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DOE OSTI2021

Temporally and spatially resolved X-ray densitometry in a shock tube

Gas densities were measured by x-ray absorption spectroscopy to examine spatial inhomogeneity in density behind incident and reflected shock waves in a miniature (12.7 mm bore) high repetition rate shock tube. Shock waves were generated in argon. The pressure and temperature behind the incident shock were P 2 ~ 1.72 bar and T 2 ~ 800 K, while those behind the reflected shock were P 5 ~ 6.5 bar and T 5 ~ 1480 K. Time-resolved line-of-sight transmission measurements using x-rays at 9 keV photon energy were made along various axial and transverse locations covering the entire shock tube cross section. The x-ray transmission at each location was converted to pathlength-integrated densities, which in some conditions could be further converted to pathlength-averaged densities. The measured gas densities were compared with those calculated by the normal shock wave relations, and good agreement was found in the preshock and immediately behind the incident shock regions. Similar agreement was found for reflected shock conditions very near the endwall. However, increasingly large differences between the measured and calculated gas densities were found as distance from the endwall increased. Furthermore, reconstruction by Abel inversion allowed time and radially resolved densities to be obtained from the transverse measurements. While the profiles measured in this experiment are of insufficient signal-to noise level and resolution to definitively assign boundary layer thicknesses, future improvements may be able to do this. The radially resolved densities reveal growing sidewall thermal boundary layers in gases behind the reflected shock. These reconstructions were compared with a model of the thermal boundary layer and are consistent with values of the thermal boundary layer thickness being between 0.25 mm and 1 mm at 0.7 ms after shock reflection.

42 ENGINEERING↗

DOE OSTI2014

The structural organization of N-methyl-2-pyrrolidone + water mixtures: A densitometry, x-ray diffraction, and molecular dynamics study

A combined approach of molecular dynamics simulations, wide angle X-ray scattering experiments, and density measurements was employed to study the structural properties of N-methyl-2-pyrrolidone (NMP) + water mixtures over the whole concentration range. Remarkably, a very good agreement between computed and experimental densities and diffraction patterns was achieved, especially if the effect of the mixture composition on NMP charges is taken into account. Analysis of the intermolecular organization, as revealed by the radial and spatial distribution functions of relevant solvent atoms, nicely explained the density maximum observed experimentally.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Integration of conductivity probe with optical and x-ray imaging systems for local air–water two-phase flow measurement

Various techniques have been developed in the past to measure different parameters in two-phase flow. Among them, the multi-sensor conductivity probe is one of the most commonly used techniques because of its good overall performance. Recently, more advanced techniques such as high speed optical imaging and fast X-ray densitometry become mature and easily accessible. The main objective of this work is to compare and integrate these different techniques, to achieve a more accurate and complete measurement of two-phase flow. In this study, a double-sensor conductivity probe is used to measure the local time-averaged parameters along the radial direction of a 2.54 cm ID round pipe. An X-ray densitometry system is used to measure the chordal averaged void fraction and gas velocity. A high speed camera system is employed to provide the visualization of the two-phase flow structure and obtain the line-averaged gas velocity. The unique advantages and main uncertainties of these three techniques are analyzed by considering their measuring principles and possible issues in practical measurements. From this, a method is developed to integrate the data obtained by the optical and X-ray systems into the probe signal processing. Finally, a better accuracy could be achieved using this method for various local two-phase flow parameters including void fraction, bubble velocity and superficial gas velocity, compared to the original probe measurements.

