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At least 19 records

Femto-second Laser’s Enabling New Length Scale Fabrications for Rapid Post Irradiation Examination of Materials: Concluding LDRD Project Poster

Mechanical testing campaigns are required to qualify materials for advanced reactor conditions, yet economical and safety limitations restrict the number of standardized mechanical tests that can be performed. Reducing the size of the sample is one approach to addressing these challenges and to accelerating testing. Previous research has shown that smaller mechanical test samples produce higher yield and ultimate stress values compared to values measured from standard sample sizes: the “smaller is stronger” effect. Specimens used in accelerated material testing campaigns must reflect bulk material performance to enable engineering scale material property measurement. The objective of this research project was to determine if engineering scale mechanical behavior—the yield stress—could be measured with micro-tensile test samples smaller than traditional standard testing geometries. The relationship between yield stress and sample size was explored with two different nuclear-relevant structural materials: Zircaloy-4 and tungsten. Mechanical testing of both metals demonstrated decreasing yield stress values with increasing sample gauge size across three different sizes. Yield stress values from the largest gauge size, fabricated with a femto-second laser ablation system, approach bulk material yield stress values reported in published literature. Preliminary analysis of the tungsten samples indicates the yield stress value depends on the grain characteristics within the gauge section, in addition to the gauge size. Accompanying modeling efforts, including response surface generation and crystal plasticity approaches, further demonstrated that the size of the sample gauge section alone cannot explain the change in yield stress values.

36 MATERIALS SCIENCE↗

Grain subdivision and structural modifications by high-energy heavy ions in UO 2 with different initial grain size

Irradiation with 84 MeV Xe ions at peak fluence above 7 × 10 17 ions/cm 2 has been carried out on two UO 2 samples with different initial grain sizes at 300 °C and 500 °C. Characterization of both grain structure and bubble morphology has been performed using transmission electron microscopy, image analysis and precession electron diffraction. The bubble size in the large-grained sample was smaller than that in the standard-grain sample, confirming fission gas precipitation resistance in the former. The ion irradiation in the high electronic energy deposition range has caused formation of a large density of dislocations which resulted in grain polygonization for the sample with standard grain size, which was observed in multiple lamellas extracted next to each other at peak dose. The sample with large grains showed inconsistent behavior. In one case, dislocation pile-up occurred, but no sub-grain formation was observed. An adjacent location showed sub-grain formation, even if to less extent compared to the standard grain-size sample. Furthermore, these findings suggest a limited polygonization resistance in large-grained UO 2 compared to standard-grain UO 2 . Recrystallization of both sample surfaces was present, leaving unclear if this is a surface effect or a consequence of the highest energy deposition rate in this area.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Sub-sized specimen testing and its relationship with Gen IV Materials Qualification

Renewed interest in advanced reactor technologies which can produce inherently safe, reliable, low carbon, low cost energy requires the development of new materials which can operate in the extreme environments proposed by Gen IV reactor designs. The primary focus of the Nuclear Materials Discovery and Qualification Initiative (NMDQi) is to accelerate the process by which new materials can make their way into commercial use, enabling new technologies and innovations within the nuclear sector. Due to limitations in the production of neutron irradiated material for testing and qualification, the use of specimens far smaller than those traditionally called for in regulatory codes becomes a necessity. While the use of these sub-sized specimens is necessary to achieve materials qualification on a realistic timeline and budget, literature showing the efficacy of these samples as an appropriate surrogate for ASME/ASTM defined samples is limited. This poster will detail historical efforts to compare the mechanical behavior of small geometry samples with bulk material behavior and the potential of sub-sized specimen testing at INL for future materials qualification efforts.

