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DOE OSTI2025

Advanced Analysis of X-ray Fluorescence Measurements of the Interfacial Density of Eu Ions at Liquid–Liquid Interfaces for Solvent Back-Extraction

X-ray fluorescence near total reflection (XFNTR) is the primary technique used to measure the element-specific interfacial density of ions at liquid−liquid interfaces. Fluorescence from ions in the bulk liquids can complicate the determination of the interfacial density; consequently, measurements have been previously limited to samples without ions in the upper phase and with concentrations on the order of 10 μM or less in the lower phase. We modify the analysis of XFNTR data to account for ions in both bulk phases, then demonstrate its use in the context of rare-earth separations processes. In a model of ion stripping (i.e., back-extraction), dodecane solutions of di(2-ethylhexyl)- phosphoric acid (HDEHP) loaded with Eu(III) at the 1 mM level are placed in contact with either pure water or aqueous solutions of nitric or citric acid at pH 3. XFNTR measurements of equilibrated, quiescent samples reveal that citric acid solutions produce a disproportionately large depletion of ions from the interface compared to that from the bulk organic solution, whereas stripping by pure water or nitric acid solutions is negligible. As a result, this advance in the methodology of XFNTR may have broad applicability to the investigation of metal ions in chemical and biological processes at liquid−liquid interfaces.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2013

Reducing Contingency through Sampling at the Luckey FUSRAP Site - 13186

Typically, the greatest risk in developing accurate cost estimates for the remediation of hazardous, toxic, and radioactive waste sites is the uncertainty in the estimated volume of contaminated media requiring remediation. Efforts to address this risk in the remediation cost estimate can result in large cost contingencies that are often considered unacceptable when budgeting for site cleanups. Such was the case for the Luckey Formerly Utilized Sites Remedial Action Program (FUSRAP) site near Luckey, Ohio, which had significant uncertainty surrounding the estimated volume of site soils contaminated with radium, uranium, thorium, beryllium, and lead. Funding provided by the American Recovery and Reinvestment Act (ARRA) allowed the U.S. Army Corps of Engineers (USACE) to conduct additional environmental sampling and analysis at the Luckey Site between November 2009 and April 2010, with the objective to further delineate the horizontal and vertical extent of contaminated soils in order to reduce the uncertainty in the soil volume estimate. Investigative work included radiological, geophysical, and topographic field surveys, subsurface borings, and soil sampling. Results from the investigative sampling were used in conjunction with Argonne National Laboratory's Bayesian Approaches for Adaptive Spatial Sampling (BAASS) software to update the contaminated soil volume estimate for the site. This updated volume estimate was then used to update the project cost-to-complete estimate using the USACE Cost and Schedule Risk Analysis process, which develops cost contingencies based on project risks. An investment of $1.1 M of ARRA funds for additional investigative work resulted in a reduction of 135,000 in-situ cubic meters (177,000 in-situ cubic yards) in the estimated base volume estimate. This refinement of the estimated soil volume resulted in a $64.3 M reduction in the estimated project cost-to-complete, through a reduction in the uncertainty in the contaminated soil volume estimate and the associated contingency costs. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

From BEYONDPLANCK to COSMOGLOBE: Preliminary WMAP Q -band analysis

We present the first application of the COSMOGLOBE analysis framework by analyzing nine-year WMAP time-ordered observations that uses similar machinery to that of BEYONDPLANCK for the Planck Low Frequency Instrument (LFI). We analyzed only the Q-band (41 GHz) data and report on the low-level analysis process based on uncalibrated time-ordered data to calibrated maps. Most of the existing BEYONDPLANCK pipeline may be reused for WMAP analysis with minimal changes to the existing codebase. The main modification is the implementation of the same preconditioned biconjugate gradient mapmaker used by the WMAP team. Producing a single WMAP Q1-band sample requires 22 CPU-hrs, which is slightly more than the cost of a Planck 44 GHz sample of 17 CPU-hrs; this demonstrates that a full end-to-end Bayesian processing of the WMAP data is computationally feasible. In general, our recovered maps are very similar to the maps released by the WMAP team, although with two notable differences. In terms of temperature, we find a ~2 μK quadrupole difference that most likely is caused by different gain modeling, while in polarization we find a distinct 2.5 μK signal that has been previously referred to as poorly measured modes by the WMAP team. In the COSMOGLOBE processing, this pattern arises from temperature-to-polarization leakage from the coupling between the CMB Solar dipole, transmission imbalance, and sidelobes. No traces of this pattern are found in either the frequency map or TOD residual map, suggesting that the current processing has succeeded in modeling these poorly measured modes within the assumed parametric model by using Planck information to break the sky-synchronous degeneracies inherent in the WMAP scanning strategy.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2017

