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DOE OSTI2022

IER-501 CED-3b: Experiment Execution Summary for the Pulsed-Neutron Die-Away Experimental Testbed for Thermal Scattering Law Benchmarks (PNDA)

This report summarizes the experiments done for IER-501, a testbed for pulsed-neutron die-away (PNDA) experiments at Lawrence Livermore National Laboratory (LLNL). The PNDA experiments were conducted in two separate two-day campaigns: one campaign for high-density polyethylene and another for Lucite. All experiments were performed at Lawrence Livermore Laboratory. They will become high-quality benchmarks that serve to optimize and validate thermal neutron scattering laws (TSLs), which are high priority nuclear data for the Department of Energy’s Nuclear Criticality Safety Program (NCSP). The report presents the PNDA design and its equipment, and it documents the experimental die-away curves. It presents the characterization measurements that have been performed to-date. Importantly, mass spectrometry measurements to determine sample impurities were not yet completed. These will be included in the final benchmark. The report gives the fitted decay constants for the die-away curves of each target sample. It also provides the data for the die-away curves in the appendices. The HDPE experiments examined twelve targets of varying size. The Lucite measurements included ten targets of varying size. Experimenters in the campaign were Daniel Siefman, William Zywiec, and Ruby Araj.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2022

High-pressure Cr 3+ R-line luminescence of zoisite and kyanite: a probe of octahedral site distortion

Here, the Cr 3+ luminescence spectra of zoisite and kyanite, two geologically important minerals, were studied up to 40 and 20 GPa, respectively, in various pressure media. Cr 3+ substitutes into the octahedral aluminum sites in both minerals and the R-line luminescence is a particularly sensitive site-specific probe of the octahedral Al site. Unlike many previous studies where Cr 3+ luminescence was utilized, both these minerals have multiple highly distorted octahedral sites resulting in very large splitting of their R-lines, ~ 300 cm -1 in zoisite and ~ 360 cm -1 in kyanite (for reference, ruby is 29 cm -1 ). For zoisite, the R-line splitting increases as pressure increases and more than triples from its ambient value by 40 GPa, while the R-line splitting in kyanite from the M1 and M2 sites does not change when compressed in a Ne pressure medium up to 20 GPa. We do not observe evidence of any phase transitions in either zoisite or kyanite across the pressure range of these new luminescence measurements. Furthermore, we present some high-pressure luminescence results where kyanite was known to be bridged between the diamond anvils and show how these spectra illustrate the different effect of uniaxial relative to hydrostatic stress on luminescence spectra.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Non-destructive spatial analysis of phosphatase activity and total protein distribution in the rhizosphere using a root blotting method

Phosphorus (P) is an essential macronutrient for plant growth, but bioavailable P in soils is often limited due to immobilization resulting from pH and geochemical interactions. Understanding the dynamics of P in soils and elucidating the mechanisms by which plants access P from their environment are critical to evaluating productivity, particularly in nutrient poor environments. Phosphorus from organic matter can act as a major source of P for organisms in soil systems. Phosphatases, enzymes that liberate inorganic P from organic sources, are produced by both plants and microbes and are considered one of the most active classes of enzymes in soil. In this work we developed a root blotting method to spatially image phosphatase activity in the rhizosphere. Proteins from the rhizosphere are transferred to a nitrocellulose membrane while retaining their enzymatic activity and two-dimensional spatial distribution. Subsequent application of a fluorogenic phosphatase indicator, DDAO phosphate, enables visualization of the distribution of phosphatase activity in the sample. The proteins can then be fixed to the membrane and treated with a SYPRO® Ruby gel stain, a fluorescent total protein stain, allowing for visualization of total protein distribution. Taken together, the images of phosphatase activity and total protein localization can be mapped back to the root architecture and provide insight into factors affecting the spatial distribution of enzymatic activity and protein accumulation in the rhizosphere. Notably, this method can be applied to plants growing in rhizoboxes containing soil or soilless growth mixtures (e.g., sand or various potting mixes) and, because of the non-destructive nature of this approach, be performed over time to track changes. We anticipate that this fluorescent indicator imaging technique on root blots can be used in diverse plant-microbe-soil systems to better understand the role of phosphatases in P acquisition and soil P cycling.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2021