36 MATERIALS SCIENCE↗

Characterizing the System Impulse Response Function from Photon-Counting LiDAR Data

NASA's Multiple Altimeter Beam Experimental LiDAR (MABEL) is an aircraft-based photon-counting laser altimeter designed as a simulator to test measurement techniques and algorithms for Advanced Topographic Laser Altimeter System (ATLAS), the sole instrument on NASA's Ice, Cloud, and land Elevation Satellite-2 (ICESat-2) mission. By measuring the time of flight, pointing angle, and absolute position for individual photons, ICESat-2 provides detailed elevation measurements of earth's surface. Calculating accurate and precise elevations requires an understanding of how photons interact with surfaces, and characterization of the photon distribution after returning from surfaces. Neither MABEL nor ATLAS records the transmitted laser pulse shape, relying instead on aggregating several pulses worth of photons, often using histograms, to characterize the pulse shape. In this paper, we assess the limitations of using histograms and propose a more robust method to describe MABEL's system impulse-response function using an exponentially modified Gaussian distribution. We also provide standard error estimates for the arithmetic mean and standard deviation calculations, and for exponentially modified Gaussian parameters using a Monte Carlo sensitivity analysis. We apply this method to photon returns from a sea ice lead and from a dry salt lake bed as case studies for estimating the standard error associated with sample size for the arithmetic mean and standard deviation, and for the exponentially modified Gaussian parameters. We use these standard errors to calculate the minimum number of photons required to find both Gaussian and exponentially modified Gaussian distribution parameters within 3 cm of their parent population values.

photoncounting↗

Evolution of lunar soil grain-size and shape parameters

Substrates at the Apollo 15 and 16 sites were analyzed and showed essentially the same graphic mean, graphic standard deviation, and graphic skewness. The graphic kurtosis of Apollo 16 soils is slightly smaller than that of Apollo 15. In Apollo 15 soil samples, grain size and graphic standard deviation increase with depth, while the trend is reversed in Apollo 16 soil samples. Lower sphericity values for Apollo 15 samples coincide with concentrations of highly irregularly shaped glass particles. Two-dimensional sphericity of Apollo 15 samples is contoured as a function of particle size and depth below lunar surface. The results are consistent with an overall model for soil development in which samples closer to the surface are more mature in response to more prolonged reworking of meteorite impact.

Lindsay, J. F.↗

An Investigation into the Grain Structure of Impact Ice

To design effective anti-icing and de-icing technology for aircraft, scientists and engineers must obtain a fundamental understanding of the microstructural characteristics of impact ice. This study investigates the effects of icing parameters, such as airspeed and liquid water content (LWC), on impact ice microstructure near the interface to a metal substrate. Ice samples were accreted in the NASA Glenn Icing Research Tunnel and tested in the NASA Revolutionary Icing Materials Evaluation Laboratory. A microtome was used to shave down the ice to a thickness of < 1 mm for examination under a microscope. Samples were imaged at multiple magnifications using bright field imaging. The average grain size was determined for each sample in accordance with ASTM standard methods, and relationships between airspeed, LWC, and grain size were identified. It was observed that the average grain area in a given cross-section was linearly related to the distance of the cross-section from the metal surface. Finally, the effects of annealing and sublimation on the microstructure were also explored. Results show significant variation in the grain structure, suggesting a means by which icing condition influences adhesion strength.

grain↗

A numerical and experimental approach to compare the effect of sample thickness in small in-situ SEM and large ex-situ tensile testing in Alloy 709