A laboratory nanoseismological study on deep-focus earthquake micromechanics

Global earthquake occurring rate displays an exponential decay down to ~300 km and then peaks around 550 to 600 km before terminating abruptly near 700 km. How fractures initiate, nucleate, and propagate at these depths remains one of the greatest puzzles in earth science, as increasing pressure inhibits fracture propagation. We report nanoseismological analysis on high-resolution acoustic emission (AE) records obtained during ruptures triggered by partial transformation from olivine to spinel in Mg 2 GeO 4 , an analog to the dominant mineral (Mg,Fe) 2 SiO 4 olivine in the upper mantle, using state-of-the-art seismological techniques, in the laboratory. AEs’ focal mechanisms, as well as their distribution in both space and time during deformation, are carefully analyzed. Microstructure analysis shows that AEs are produced by the dynamic propagation of shear bands consisting of nanograined spinel. These nanoshear bands have a near constant thickness (~100 nm) but varying lengths and self-organize during deformation. This precursory seismic process leads to ultimate macroscopic failure of the samples. Several source parameters of AE events were extracted from the recorded waveforms, allowing close tracking of event initiation, clustering, and propagation throughout the deformation/transformation process. AEs follow the Gutenberg-Richter statistics with a well-defined b value of 1.5 over three orders of moment magnitudes, suggesting that laboratory failure processes are self-affine. The seismic relation between magnitude and rupture area correctly predicts AE magnitude at millimeter scales. A rupture propagation model based on strain localization theory is proposed. Future numerical analyses may help resolve scaling issues between laboratory AE events and deep-focus earthquakes.

58 GEOSCIENCES↗

DOE OSTI2023

Data for Application of Time-Domain 1H NMR for Investigating Dynamics of Vegetative Lipids in Bioenergy Crops at Different Developmental Stages

Sweet sorghum is typically cultivated for the food and fodder market. Recently, sweet sorghum varieties are being metabolically transitioned to enhance energy density by accumulating oil droplets in their vegetative tissues for bioenergy applications. Owing to the high biomass yield of sorghum, the transgenic lines can compete with oil-seed crops for biodiesel yield per unit area. In the initial phase of transgenic development, a high-throughput phenotyping method can bridge the gap between the production pipeline and analysis to improve the efficiency of the process. To meet the requirement, the present study extends the application of time-domain 1H-NMR spectroscopy for rapid quantification and characterization of the total in-situ lipids of sweet sorghum ‘ramada’ to lay the groundwork for analyzing the upcoming large quantity of transgenic samples. NMR technology has been successfully established for analyzing lipid contents of vegetative tissues of non-transgenic variety. The multiexponential analysis of spin-lattice (T1) relaxation spectra obtained from TD-NMR aided the investigation of the dynamics of the free and bound lipid fraction with plant development. The total lipid concentration of bagasse and leaves of non-transgenic sweet sorghum remained unchanged throughout the plant development. Leaves displayed a higher percentage of bound lipids as compared to bagasse. A significant variation in the lipid concentration of juice was observed at the different growth stages with a maximum lipid accumulation of 1.21 ± 0.04% w/w at the boot stage that decreased with further maturity of the plant.

Biomass Analytics↗

DOE OSTI2022

Preservation of high-pressure volatiles in nanostructured diamond capsules

High pressure induces dramatic changes and novel phenomena in condensed volatiles(1,2) that are usually not preserved after recovery from pressure vessels. In this study we report a process that pressurizes volatiles into nanopores of type 1 glassy carbon precursors, converts glassy carbon into nanocrystalline diamond by heating and synthesizes free-standing nanostructured diamond capsules (NDCs) capable of permanently preserving volatiles at high pressures, even after release back to ambient conditions for various vacuum-based diagnostic probes including electron microscopy. As a demonstration, we perform a comprehensive study of a high-pressure argon sample preserved in NDCs. Synchrotron X-ray diffraction and high-resolution transmission electron microscopy show nanometre-sized argon crystals at around 22.0 gigapascals embedded in nanocrystalline diamond, energy-dispersive X-ray spectroscopy provides quantitative compositional analysis and electron energy-loss spectroscopy details the chemical bonding nature of high-pressure argon. The preserved pressure of the argon sample inside NDCs can be tuned by controlling NDC synthesis pressure. To test the general applicability of the NDC process, we show that high-pressure neon can also be trapped in NDCs and that type 2 glassy carbon can be used as the precursor container material. Additional experiments on other volatiles and carbon allotropes open the possibility of bringing high-pressure explorations on a par with mainstream condensed-matter investigations and applications.