Structural transitions of 4:1 methanol–ethanol mixture and silicone oil under high pressure

A 4:1 (volume ratio) methanol–ethanol (ME) mixture and silicone oil are two of the most widely used liquid pressure-transmitting media (PTM) in high-pressure studies. Their hydrostatic limits have been extensively studied using various methods; however, the evolution of the atomic structures associated with their emerging nonhydrostaticity remains unclear. Here, we monitor their structures as functions of pressure up to ∼30 GPa at room temperature using in situ high-pressure synchrotron x-ray diffraction (XRD), optical micro-Raman spectroscopy, and ruby fluorescence spectroscopy in a diamond anvil cell. No crystallization is observed for either PTM. The pressure dependence of the principal diffraction peak position and width indicates the existence of a glass transition in the 4:1 ME mixture at ∼12 GPa and in the silicone oil at ∼3 GPa, beyond which a pressure gradient emerges and grows quickly with pressure. There may be another liquid-to-liquid transition in the 4:1 ME mixture at ∼5 GPa and two more glass-to-glass transitions in the silicone oil at ∼10 GPa and ∼16 GPa. By contrast, Raman signals only show peak weakening and broadening for typical structural disordering, and Raman spectroscopy seems to be less sensitive than XRD in catching these structural transitions related to hydrostaticity variations in both PTM. These results uncover rich pressure-induced transitions in the two PTM and clarify their effects on hydrostaticity with direct structural evidence. The high-pressure XRD and Raman data on the two PTM obtained in this work could also be helpful in distinguishing between signals from samples and those from PTM in future high-pressure experiments.

Chen, Xiehang (ORCID:0000000168541506)↗

DOE OSTI2023

Photoluminescence of Cr 3+ in β-Ga 2 O 3 and (Al 0.1 Ga 0.9 ) 2 O 3 under pressure

The effects of pressure on single crystals of Cr-doped gallium oxide (β-Ga 2 O 3 :Cr 3+ ) and aluminum gallium oxide [(Al 0.1 Ga 0.9 ) 2 O 3 ] were examined by measuring the wavelength shift in the spectral R lines. Photoluminescence (PL) spectra of these materials were collected from samples in diamond anvil cells at pressures up to 9 GPa. The β-Ga 2 O 3 :Cr 3+ R lines were found to shift linearly under hydrostatic pressure. The (Al 0.1 Ga 0.9 ) 2 O 3 R lines also show a linear shift but the R 1 line shifted less than for β-Ga 2 O 3 :Cr 3+ . The ratio of R 2 to R 1 peak areas vs pressure is dominated by nonradiative recombination. X-ray diffraction measurements of (Al 0.1 Ga 0.9 ) 2 O 3 indicate that its equation of state is similar to that of β-Ga 2 O 3 . β-Ga 2 O 3 :Cr 3+ was examined under non-hydrostatic conditions by using mineral oil as a pressure transmitting medium. Similar to the case in ruby, the R 1 line is much more sensitive to non-hydrostatic stress than R 2 . Spatially resolved PL of a sample at 8 GPa in mineral oil showed significant variations in the R 1 emission wavelength. Furthermore, these results suggest that the R 1 line can serve as a sensitive probe of alloy composition and non-hydrostatic stress, while the R 2 line is insensitive to these perturbations.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Simultaneous measurements of volume, pressure, optical images, and crystal structure with a dynamic diamond anvil cell: A real-time event monitoring system