42 ENGINEERING↗

DOE OSTI2020

Development of a Comprehensive Two-Phase Flow Database for the Validation of NEK-2P

Three-dimensional (3-D) two-phase Computational Fluid Dynamics (CFD) codes are emerging as a powerful and potentially practical tool for applications in which detailed local flow information is needed. However, two-phase flow models and associated closure relations are not well established for CFD applications, which is partly due to the lack of high-quality validation data. The main objective of this work is to develop a comprehensive database of two-phase flows that can be used to validate two-phase CFD codes such as NEK-2P. In this project, four advanced local measurement systems, including Particle Image Velocimetry and Planar Laser-Induced Fluorescence (PIV-PLIF), high-speed imaging, x-ray densitometry, and multi-sensor conductivity probe are employed to measure the local two-phase flow parameters of both gas and liquid phases. By combining these techniques, the local void fraction, bubble velocity, interfacial area concentration, bubble frequency, liquid velocity, turbulence intensity, etc., in various two-phase flow regimes can be obtained. These local measurement techniques are first used in a 25.4 mm circular pipe test section. Seven air-water two-phase flow conditions spanning the bubbly, slug, churn-turbulent, and annular flow regimes are measured in this facility. The obtained database contains the radial profiles of both gas- and liquid-phase parameters at three axial locations along the test section. The second facility used in this work contains a 30 mm × 10 mm rectangular test section, in which three two-phase flow and two single-phase flow conditions are measured. Two-dimensional distributions of local two-phase flow parameters in the cross-sectional plane are measured in this facility at three axial locations as well. A facility featuring a 3×3 electrically heated rod bundle is also designed and being constructed in this project. This facility is specially designed for optical measurements and is expected to provide high-quality boiling data in the future. Preliminary analyses have been performed for the data taken in the 25.4 mm circular pipe. Both center-peaked and wall-peaked void fraction profiles have been observed in the data depending on the two-phase flow conditions and/or developing lengths. The 1-D drift-flux model was evaluated with the newly obtained datasets, in which both gas- and liquid-phases data were directly measured. The distribution parameter model has been optimized based on a new void-profile classification method proposed in this study. The optimized drift-flux model shows a significant improvement in predicting both gas velocity and void fraction. The measured liquid-phase turbulence was used to benchmark Sato’s turbulence model considering the bubble-induced shear stress for the three tested bubbly flows. The benchmark results showed good agreement between the PIV measurements and model predictions. In the bubbly flows tested that have low void fractions less than 3%, the effect of the bubble-induced turbulence was found not significant. However, the bubble-induced shear stress becomes important with the increase of the void fraction. The Conjugate Heat Transfer (CHT) model was developed and implemented in NEK-2P. This model allows the coupled simulation of the solid domain and two-phase fluid domain, allowing the specification of realistic boundary conditions. The CHT implementation was verified first with non-boiling simulations. The predicted temperatures in the fluid domain were shown to be identical in simulations with or without the CHT model. The CHT model was then validated through simulations of three Becker benchmark CHF tests performed under both Dryout (DO) and Departure from Nucleate Boiling (DNB) conditions. Reasonably good agreement was obtained between calculated wall temperatures and corresponding experimental data.

42 ENGINEERING↗

DOE OSTI2016

Trace metal analysis by laser ablation-inductively coupled plasmamass spectrometry and x-ray K-edge densitometry of forensic samples

This dissertation describes a variety of studies on the determination of trace elements in samples with forensic importance. Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) was used to determine the trace element composition of numerous lipstick samples. Lipstick samples were determined to be homogeneous. Most lipstick samples of similar colors were readily distinguishable at a 95% confidence interval based on trace element composition. Numerous strands of a multi-strand speaker cable were analyzed by LA-ICP-MS. The strands in this study are spatially heterogeneous in trace element composition. In actual forensic applications, the possibility of spatial heterogeneity must be considered, especially in cases where only small samples (e.g., copper wire fragments after an explosion) are available. The effects of many unpredictable variables, such as weather, temperature, and human activity, on the retention of gunshot residue (GSR) around projectile wounds were assessed with LAICP- MS. Skin samples around gunshot and stab wounds and larvae feeding in and around the wounds on decomposing pig carcasses were analyzed for elements consistent with GSR (Sb, Pb, Ba, and Cu). These elements were detected at higher levels in skin and larvae samples around the gunshot wounds compared to the stab wounds for an extended period of time throughout decomposition in both a winter and summer study. After decomposition, radiographic images of the pig bones containing possible damage from bullets revealed metallic particles embedded within a number of bones. Metallic particles within the bones were analyzed with x-ray, K-edge densitometry and determined to contain lead, indicating that bullet residue can be retained throughout decomposition and detected within bones containing projectile trauma.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