36 MATERIALS SCIENCE↗

NASA NTRS2018

Potential Mercurian Analogues: Aubrite and Enstatite Chondrite Impact Melt Meteorites

The MESSENGER (MErcury Surface Space ENvironment GEochemistry and Ranging Spacecraft) mission provided new data that have helped us better constrain the surficial mineralogy and composition of Mercury. Mercury has an extremely low oxygen fugacity (f O2) (Iron Wustite (IW) -7.3 to IW -2.6), and at these unique conditions, elements, which usually exhibit lithophile behavior on Earth, can exhibit chalcophile or siderophile behavior on Mercury. No samples have been returned from Mercury; therefore, we must study candidate meteorite analogs to better understand the formation conditions of minerals inferred to be present at the Mercurian surface and Mercurian magmatic processes. In this study, we present a comprehensive analysis of a representative suite of eight aubrites and four enstatite chondrite impact melts (ECIM), which both have a similar f O2 to Mercury, and contain exotic sulfides that have been inferred to be present at the Mercurian surface. These characteristics allow us to assess their relevance for understanding the mineralogy and magmatic processes of Mercury. The ECIM were previously classified as aubrites, but we show that they are actually ECIM with a potential EH (high enstatite) parent body origin due to the presence of niningerite, Si-enriched kamacite, and uniform Ni in schreibersite. We propose that, with respect to the aubrites, the ECIM represent an ideal candidate for Mercurian studies due to their mineralogy and modal mineralogy. Compared to the aubrites, the ECIM samples do not contain forsterite or diopside, show a poorer sulfide diversity, contain graphite, and have a higher volume percentage of metal phases. Although the Mercurian surface contains forsterite and diopside, graphite and a similar amount of metal and sulfides as seen in the ECIM are inferred to be present on Mercury. According to the calculated normative Mercurian mineralogy, both candidate meteorites are most analogous to the Caloris Basin and Northern Plains Lower Mg regions.

Wilbur, Zoe E.↗

DOE OSTI2023

Mammalian Chromosome Analysis and Sorting by Flow Cytometry

The analysis of chromosomes by flow cytometry is termed flow cytogenetics, and it involves the analysis and sorting of single mitotic chromosomes in suspension. The study of flow karyograms provides insight into chromosome number and structure to provide information on chromosomal DNA content and can enable the detection of deletions, translocations, or any forms of aneuploidy. Beyond its clinical applications, flow cytogenetics greatly contributed to the Human Genome Project through the ability to sort pure populations of chromosomes for gene mapping, cloning, and the construction of DNA libraries. Maximizing the potential of these important applications of flow cytogenetics relies on precise instrument setup and optimal sample processing, both of which impact the accuracy and quality of the data that are generated. This article is a compilation of the existing protocols that describe the stepwise methodology of accumulating, isolating, and staining metaphase chromosomes to prepare single-chromosome suspensions for flow cytometric analysis and sorting. Although the chromosome preparation protocols have remained largely unchanged, cytometer technology has advanced dramatically since these protocols were originally developed. Advances in cytometry technologies offer new and exciting approaches for understanding and monitoring chromosomal aberrations, but the hallmark of these protocols remains their simplicity in methodologies and reagent requirements and the accuracy of data resolvable to every chromosome of the cell.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2013

Synthesis and magnetization studies of nanopowder Fe₇₀Ni₂₀Cr₁₀ alloys prepared by high energy milling

Nanocrystalline Fe{sub 1–x–y}Ni x Cr y (x=20, y=10% in Wt)) alloy samples were prepared by mechanical alloying process. Fe, Ni and Cr elemental powders have been ball milled in a planetary mill for various periods of time, up to 27 h. XRD analysis allowed the determination of the structure of the mixture, the average crystallite size and the lattice parameter as a function of milling time. The complete formation of FeNiCr is observed after 27 h milling. With increasing milling time from 0 to 27 h, it is observed that the lattice parameter increases from 0.3515 to 0.3593 nm as well as an increase of microstrain from 0.15 to 0.40%, whereas the grain size decreases from 48 to 13 nm. Grain morphology of the powders at different formation stages was examined using SEM. Saturation magnetization and coercive fields derived from the hysteresis curves are discussed as a function of milling time. - Graphical abstract: Fe₇₀Ni₂₀Cr₁₀ nanopowders were prepared using a planetary ball mill. The structure and microstructure vary with milling time; thereby important modifications of the magnetic properties were observed and discussed. Highlights: • Nanocrystalline Fe₇₀Ni₂₀Cr₁₀ alloy were prepared by the mechanical alloying process. • The complete formation of Fe₇₀Ni₂₀Cr₁₀ is observed after 24 h milling. • With increasing milling time, the grain size decreases, while the strain increases. • The SEM images allowed following the morphology of the materials at different stages. • M s and H C derived from the hysteresis are discussed as a function of milling time.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