The dynamic diamond anvil cell (dDAC) technique has attracted great interest because it possibly provides a bridge between static and dynamic compression studies with fast, repeatable, and controllable compression rates. The dDAC can be a particularly useful tool to study the pathways and kinetics of phase transitions under dynamic pressurization if simultaneous measurements of physical quantities are possible as a function of time. We report the development of a real-time event monitoring (RTEM) system with dDAC, which can simultaneously record the volume, pressure, optical image, and structure of materials during dynamic compression runs. In particular, the volume measurement using both Fabry–Pérot interferogram and optical images facilitates the construction of an equation of state (EoS) using the dDAC in a home-laboratory. We also developed an in-line ruby pressure measurement (IRPM) system to be deployed at a synchrotron x-ray facility. This system provides simultaneous measurements of pressure and x-ray diffraction in low and narrow pressure ranges. The EoSs of ice VI obtained from the RTEM and the x-ray diffraction data with the IRPM are consistent with each other. The complementarity of both RTEM and IRPM systems will provide a great opportunity to scrutinize the detailed kinetic pathways of phase transitions using dDAC.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2026

PIPS-2025: an updated practical pressure scale for the large-volume presses

In 1997, AIRAPT recommended a set of room-temperature pressure reference points (PRPs) for the large-volume press (LVP) community, known as the Practical International Pressure Scale (PIPS-97). With recent AIRAPT-recommended ruby scale Ruby2020 for diamond-anvil cell (DAC) experiments, it is now necessary to re-examine PIPS-97 for consistency with the DAC pressure scale. Here, we reconstruct equations of state (EOSs) for NaCl and Au that are explicitly tied to Ruby2020 and recalculate the PRPs using these EOSs. The revised PRP values are given. GaAs is removed from the PRP list because of the complexity of its phase transitions. The ZnS value, although retained, requires further investigation. Overall, the revised pressures are systematically higher than PIPS-97 by up to 4% at 35 GPa. We propose that this updated set of PRPs, referred to as PIPS-2025, be adopted for LVP experiments to improve pressure consistency between the LVP and DAC communities.

Large volume press↗

DOE OSTI2023

Prevalence of erythromycin-resistant emm92 -type invasive group A streptococcal infections among injection drug users in West Virginia, United States, 2021–23

Abstract Background Increasing incidence of invasive group A Streptococcus (iGAS) disease has been reported in Europe and the USA over the past several years. Coupled with this are observations of higher rates of resistance to erythromycin and clindamycin. Objectives To characterize iGAS and pharyngitis isolates from West Virginia (WV), a US state outside of the national Active Bacteria Core surveillance purview, where risk factors associated with iGAS infections are prevalent. Methods Seventy-seven invasive group A Streptococcus isolates were collected from 67 unique patients at the J.W. Ruby Memorial Hospital Clinical Microbiology Laboratory in WV from 2021 to 2023. Invasive isolates and 20 unique pharyngitis isolates were tested for clindamycin and erythromycin susceptibility in the clinical laboratory. Patient demographic and clinical information was retrieved from patient electronic health records. Isolates were further characterized based on emm subtype and detection of MLSB resistance determinants. Results Twenty-six (39%) isolates were of a single emm92 type. All emm92 isolates were uniformly erythromycin/clindamycin resistant with inducible or constitutive MLSB resistance imparted by the plasmid-borne erm(T) gene. The majority of emm92 infections were associated with adult patients who reported IV drug use, whereas no pharyngitis infections were caused by an emm92 strain. Overall, 51 (76%) of the 67 iGAS isolates were determined to carry MLSB resistance. Conclusions Isolates of emm92 type (clonal subtype emm92.0) were associated with iGAS infections in adult IV drug users, but not with paediatric pharyngitis, and were uniformly resistant to erythromycin and clindamycin.

Powell, Lillie M.↗

DOE OSTI2025

Viral delivery of recombinases activates heritable genetic switches in plants

Viral vectors provide an increasingly versatile platform for transformation-free reagent delivery to plants. RNA viral vectors can be used to induce gene silencing, overexpress proteins, or introduce gene editing reagents; however, they are often constrained by carrying capacity or restricted tropism in germline cells. Site-specific recombinases that catalyze precise genetic rearrangements are powerful tools for genome engineering that vary in size and, potentially, efficacy in plants. In this work, we show that viral vectors based on tobacco rattle virus (TRV) deliver and stably express four recombinases ranging in size from ~0.6kb to ~1.5kb and achieve simultaneous marker removal and reporter activation through targeted excision in transgenic Nicotiana benthamiana lines. TRV vectors with Cre, FLP, CinH, and Integrase13 efficiently mediated recombination in infected somatic tissue and led to heritable modifications at high frequency. Here, an excision-activated Ruby reporter enabled simple and high-resolution tracing of infected cell lineages without the need for molecular genotyping. Together, our experiments broaden the scope of viral recombinase delivery and offer insights into infection dynamics that may be useful in developing future viral vectors.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2025