Application of Hybrid K-Edge Densitometry in Reprocessing Facilities

During reprocessing operations, accurately determining the elemental concentrations of uranium and plutonium is critical for nuclear security. Reprocessing facilities processes hundreds of tons of nuclear material annually, requiring accurate measurements to ensure effective nuclear material control and accountability. Hybrid K-edge densitometry (HKED) system combines K-edge absorption densitometry with x-ray fluorescence to measure actinide elemental concentrations with a low uncertainty. This system uses high-purity germanium gamma-ray detectors and advanced signal processing equipment to detect x-ray accurately. This document provides guidance on how to achieve effective performance from an HKED system for measuring uranium and plutonium concentrations in reprocessing facilities. It includes best practices for the setup and operation of an HKED system, while highlighting factors influencing uncertainties.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Fabrication of Ta-Reinforced Cu-Based Bulk Metallic Glass Composites by High-Pressure Torsion

Ex situ Cu{sub 54}Zr{sub 22}Ti{sub 18}Ni{sub 6} matrix bulk metallic glass composites (BMGCs) reinforced with Ta particles (10–30 vol.%) were fabricated by high-pressure torsion (HPT) under applied pressure of 6 GPa for 1–3 turns at temperatures of 25 or 200 °C. The densification, structure, thermal, and mechanical properties of BMGC samples were investigated by Archimedes densitometry, optical microscopy, x-ray diffraction, differential scanning calorimetry, small punch test, and microhardness measurements. Near full-density BMGC disks (relative densities higher than 0.97) are fabricated using HPT, irrespective of the processing strain and temperature. The microhardness of BMGCs is improved by increasing the number of turns, or the processing temperature due to the improvement in the deformation degree of both the amorphous and Ta particles as well as the reduction in the interlayer spacing of Ta particles. Nevertheless, there is an optimal amount of Ta which gives rise to the peak hardness in the BMGC samples, depending on the amount of imposed strain during HPT. The results of small punch test indicate that the addition of Ta to the monolithic BMG and increasing the HPT temperature significantly enhance the fracture load and deflection.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Performance evaluation of the ORNL multi-elemental XRF analysis algorithms

Hybrid K-Edge Densitometer (HKED) systems integrate both K-Edge Densitometry (KED) and X-Ray Fluorescence (XRF) analyses to provide accurate rapid, assay results of the uranium and plutonium content of dissolver solution samples from nuclear fuel reprocessing facilities. Introduced for international safeguards applications in the late 1980s, the XRF component of the hybrid analyses is limited to quantification of U and Pu over a narrow range of U:Pu concentration ratios in the vicinity of ≈100. The analysis was further limited regarding the presence of minor actinide components where only a single minor actinide (typically Am) is included in the analysis and then only treated as an interference. The evolving nuclear fuel cycle has created the need to assay more complex dissolver solutions where uranium may no longer be the dominant actinide in the solution and the concentrations of the so called minor actinides (e.g., Th, Np, Am, and Cm) are sufficiently high that they can no longer be treated as impurities and ignored. Extension of the traditional HKED Region of Interest (ROI) based analysis to include these additional actinides is not possible due to the increased complexity of the XRF spectra. Oak Ridge National Laboratory (ORNL) has developed a spectral fitting approach to the HKED XRF measurement with an enhanced algorithm set to accommodate these complex XRF spectra. This report provides a summary of the spectral fitting methodology and examines the performance of these algorithms using data obtained from the ORNL HKED system, as well as data provided by the International Atomic Energy Agency (IAEA) on actual dissolver solutions.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2015

Integrated X-ray detection system for determination of nuclear material concentration