ASTM standards for tensile tests define specific sample size requirements regardless of grain size of the material. However, sample size requirements for testing should be considered in conjunction with the number of grains within its reduced cross-sectional area. This is particularly important for in-situ Scanning Electron Microscope (SEM) tensile tests, as they have to be conducted on smaller samples. In this study, a comprehensive experimental and numerical evaluation of the effect of specimen thickness (and the resulting number of grains within the cross-section) were conducted using in-situ SEM tensile test (on submillimeter thick samples) and ex-situ tensile tests (on samples of 0.68–5.9 mm thickness) and the results are compared with FEM simulations outcome. All tests were conducted at room temperature and the results are correlated to the number of grains within the thickness of specimens. The tensile test results indicated that even though the 0.2% proof stress and the tensile strength do not vary for the current range of thicknesses (with number of grains in the cross-section varying from 13 to 118), a difference in necking mechanism exists. Post tensile strength, thinner samples undergo more shear failure and diagonal localized necking whereas thicker samples experience more diffuse necking indicated by decreased area of shear failure at the edges and increased area of dimpled tensile failure at the center of the sample. Further, FEM results complement the experimental findings by showing the formation of conjugated localized shear bands on the upper and lower surface in the 0.68 mm thick sample and shear bands combining to form singular shear bands in thicker samples. These results also confirm the validity of the in-situ SEM tensile tests conducted on thinner samples as long as the required minimum number of grains exist within the cross-section.

36 MATERIALS SCIENCE↗

(U)SAXS characterization of porous microstructure of chert: insights into organic matter preservation

This study characterizes the microstructure and mineralogy of 132 (ODP sample), 1000 and 1880 million-year-old chert samples. By using ultra-small-angle X-ray scattering (USAXS), wide-angle X-ray scattering and other techniques, the preservation of organic matter (OM) in these samples is studied. The scarce microstructural data reported on chert contrast with many studies addressing porosity evolution in other sedimentary rocks. The aim of this work is to solve the distribution of OM and silica in chert by characterizing samples before and after combustion to pinpoint the OM distribution inside the porous silica matrix. The samples are predominantly composed of alpha quartz and show increasing crystallite sizes up to 33 ± 5 nm (1σ standard deviation or SD). In older samples, low water abundances (~0.03%) suggest progressive dehydration. (U)SAXS data reveal a porous matrix that evolves over geological time, including, from younger to older samples, (1) a decreasing pore volume down to 1%, (2) greater pore sizes hosting OM, (3) decreasing specific surface area values from younger (9.3 ± 0.1 m 2 g -1 ) to older samples (0.63 ± 0.07 m 2 g -1 , 1σ SD) and (4) a lower background intensity correlated to decreasing hydrogen abundances. The pore-volume distributions (PVDs) show that pores ranging from 4 to 100 nm accumulate the greater volume fraction of OM. Raman data show aromatic organic clusters up to 20 nm in older samples. Raman and PVD data suggest that OM is located mostly in mesopores. Observed structural changes, silica–OM interactions and the hydro­phobicity of the OM could explain the OM preservation in chert.