Dynamic compression effects of H 2 ⁡O in a dynamic diamond anvil cell: Origin of metastable ice VII and its crystal growth kinetics

We report on the structural verification of metastable ice VII solidifying in the phase space of ice VI at 1.80 GPa at room temperature. Using time-resolved (TR) x-ray diffraction and TR ruby luminescence paired with high-speed microphotography utilizing a dynamic diamond anvil cell, an initial compression rate range from 0.12 to 95.84 GPa/s was explored. The solidification pressure of metastable ice VII has a potential sigmoidal dependence upon compression rate with a turnover compression rate of ∼80 GPa/s. The preferred crystallization of ice VII in the stability field of ice VI is due to the increased nucleation rate of ice VII over ice VI at 1.77 GPa that is driven by the surface energy difference between the liquid and solid phases along with the change in Gibbs free energy of solidification. The dynamic pressure-volume–compression behaviors of ice phases (VI and VII) show a lattice stiffening in both phases, especially during the compression loading. It is also found that the compression rate greatly affects the solid-solid phase transition between ice VI and VII but does not affect the liquid-solid transition between water and ice VI as much. Lastly, a third phase transition was found to occur after metastable ice VII transforms into high-density amorphous (HDA) ice, which could be a disordered hydrogen-bonded network configuration of ice VII forming out of HDA ice facilitated by the decoupling of the oxygen movement and reorientation of the H 2⁡ O molecule. These results demonstrate the complexity of a seemingly simple molecule H 2⁡ O, how it can readily change its static properties with the modification of (de)compression rate, and highlight the need to use multiple TR structural and spectroscopic probes at higher time resolutions to realize the most comprehensive understanding.

Chemical bonding↗

DOE OSTI2025

Electronic and optical properties of transition metal impurities in GaN and AlN

The optical properties of Cr(III) impurities are well studied and exploited in 𝛼−Al 2 ⁢O 3 , which enables ruby lasers. Photoluminescence spectra resembling the famous 1.78 eV emission of Cr in 𝛼−Al 2 ⁢O 3 have been observed in other wide-band-gap host materials, in particular AlN. However, it is unclear whether Cr would produce the same emission in the nitrides as in 𝛼−Al 2 ⁢O 3 , especially given the different local environment (tetrahedral vs octahedral coordination). We investigate the electronic and optical properties of transition metal substitutional impurities (Cr, Co, Ni, and Cu) in wurtzite GaN and AlN from first principles, utilizing hybrid density functional theory. We calculate the optical transition energies using a constrained occupation approach that accounts for the multideterminant nature of the excited states. Our results indicate that substitutional Cr(III) is not responsible for the emission near 1.78 eV observed in the nitrides. Among the examined impurities, only substitutional Co(II) produces emission near 1.78 eV. Based on the favorable properties of Co(II) (low formation energy, small Huang-Rhys factor, and an 𝑆 = 3/2 ground state) we propose it as a promising single-photon emitter or spin qubit. We additionally assign the PL peak observed near 1.05 eV in GaN and AlN to the 2 𝐸→ 4 𝐴 2 transition of the Ni(III) substitution.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Data for "Viral Delivery of Recombinases Activates Heritable Genetic Switches in Plants"