An integrated system of X-ray Absorption Spectrometry (XAS), also called L-edge densitometry for uranium (LED) and X-ray Fluorescence spectrometry (XRF) is designed using Monte Carlo simulation for determining concentration of uranium and minor actinides for safeguard. The system can be useful to determination uranium and minor actinide, such as plutonium, neptunium, and etc., concurrently. The equipment is compact compared to the K-edge densitometer with high purity germanium detector which needs liquid nitrogen cooling since a low energy X-ray source is used. The system has been validated from simulation and analysis of the transmitted and reflected spectrum. The concentrations of nuclear material samples are obtained from this study. (authors)

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2022

Synchrotron X-ray based particle image velocimetry to measure multiphase streamflow and densitometry

Synchrotron-based radiation techniques are increasingly used in the field of flow condition measurements. As a complicated multiphase flow, cavitation has been investigated in a wide variety of industrial fields, to prevent damages on spillways at large dams or intensify the bacteria eradication rate during water treatments. To control the detrimental effects of cavitating flows, the dynamics of and mechanisms affecting cavitation development shall be visualized and identified in real-time. Due to the large reflection and scattering effects of multiphase flow, standard visible-light imaging technologies cannot penetrate vapor bubbles and provide extremely limited information. In this study, the synchrotron source emitted high-flux X-ray pulses are used to capture flow motion and visualize internal structures with sufficiently high spatial and temporal resolutions. The image processing procedures on raw x-ray images are developed using 2D Fourier transform (FT) and wavelet transform (WT) to implement the contrast enhancement and de-noising. Through the edge detection algorithm, tracking either seeded particles or phase interfaces inside the opaque multiphase flow can be achieved to perform the particle image velocimetry. Further, with decomposing particle-only and particle-eliminated subplots from the X-ray phase-contrast image, the time-resolved velocity and void fraction fields are obtained simultaneously, paving a way for further flow condition analysis such as densitometry.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2019

A Self-Irradiation Correction for the Hybrid K-Edge Densitometer

Hybrid x-ray fluorescence and K-edge densitometry is used at nuclear fuel reprocessing facilities to determine the concentrations of uranium and plutonium in the input accountability vessel. The uranium concentration is determined by K-edge densitometry, that is, from the step-difference in transmission on either side of the K-absorption edge measured using a continuous x-ray spectrum on a vial of the solution defining a well-known geometry. Historically this was done using a basic region of interest analysis but recently to accommodate more challenging solution full spectral analysis has been developed with considerable benefits. In parallel with the transmission measurement, the relative plutonium-to-uranium concentration is obtained from the relative strength of the x-ray–induced K-shell x-ray fluorescence production measured at a backward angle in energy-dispersive mode. However, gamma-ray emissions from fission products present in the solution also cause fluorescence of the characteristic actinide x-rays. Uncorrected, these self-irradiation–induced x-rays can introduce a bias into the reported U:Pu result. The commonly implemented method to correct this interference requires acquisition of a long (~8 hour) passive spectra for the sample. Although effective, it is often impractical to perform a passive measurement on every sample such that a representative passive spectrum is used. We have developed an alternative correction methodology using only the active x-ray fluorescence spectrum that eliminates the requirement for the time-consuming passive count. The active self-interrogation methodology will be discussed and initial performance results presented.

Mcelroy Jr, Robert↗

DOE OSTI2012

Condensation of Self-Assembled Lyotropic Chromonic Liquid Crystal Sunset Yellow in Aqueous Solutions Crowded with Polyethylene Glycol and Doped with Salt