(U)SAXS↗

Laboratory Investigation of the Effect of Venusian Weathering on Mineral Spectra

Introduction: The recent selection of two missions to Venus has renewed the importance of deter-mining weathering reactions between minerals and the Venusian atmosphere, and the spectral signatures of minerals before, during, and after these reactions. The rate at which weathering reactions progress also constrain show long unstable minerals will be present on the surface (e.g., [1]), and enables the use of mineralogy as a constraint on surface age(e.g., [2-3]).In order to gain an understanding of how mineral compositions and spectra change with weathering, we have begun conducting experiments in a 1 atm experimental setup at Wesleyan University. This setup exposes minerals to the temperature and most abundant gases of the Venus atmosphere (CO2, SO2, N2).We conducted initial experiments using biotite, calcite, and montmorillonite in order to test our methodology with minerals that may be relevant to recording the history of water on Venus. Methods: Experiments were conducted in Thermo Fisher Scientific Lindberg/Blue M Mini-Mite horizontal tube furnaces at Wesleyan University. Experiments used natural mineral chips and powders, and were conducted at 1 atmosphere and 460 °C under pre-mixed gases provided by Air Gas(Table 1). The furnaces are set up in a flow through configuration so that solid samples are exposed to a fixed gas composition, and quartz glass process tubes were used in all experiments (1/4” diameter for experiment V4, ½” diameter for all others). These conditions were maintained for the du-rations listed in Table 1, at which point the furnace was turned off with gas flowing until the sample was cool enough to extract under N2and be placed in a desiccator for storage. Run products were carbon coated and examined using a Hitachi SU5000 Field Emission Gun Scanning Electron Microscope (SEM) equipped with an EDAX Octane Pro EDS detector located at Wesley-an University. Visible-Near Infrared Spectroscopy (VNIR) analysis was performed on powdered samples under a nitrogen atmosphere using an ASD Fieldspec Proover the 350-2500 nm range. Powdered mineral samples were milled to a particle size of < 45μm and were spiked with an internal standard (Al2O3, corundum) to obtain quantitative mineralogy. Samples were analyzed using a Panalytical X’Pert pro X-ray Diffractometer (XRD), with an X’Celerator high speed detector and Co Kα radiation, with data collected at a step size of 0.02 ̊/minute step counting rate from 2 to 80 degrees 2θ at 45 mA/40kV in the X-ray Diffraction Laboratory located at NASA Johnson Space Center. Materials Data Inc (MDI) software suite, JadeTMv9 was used for Rietveld refinement to determine phase abundances and mineral identification by comparing XRD patterns to International Center for Diffraction Data (ICDD) database patterns. Table 1: Experimental matrix. Experiment Name Duration (Days)Gas Com-position (trace gas)MineralsV487SO2/N2(1.4%)Montmorillonite, biotiteV519SO2/N2(1.4%)CalciteV619CO2/SO2/N2(1.4% SO2, 2.1% N2)Montmorillonite, biotiteV828SO2/N2(1.4%)Biotite, calcite Results: Calcite. In both experiments, calcite was exposed to the SO2/N2gas mixture, and in both experimental run products, XRD analysis detected anhydrite, which is consistent with EDS measurements conducted in the SEM. The XRD analyses show greater amounts of anhydrite present after 28 days than 19, suggesting the calcite reaction progressed further given longer duration. Grain surface morphology as seen in the SEM also shows secondary mineral growth (Fig. 1). VNIR spectra show no change, as expected since anhydrite lacks spectral features in this wavelength range. Montmorillonite. Montmorillonite was exposed to two different gas mixtures, the SO2/N2mix and CO2/SO2/N2mix over different durations (87 and 19 days, respectively). VNIR analyses of both run products show a reduction in the 1441and1910 nm water features as well as a shift of the 1411 and 2011 nm features to shorter wavelengths that may indicate re-structuring in the crystal lattice and the production of amorphous phases [4]. XRD results are consistent with this, showing a shift of the 001 peak from 15Åto 10Åin both run products. The amount of X-ray amorphous material in the montmorillonite run products was greater than that present in the unreacted clay, being the greatest in the 87 day V4 experiment. No other secondary phases were detected in the run products, however sulfur was present in EDS analyses of powder samples.

A R Santos↗

Active Galactic Nuclei Continuum Reverberation Mapping Based on Zwicky Transient Facility Light Curves

We perform a systematic survey of active galactic nuclei (AGNs) continuum lags using ~3 days cadence gri-band light curves from the Zwicky Transient Facility. We select a sample of 94 type 1 AGNs at z < 0.8 with significant and consistent inter-band lags based on the interpolated cross-correlation function method and the Bayesian method JAVELIN. Within the framework of the "lamp-post" reprocessing model, our findings are: (1) The continuum emission (CE) sizes inferred from the data are larger than the disk sizes predicted by the standard thin-disk model. (2) For a subset of the sample, the CE size exceeds the theoretical limit of the self-gravity radius (12 lt-days) for geometrically thin disks. (3) The CE size scales with continuum luminosity as R CE ∝ L 0.48±0.04 with a scatter of 0.2 dex, analogous to the well-known radius–luminosity relation of broad Hβ. These findings suggest a significant contribution of diffuse continuum emission from the broad-line region (BLR) to AGN continuum lags. We find that the R CE –L relation can be explained by a photoionization model that assumes ~23% of the total flux comes from the diffuse BLR emission. In addition, the ratio of the CE size and model-predicted disk size anticorrelates with the continuum luminosity, which is indicative of a potential nondisk BLR lag contribution evolving with the luminosity. Finally, a robust positive correlation between the CE size and black hole mass is detected.