Viral vectors provide an increasingly versatile platform for transformation-free reagent delivery to plants. RNA viral vectors can be used to induce gene silencing, overexpress proteins, or introduce gene editing reagents; however, they are often constrained by carrying capacity or restricted tropism in germline cells. Site-specific recombinases that catalyze precise genetic rearrangements are powerful tools for genome engineering that vary in size and, potentially, efficacy in plants. In this work, we show that viral vectors based on tobacco rattle virus (TRV) deliver and stably express four recombinases ranging in size from ∼0.6 to ∼1.5 kb and achieve simultaneous marker removal and reporter activation through targeted excision in transgenic Nicotiana benthamiana lines. TRV vectors with Cre, FLP, CinH, and Integrase13 efficiently mediated recombination in infected somatic tissue and led to heritable modifications at high frequency. An excision-activated Ruby reporter enabled simple and high-resolution tracing of infected cell lineages without the need for molecular genotyping. Together, our experiments broaden the scope of viral recombinase delivery and offer insights into infection dynamics that may be useful in developing future viral vectors.

gene editing↗

DOE OSTI2024

Shadow of a laser beam

Light, being massless, casts no shadow; under ordinary circumstances, photons pass right through each other unimpeded. Here, we demonstrate a laser beam acting like an object — the beam casts a shadow upon a surface when the beam is illuminated by another light source. We observe a regular shadow in the sense it can be seen by the naked eye, it follows the contours of the surface it falls on, and it follows the position and shape of the object (the laser beam). Specifically, we use a nonlinear optical process involving four atomic levels of ruby. We are able to control the intensity of a transmitted laser beam by applying another perpendicular laser beam. We experimentally measure the dependence of the contrast of the shadow on the power of the laser beam, finding a maximum of approximately 22%, similar to that of a shadow of a tree on a sunny day. We provide a theoretical model that predicts the contrast of the shadow. This work opens new possibilities for fabrication, imaging, and illumination.

47 OTHER INSTRUMENTATION↗

DOE OSTI2024

MultiGreen: A multiplexing architecture for GreenGate cloning

Genetic modification of plants fundamentally relies upon customized vector designs. The ever-increasing complexity of transgenic constructs has led to increased adoption of modular cloning systems for their ease of use, cost effectiveness, and rapid prototyping. GreenGate is a modular cloning system catered specifically to designing bespoke, single transcriptional unit vectors for plant transformation—which is also its greatest flaw. MultiGreen seeks to address GreenGate’s limitations while maintaining the syntax of the original GreenGate kit. The primary limitations MultiGreen addresses are 1) multiplexing in series, 2) multiplexing in parallel, and 3) repeated cycling of transcriptional unit assembly through binary intermediates. MultiGreen efficiently concatenates bespoke transcriptional units using an additional suite of level 1acceptor vectors which serve as an assembly point for individual transcriptional units prior to final, level 2, condensation of multiple transcriptional units. Assembly with MultiGreen level 1 vectors scales at a maximal rate of 2*⌈ log 6 n ⌉+3 days per assembly, where n represents the number of transcriptional units. Further, MultiGreen level 1 acceptor vectors are binary vectors and can be used directly for plant transformation to further maximize prototyping speed. MultiGreen is a 1:1 expansion of the original GreenGate architecture’s grammar and has been demonstrated to efficiently assemble plasmids with multiple transcriptional units. MultiGreen has been validated by using a truncated violacein operon from Chromobacterium violaceum in bacteria and by deconstructing the RUBY reporter for in planta functional validation. MultiGreen currently supports many of our in-house multi transcriptional unit assemblies and will be a valuable strategy for more complex cloning projects.

Science & Technology - Other Topics↗

DOE OSTI2021

Two-Phase Equation of State for Al 2 O 3

Two-phase equation of state (EOS) for AI 2 O 3 (alumina) is calibrated using the experimental/simulation calibration data uploaded to the caldata repository. The two phases are solid α-Al 2 O 3 (corundum, sapphire, ruby) and its melt. The enthalpy of formation is set to that available from the NIST-JANAF database at T = 0K, P =1 bar. The expected applicability range of the EOS is from the ambient conditions to temperatures of ~ 5000 K and pressures of ~ 50-100 GPa.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Performance Evaluation and Costs of a Combined Ground Source Heat Pump and Solar Photovoltaic Storage System in an Extreme Cold Climate