The impact of spectroscopic incompleteness in direct calibration of redshift distributions for weak lensing surveys

ABSTRACT Obtaining accurate distributions of galaxy redshifts is a critical aspect of weak lensing cosmology experiments. One of the methods used to estimate and validate redshift distributions is to apply weights to a spectroscopic sample, so that their weighted photometry distribution matches the target sample. In this work, we estimate the selection bias in redshift that is introduced in this procedure. We do so by simulating the process of assembling a spectroscopic sample (including observer-assigned confidence flags) and highlight the impacts of spectroscopic target selection and redshift failures. We use the first year (Y1) weak lensing analysis in Dark Energy Survey (DES) as an example data set but the implications generalize to all similar weak lensing surveys. We find that using colour cuts that are not available to the weak lensing galaxies can introduce biases of up to Δz ∼ 0.04 in the weighted mean redshift of different redshift intervals (Δz ∼ 0.015 in the case most relevant to DES). To assess the impact of incompleteness in spectroscopic samples, we select only objects with high observer-defined confidence flags and compare the weighted mean redshift with the true mean. We find that the mean redshift of the DES Y1 weak lensing sample is typically biased at the Δz = 0.005−0.05 level after the weighting is applied. The bias we uncover can have either sign, depending on the samples and redshift interval considered. For the highest redshift bin, the bias is larger than the uncertainties in the other DES Y1 redshift calibration methods, justifying the decision of not using this method for the redshift estimations. We discuss several methods to mitigate this bias.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2025

Quantum algorithm to simulate Lindblad master equations

We present a quantum algorithm for simulating a family of Markovian master equations that can be realized through a probabilistic application of unitary channels and state preparation. Our approach employs a second-order product formula for the Lindblad master equation, achieved by decomposing the dynamics into dissipative and Hamiltonian components and replacing the dissipative segments with randomly compiled, easily implementable elements. The sampling approach eliminates the need for ancillary qubits to simulate the dissipation process and reduces the gate complexity in terms of the number of jump operators. We provide a rigorous performance analysis of the algorithm. We also extend the algorithm to time-dependent Lindblad equations, generalize the family of Markovian master equations it can be applied to, and explore applications beyond the Markovian noise model. A new error bound, in terms of the diamond norm, for second-order product formulas for time-dependent Liouvillians is provided that might be of independent interest. Published by the American Physical Society 2025

Borras, Evan (ORCID:000900017709037X)↗

DOE OSTI2013

Search for supersymmetry in pp collisions at $\sqrt{s} =7$ TeV in events with a single lepton, jets, and missing transverse momentum

Results are reported from a search for new physics processes in events containing a single isolated high-transverse-momentum lepton (electron or muon), energetic jets, and large missing transverse momentum. The analysis is based on a 4.98 fb -1 sample of proton–proton collisions at a center-of-mass energy of 7 TeV, obtained with the CMS detector at the LHC. Three separate background estimation methods, each relying primarily on control samples in the data, are applied to a range of signal regions, providing complementary approaches for estimating the background yields. The observed yields are consistent with the predicted standard model backgrounds. The results are interpreted in terms of limits on the parameter space for the constrained minimal supersymmetric extension of the standard model, as well as on cross sections for simplified models, which provide a generic description of the production and decay of new particles in specific, topology based final states.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2022

Water Imbibition and Oil Recovery in Shale: Dynamics and Mechanisms Using Integrated Centimeter-to-Nanometer-Scale Imaging

Water imbibition, and the associated oil displacement, is an important process in shale oil reservoirs after hydraulic fracturing and in water-based enhanced oil recovery (EOR). Current techniques for water imbibition measurement are mostly “black-box”-type methods. A more explicit understanding of the water imbibition/oil recovery dynamics and geological controls is in demand. In this paper, a multiscale imaging technique that covers centimeter to nanometer scale (i.e., core to pore scale), integrating neutron radiography, microcomputed tomography (micro-CT), and scanning electron microscope (SEM) is applied to investigate the water imbibition depth and rate and the cause of heterogeneity of imbibition in shale samples. The dynamic processes of water imbibition in the 1-in. (25.4-mm) core sample were explicitly demonstrated, and the imbibition along the matrix and imbibition through microfractures are distinguished through neutron radiography image analysis. The causes of observed imbibition heterogeneity were further investigated through micro-CT and SEM image analysis for 1.5-mm diameter miniplug samples from different laminas of the 1-in. core samples. Imbibition depth and rate were calculated on the basis of image analysis as well. Estimation of oil recovery through water imbibition in shale matrix was performed for an example shale field. Here this innovative and integrated multiscale imaging technique provides a “white/gray-box” method to understand water imbibition and water-oil displacement in shale. The wide span of the length scale (from centimeter to nanometer) of this technique enables a more comprehensive, accurate, and specific understanding of both the core-scale dynamics and pore-scale mechanisms of water imbibition, oil recovery, and matrix-fracture interaction.