79 ASTRONOMY AND ASTROPHYSICS↗

Apollo 16: Core 60004 - Preliminary study of less than 1 mm fines

The article studies the possible variation of mineralogy as a function of both grain size and depth within the core of less than 1 mm fines, for the core section 60004 from Apollo 16. Twelve samples of the fines were dry sieved. The grain size analysis showed a bimodal distribution for all samples, indicating a competing process of grain size degeneration and agglutinate formation. Approximately 99% of the minerals in the samples examined consisted of plagioclase feldspar, pyroxene and olivine, with plagioclase the dominant phase. The various minerals were analyzed, using standard electron microprobe techniques, as a function of size range for each sample, and the representative analyses are presented. Several types of glass were also analyzed, ranging in color from orange through yellow and green to colorless. The investigation of the chemical variations of mineral and lithic clasts from the top and the bottom of the core suggests that although minor variations are present, the regolith was derived from fairly homogeneous sources.

Meyer, H. O. A.↗

Variance-Reduced Accelerated First-Order Methods: Central Limit Theorems and Confidence Statements

In this paper, we consider a strongly convex stochastic optimization problem and propose three classes of variable sample-size stochastic first-order methods: (i) the standard stochastic gradient descent method, (ii) its accelerated variant, and (iii) the stochastic heavy-ball method. In each scheme, the exact gradients are approximated by averaging across an increasing batch size of sampled gradients. We prove that when the sample size increases at a geometric rate, the generated estimates converge in mean to the optimal solution at an analogous geometric rate for schemes (i)–(iii). Based on this result, we provide central limit statements, whereby it is shown that the rescaled estimation errors converge in distribution to a normal distribution with the associated covariance matrix dependent on the Hessian matrix, the covariance of the gradient noise, and the step length. If the sample size increases at a polynomial rate, we show that the estimation errors decay at a corresponding polynomial rate and establish the associated central limit theorems (CLTs). Under certain conditions, we discuss how both the algorithms and the associated limit theorems may be extended to constrained and nonsmooth regimes. As a result, we provide an avenue to construct confidence regions for the optimal solution based on the established CLTs and test the theoretical findings on a stochastic parameter estimation problem.

Lei, Jinlong↗

Application of Scanning-Imaging X-Ray Microscopy to Fluid Inclusion Candidates in Carbonates of Carbonaceous Chondrites

In order to search for such fluid inclusions in carbonaceous chondrites, a nondestructive technique using x-ray micro-absorption tomography combined with FIB sampling was developed and applied to a carbonaceous chondrite. They found fluid inclusion candidates in calcite grains, which were formed by aqueous alteration. However, they could not determine whether they are really aqueous fluids or merely voids. Phase and absorption contrast images can be simultaneously obtained in 3D by using scanning-imaging x-ray microscopy (SIXM). In refractive index, n=1-sigma+i(beta), in the real part, 1-sigma is the refractive index with decrement, sigma, which is nearly proportional to the density, and the imaginary part, beta, is the extinction coefficient, which is related to the liner attenuation coefficient, mu. Many phases, including water and organic materials as well as minerals, can be identified by SIXM, and this technique has potential availability for Hayabusa-2 sample analysis too. In this study, we examined quantitative performance of d and m values and the spatial resolution in SIXM by using standard materials, and applied this technique to carbonaceous chondrite samples. We used POM ([CH2O]n), silicon, quartz, forsterite, corundum, magnetite and nickel as standard materials for examining the sigma and mu values. A fluid inclusion in terrestrial quartz and bi-valve shell (Atrina vexillum), which are composed of calcite and organic layers with different thickness, were also used for examining the spatial resolution. The Ivuna (CI) and Sutter's Mill (CM) meteorites were used as carbonaceous chondrite samples. Rod- or cube-shaped samples 20-30 micron in size were extracted by using FIB from cross-sectional surfaces of the standard materials or polished thin sections of the chondrites, which was previously observed with SEM. Then, the sample was attached to a thin W-needle and imaged by SIXM system at beamline BL47XU, SPring-8, Japan. The slice thickness was 109.3 nm and the pixel size was mostly 100 nm.

