a PuGa alloy assuming a damage rate of 0.1 dpa/year. After irradiation, all samples were exposed to an accelerated aging process induced by thermal treatment at 350 °C for 1 hour in air. This resulted in the growth of a mixed oxide layer (Cu₂O and CuO) which was characterized in detail using several complementary analytical techniques: Scanning Electron Microscopy, Raman spectroscopy, Synchrotron X-ray diffraction (transmission mode), and Grazing Incidence X-ray diffraction. The oxide layer growth of irradiated Cu at 350°C is distinctly modified as a result of the ion irradiation. Most notably, the growth of the CuO phase is suppressed with increasing radiation damage on the Cu substrate, and structural changes occurred in the Cu₂O phase. These results indicate that damage from self-irradiation over time can cause quantifiable modifications in the oxidation process of metals that could be harnessed for their use as a novel forensic tool.

36 MATERIALS SCIENCE↗