04 OIL SHALES AND TAR SANDS↗

DOE OSTI2017

Implementation of Energy Code Controls Requirements in New Commercial Buildings

This study used a three-step process to evaluate the degree to which high-impact controls requirements included in commercial energy codes are realizing their savings potential. The three-step process included: (1) interviews of commissioning agents; (2) field audits of a sample of commercial buildings to determine how well control measures are being designed, commissioned and correctly implemented; and (3) analysis of the information gathered.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

DOE OSTI2023

Arctic Mixed-Phase Cloud Base Ice Precipitation Properties Over the NSA Site

Cloud-climate feedbacks are still the greatest source of uncertainty in current climate projections. Arctic clouds, which are predominantly stratiform and supercooled, often long-lived, and nearly continuously precipitate ice particles, contribute roughly 10% of the uncertainty attributed to the global cloud feedback. This arctic cloud uncertainty is driven by incomplete observational and theoretical knowledge required to estimate and explain the state and active processes occurring in those clouds. A focus on ice precipitation properties at arctic cloud base rather than the surface deconfounds the product of cloud condensate sink processes from the influence of the atmospheric thermodynamic state below cloud base, rendering cloud-base properties a more appealing target for inference and evaluation of model simulations. This data set provides more than 1800 samples of cloud-base ice precipitation properties over Utqiagvik, North Slope of Alaska, all of which were retrieved using the synthesis of ARM radar and lidar measurements. The retrieved ice precipitation variables in this data set include, among others, the ice number concentration, water content, PSD parameters, precipitation rate, mass-weighted fall velocity, vertical air motion, and effective radius, all of which are highly valuable for model evaluation and a general understanding of polar cloud sink processes. Each variable sample includes its mean value and associated uncertainty. Additional variables based on ARM measurements (liquid layer statistics, etc.) are included in this data set. The retrieval algorithm and analysis of this data set are described in Silber (JGR, 2023, https://doi.org/10.1029/2022JD038202).

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1971

Automatic bio-sample bacteria detection system

Electromechanical device analyzes urine specimens in 15 minutes and processes one sample per minute. Instrument utilizes bioluminescent reaction between luciferase-luciferin mixture and adenosine triphosphate (ATP) to determine number of bacteria present in the sample. Device has potential application to analysis of other body fluids.

Chappelle, E. W.↗

NASA NTRS1981

An inventory of California's irrigated land

Currently in the fourth year of its applications pilot test project to assess irrigated lands for water management, California officials found that the performance goal of plus or minus 5% at the 95% confidence level by each of the state's 10 major hydrologic basins was bettered in all but a few cases using manual analysis techniques for estimation. The process used was photointerpretation of enlarged LANDSAT scenes (1:150,000 scale), adjusting the determined acreage using a regression estimator and ground truth data from 637 sample cells. Sample cells were allocated to areas stratified on the basis of field size and selected crop types. Interpretation of three dates of imagery was required to span the complete time during which irrigated crops are grown in California. The registration of multitemporal data and classification procedures for estimating irrigated land using digital techniques are being studied as part of the second task in the project.

Sawyer, G. B.↗

NASA NTRS1984

Preparation and cleanliness verifications of a space simulation chamber for contamination sensitive test specimens

Contamination sensitive optical devices were to be evaluated under thermal vacuum conditions. Test specifications called for an extremely clean chamber environment, ambient temperature chamber walls, and optical surface temperatures at approximately - 30 C. Chamber preparation included the replacement of diffusion pumps with cryopumps and the cleaning of the chamber walls to reduce contamination levels. Chamber cleaning using vacuum bake was tried and abandoned as time consuming and ineffective. Chemical cleaning and cleanliness verification methods were developed. Gas chromatograph analysis techniques were used extensively throughout the cleaning process to verify cleanliness levels prior to evacuating the chamber. A chamber cleanliness verification test using a thermoelectric quartz crystal microbalance and witness samples was performed to demonstrate that an appropriate cleanliness level was achieved.

Koch, W. R.↗