Tsuchiyama, Akira↗

Introducing the embedded random phase approximation: H 2 dissociative adsorption on Cu(111) as an exemplar

The random phase approximation (RPA) as a means of treating electron correlation recently has been shown to outperform standard density functional theory (DFT) approximations in a variety of cases. However, the computational cost of the RPA is substantially more than DFT, especially when aiming to study extended surfaces. Properly accounting for sufficient surface ensemble size, Brillouin zone sampling, and vacuum separation of periodic images in standard periodic-planewave-based DFT code raises the cost to achieve converged results. Here, we show that sub-system embedding schemes enable use of the RPA for modeling heterogeneous reactions at reduced computational cost. Further, we explore two different embedded RPA (emb-RPA) approaches, periodic emb-RPA and cluster emb-RPA. We use the (experimentally and theoretically) well-studied H 2 dissociative adsorption on Cu(111) as our exemplar, and first perform full periodic RPA calculations as a benchmark. The full RPA results match well the semi-empirical barrier fit to experimental observables and others derived from high-level computations, e.g., from recent embedded n-electron valence second order perturbation theory [Zhao et al., J. Chem. Theory Comput. 16(11), 7078–7088 (2020)] and quantum Monte Carlo [Doblhoff-Dier et al., J. Chem. Theory Comput. 13(7), 3208–3219 (2017)] simulations. Among the two emb-RPA approaches tested, the cluster emb-RPA accurately reproduces the energy profile (maximum error of 50 meV along the reaction pathway) while reducing the computational cost by approximately two orders of magnitude. We therefore expect that the embedded cluster approach will enable wider RPA implementation in heterogeneous catalysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The effect of sample holder material on ion mobility spectrometry reproducibility

When a positive detection of a narcotic occurs during the search of a vessel, a decision has to be made whether further intensive search is warranted. This decision is based in part on the results of a second sample collected from the same area. Therefore, the reproducibility of both sampling and instrumental analysis is critical in terms of justifying an in depth search. As reported at the 2nd Annual IMS Conference in Quebec City, the U.S. Coast Guard has determined that when paper is utilized as the sample desorption medium for the Barringer IONSCAN, the analytical results using standard reference samples are reproducible. A study was conducted utilizing papers of varying pore sizes and comparing their performance as a desorption material relative to the standard Barringer 50 micron Teflon. Nominal pore sizes ranged from 30 microns down to 2 microns. Results indicate that there is some peak instability in the first two to three windows during the analysis. The severity of the instability was observed to increase as the pore size of the paper is decreased. However, the observed peak instability does not create a situation that results in a decreased reliability or reproducibility in the analytical result.

Jadamec, J. Richard↗

Modular Design of High Temperature and Pressure Heat Exchangers Using 3D Printing

Functionally graded material (FGM), leveraged by latest additive manufacturing (AM) technologies, can add significant values to high temperature applications such as the HTR in supercritical sCO2 Brayton cycles. The project was focused on fabricating FGMs with complex geometries such as flow channels using DED and L-PBF technologies to support the modular design concept in achieving high-performance and low-cost high temperature recuperators for the sCO2 Brayton cycle. Samples printed from the base materials including both SS 316 and Inconel 625 have mostly met the material standards. L-PBF samples have achieved the fine feature sizes with good geometrical accuracy. In addition, DED has demonstrated its printability on LPBF part with both direct transition and using 50/50 mixed powders. Despite various challenging, the project helped advance the current state-of-the-art of DED technology in terms of printing fine geometries.