We use optical and fluorescence microscopy, densitometry, cryo-transmission electron microscopy (cryo-TEM), spectroscopy, and synchrotron X-ray scattering to study the phase behavior of the reversible self-assembled chromonic aggregates of an anionic dye Sunset Yellow (SSY) in aqueous solutions crowded with an electrically neutral polymer polyethylene glycol (PEG) and doped with the salt NaCl. PEG causes the isotropic SSY solutions to condense into a liquid-crystalline region with a high concentration of SSY aggregates, coexisting with a PEG-rich isotropic (I) region. PEG added to the homogeneous nematic (N) phase causes separation into the coexisting N and I domains; the SSY concentration in the N domains is higher than the original concentration of PEG-free N phase. Finally, addition of PEG to the highly concentrated homogeneous N phase causes separation into the coexisting columnar hexagonal (C) phase and I phase. This behavior can be qualitatively explained by the depletion (excluded volume) effects that act at two different levels: at the level of aggregate assembly from monomers and short aggregates and at the level of interaggregate packing. We also show a strong effect of a monovalent salt NaCl on phase diagrams that is different for high and low concentrations of SSY. Upon the addition of salt, dilute I solutions of SSY show appearance of the condensed N domains, but the highly concentrated C phase transforms into a coexisting I and N domains. We suggest that the salt-induced screening of electric charges at the surface of chromonic aggregates leads to two different effects: (a) increase of the scission energy and the contour length of aggregates and (b) decrease of the persistence length of SSY aggregates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2012

Systems Analysis of hiRX for Improved Reprocessing Safeguards

The goal of this work was to examine the potential safeguards improvement of the High Resolution X-ray (hiRX) technology for aqueous reprocessing plants. Existing plants utilize KEdge and Hybrid K-Edge Densitometry for routine accountancy measurements for the key input and output accountability tanks. The IAEA also use these technologies for verification measurements. The hiRX technology has the potential to significantly reduce the measurement uncertainty with an equally simple but less costly instrument that uses a much smaller sample size. Such a technology could be highly desirable for both the operator and inspector. This work utilizes a Separations and Safeguards Performance Model of a PUREX reprocessing plant to determine the safeguards improvement offered by the reduced measurement uncertainty of hiRX. Results show that a significant improvement in the ability to detect a protracted diversion may be possible.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2020

Molecular Structure of Sphingomyelin in Fluid Phase Bilayers Determined by the Joint Analysis of Small-Angle Neutron and X-ray Scattering Data

In this work, we have determined the fluid bilayer structure of palmitoyl sphingomyelin (PSM) and stearoyl sphingomyelin (SSM) by simultaneously analyzing small-angle neutron and X-ray scattering data. Using a newly developed scattering density profile (SDP) model for sphingomyelin lipids, we report structural parameters including the area per lipid, total bilayer thickness, and hydrocarbon thickness, in addition to lipid volumes determined by densitometry. Unconstrained all-atom simulations of PSM bilayers at 55 °C using the C36 CHARMM force field produced a lipid area of 56 Å 2 , a value that is 10% lower than the one determined experimentally by SDP analysis (61.9 Å2). Furthermore, scattering form factors calculated from the unconstrained simulations were in poor agreement with experimental form factors, even though segmental order parameter (S CD ) profiles calculated from the simulations were in relatively good agreement with S CD profiles obtained from NMR experiments. Conversely, constrained area simulations at 61.9 Å 2 resulted in good agreement between the simulation and experimental scattering form factors, but not with S CD profiles from NMR. We discuss possible reasons for the discrepancies between these two types of data that are frequently used as validation metrics for molecular dynamics force fields.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Quantifying uncertainty in uranium concentration measurements via K-edge densitometry

This study quantifies the uncertainty in uranium concentration predictions of fluoride and chloride-based salts within a steel pipe using K-edge densitometry. Modeling and simulation was conducted with the Monte Carlo N-Particle Transport (MCNP) code. The quality of of this technique’s prediction in a pipe requires proper characterization of the pipe’s thickness, which is dependent on the source size and axial offset from the pipe centerline. The thickness was determined as either the center-line thickness seen by the X-ray source or an average value determined through random sampling. Generally, the predicted concentrations were slightly better at lower offset with the random sampling thickness and using the center-line thickness for the highest offsets. For a line-beam source and varying axial offsets, the relative error of concentration was within 1% of the true value but uncertainty increased by 2 orders of magnitude. Similarly, for no axial offset, the relative error was significantly less than 1% while no trend for uncertainty was found. However, at the largest possible offset for a given source size, the concentrations become erroneous and greater than the allowable 1% relative error. Furthermore, high offsets tended to increase the variance of the transmission spectra by 3 orders of magnitude.

Characterization and Analytical Technique↗