This report outlines the effectiveness and economics of a ground source heat pump system installed together with solar photovoltaic panels and a battery storage system in a local community building situated in a cold climate. The community building is a tribal building located in Ruby, Alaska. Power from solar photovoltaic panels is supplemented by electricity purchased from the local community microgrid. A ground source heat pump was commissioned three years after the building was occupied, and supplements the heat generated by a boiler for both heat and domestic hot water. Data collected over the 2021-2022 heating season shows that the heat pump is providing heat to the building about 19% of the time with an average coefficient of performance of 2.68, ranging from below 2.5 in winter to above 3.0 in summer. The solar photovoltaic panels provided 4,700 kWh of power used within the building and an additional 2,900 kWh exported to the microgrid. The solar-produced power used within the building nearly offsets the estimated annual electrical draw of the heat pump of 5,700 kWh. Due to the very high costs for shipping and installation to remote locations, projects such as this, while not economically feasible if self-funded, can save the community an estimated $76,051 over a period of 20-years. Fuel prices increasing by more than 25%, or subsidized electricity prices decreasing by more than 25%, make the ground source heat pump a more viable option economically. Unsubsidized electricity prices increasing by 25% or more make a solar photovoltaic system with battery storage nearly economically viable after a 20-year period for commercial or school buildings that are not eligible for Alaska's Power Cost Equalization program.

14 SOLAR ENERGY↗

DOE OSTI2021

Overcoming Barriers to Radiopharmaceutical Therapy (RPT): An Overview From the NRG-NCI Working Group on Dosimetry of Radiopharmaceutical Therapy

Radiopharmaceutical therapy (RPT) continues to demonstrate tremendous potential in improving the therapeutic gains in radiation therapy by specifically delivering radiation to tumors that can be well assessed in terms of dosimetry and imaging. Dosimetry in external beam radiation therapy is standard practice. This is not the case, however, in RPT. This NRG (acronym formed from the first letter of the 3 original groups: National Surgical Adjuvant Breast and Bowel Project, the Radiation Therapy Oncology Group, and the Gynecologic Oncology Group)-National Cancer Institute Working Group review describes some of the challenges to improving RPT. The main priorities for advancing the field include (1) developing and adopting best practice guidelines for incorporating patient-specific dosimetry for RPT that can be used at both large clinics with substantial resources and more modest clinics that have limited resources, (2) establishing and improving strategies for introducing new radiopharmaceuticals for clinical investigation, (3) developing approaches to address the radiophobia that is associated with the administration of radioactivity for cancer therapy, and (4) solving the financial and logistical issues of expertise and training in the developing field of RPT.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2022

Direct Visualization of Magnetic Correlations in Frustrated Spinel ZnFe 2 O 4

Magnetic materials with the spinel structure (A 2+ B 3+ 2 O 4 ) form the core of numerous magnetic devices, and ZnFe 2 O 4 constitutes a peculiar example where the nature of the magnetism is still unresolved. Susceptibility measurements revealed a cusp around T c = 13 K resembling an antiferromagnetic transition, despite the positive Curie–Weiss temperature determined to be Θ CW = 102.8(1) K. Bifurcation of field-cooled and zero-field-cooled data below T c in conjunction with a frequency dependence of the peak position and a non-zero imaginary component below T c shows it is in fact associated with a spin-glass transition. Highly structured magnetic diffuse neutron scattering from single crystals develops between 50 K and 25 K revealing the presence of magnetic disorder which is correlated in nature. Here, the 3D-mΔPDF method is used to visualize the local magnetic ordering preferences, and ferromagnetic nearest-neighbor and antiferromagnetic third nearest-neighbor correlations are shown to be dominant. Their temperature dependence is extraordinary with some flipping in sign and a strongly varying correlation length. The correlations can be explained by orbital interaction mechanisms for the magnetic pathways and a preferred spin cluster. This study demonstrates the power of the 3D-mΔPDF method in visualizing complex quantum phenomena thereby providing a way to obtain an atomic-scale understanding of magnetic frustration.

36 MATERIALS SCIENCE↗