14 SOLAR ENERGY↗

Porosity and Permeability of Chondritic Materials

We have investigated the porosity of a large number of chondritic interplanetary dust particles and meteorites by three techniques: standard liquid/gas flow techniques, a new, non-invasive ultrasonic technique, and image processing of backscattered images . The latter technique is obviously best suited to sub-kg sized samples. We have also measured the gas and liquid permeabilities of some chondrites by two techniques: standard liquid/gas flow techniques, and a new, non-destructive pressure release technique. We find that chondritic IDP's have a somewhat bimodal porosity distribution. Peaks are present at 0 and 4% porosity; a tail then extends to 53%. These values suggest IDP bulk densities of 1.1 to 3.3 g/cc. Type 1-3 chondrite matrix porosities range up to 30%, with a peak at 2%. The bulk porosities for type 1-3 chondrites have the same approximate range as exhibited by matrix, indicating that other components of the bulk meteorites (including chondrules and aggregates) have the same average porosity as matrix. These results reveal that the porosity of primitive materials at scales ranging from nanogram to kilogram are similar, implying similar accretion dynamics operated through 12 orders of size magnitude. Permeabilities of the investigated chondrites vary by several orders of magnitude, and there appears to be no simple dependence of permeability with degree of aqueous alteration, or chondrite type.

Zolensky, Michael E.↗

Understanding Biases in Sample Preparation Techniques for Coupled Scanning Electron Microscopy and MAMA PuO 2 Morphological Analysis

In this project, the scanning electron microscopy (SEM) sampling method used during the statistical design study (SDS) was investigated to determine if any sampling biases were present in the analyzed data. Using standard particle size distribution powders from the National Institute of Standards and Technology (NIST 1984 standard reference material) with the origin wet dispersion method, it was determined that a bias to smaller particles was present. This was supported by theoretical calculations using Stokes’ law to determine the settling rate of spherical particles of roughly the same size and mass as those found in the SDS. Based on the theoretical calculations, it was determined that the settling rate for each of the 76 powder sets in the SDS could be unique based on specific particle shape and mass distributions, making a universal correction factor/formula not applicable. Therefore, priority shifted to developing an improved wet dispersion method that significantly reduced the particle settling rate for all particle size and shapes. This was achieved by replacing the original solvent (isopropyl alcohol) with a heavy liquid (lithium heteropolytungstates), which dramatically slowed the settling rate and allowed for the capture of a suitable homogeneous aliquot. SEM imaging and Morphological Analysis for Material Attribution (MAMA) software analysis were conducted on the NIST standard, and the SEM/MAMA data were compared to data captured by a dynamic image analysis particle size analyzer. The resulting data confirmed that the new wet dispersion method does indeed deliver an improved representative aliquot to the SEM stub. For instance, in the NIST certificate, the average particle size is ~17.1 µm ± 2.2 µm with a normal distribution. The initial wet dispersion method resulted in a drastically reduced average particle size of 6.1 µm in addition to a non-representative heavy bi-modal distribution whereas the improved LST wet dispersion method resulting in an average particle size that was much closer to the NIST certificate (12.7 µm) with a similar normal distribution. Although the improved method was still short of the NIST certificate average, atomic force microscopy analysis determined that the resulting ~20-25% reduction in size was due to particles sinking into the carbon sticky tape used for SEM imaging. It is believed that that this bias can be calibrated in a much more predicable manner than the original settling rate bias. In addition, the matching normal distribution curves between the NIST certificate and the heavy liquid method indicate a much-improved representative aliquot has been sampled and imaged. A surrogate CeO 2 powder was used to reflect PuO 2 more accurately and to aid in implementing radiological controls and shielding. The resulting data sets from the SEM/MAMA method and the particle size analyzer give almost identical average particle sizes and particle distribution statistics. Future work will re-analyze several select runs from the SDS to determine if morphological signatures can be found with the improved sampling method.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