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At least 163 records · Page 9

All sources NASA NTRS DOE OSTI

DOE OSTI2021

Highly efficient, rapid, and concurrent removal of toxic heavy metals by the novel 2D hybrid LDH–[Sn 2 S 6 ]

According to a United Nations report, by 2050 nearly six billion people worldwide will suffer from clean water scarcity. This is mostly because of the exponential proliferation of world population, urbanization, industrialization, and water pollution. Heavy metals are common water pollutants that can pose grave public health consequences. Existing water purification systems are lack of materials that have the potential for quick, simultaneous, efficient, and cost-efficient removal of numerous toxic metals from wastewater. Here, in this work, we report the design and synthesis of an economically viable Layered Double Hydroxides - Stannic Sulfide, LDH–[Sn 2 S 6 ] that exhibits a rapid, efficient, selective, and concurrent removal of Cu 2+ , Ag + , Cd 2+ , Pb 2+ , and Hg 2+ from parts per million (ppm) level to below 5 parts per billion (ppb) satisfying World Health Organization’s (WHO) safe drinking water limit. Moreover, LDH–[Sn 2 S 6 ] shows exceptionally high removal efficiencies of the above metals in acidic, neutral, and basic conditions. LDH–[Sn 2 S 6 ] also demonstrates enormous sorption capacities of 378, 978, 332, 579, and 666 mg/g for Cu 2+ , Ag + , Cd 2+ , Pb 2+ , and Hg 2+ , respectively. Remarkably, LDH–[Sn 2 S 6 ] displays extraordinary tolerance to the concentrations of Na + , Ca 2+ , Mg 2+ , Cl - , CO 3 2– , NO 3 – ,and SO 4 2- , and other constituents in tap and river water, it efficiently sequestrates Cu 2+ , Ag + , Cd 2+ , Pb 2+ , and Hg 2+ from ppm to safe drinking water levels in minutes. LDH–[Sn 2 S 6 ] shows pseudo-second-order sorption kinetics suggesting chemisorption adsorption mechanism involving M–S bonding. Altogether, the regeneratable LDH–[Sn 2 S 6 ] becomes an exceptional material that shows ultrahigh removal, unprecedented selectivity, rapid adsorption kinetics, wide pH stability, and a massive adsorption capacity. The integration of these features places LDH–[Sn 2 S 6 ] at the top of all adsorbents known to date and thus could be used for wastewater purifications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Examining infrared thermography based approaches to rapid fatigue characterization of additively manufactured compression molded short fiber thermoplastic composites

A novel additive manufacturing (AM) methodology combined with a compression molding (CM) process has been developed to optimize the microstructure of short fiber thermoplastic composites (SFTs)with higher fiber alignment and lower porosity, yielding superior stiffness, strength, and structural integrity. Here, the current work examines the efficacy of the ‘passive’ infrared thermography (IRT) techniques for rapid fatigue characterization of SFTs that use the surface temperature evolution during cyclic loading due to self-heating as a fatigue indicator. A comparison of fatigue limits obtained from traditional stress-life (SN) (≈53.1%σ uts ) and IRT (≈54.1%σ uts ) shows a close match. However, the SN curve required 18 specimens and two weeks of continuous cyclic testing, while IRT used three specimens with 5 hours of testing. Thus, the IRT approach provides an accelerated testing framework for rapidly estimating the fatigue limit. Additionally, existing phenomenological approaches to IRT fatigue characterization have been examined.

42 ENGINEERING↗

DOE OSTI2026

Rapid Coal-Ash Characterization using Geophysical Methods & Machine Learning

Coal combustion products (CCP) are challenging to delineate in heterogeneous field settings. Conventional methods (test pits, coring, and laboratory analyses) are labor-intensive, slow, invasive, and provide sparse spatial coverage. This study evaluates whether rapid non-invasive geophysical screening methods—induced polarization (IP), magnetic susceptibility, and nuclear magnetic resonance (NMR) —combined with surface colorimetry (RGB_24), can discriminate CCP-soil mixtures and provide reliable estimates of CCP content. Laboratory measurements were collected on five CCP-soil mixtures (series) and modeled using (i) a linear baseline, (ii) a calibrated non-linear (power-mean) model, and (iii) a machine-learning (ML) Random Forest approach, with validation via leave-one-series-out and site-specific tests. Across the five series, individual signals—particularly IP and magnetic susceptibility—were strongly predictive of ash content but were consistently outperformed by combined models. The pooled calibrated non-linear and ML models captured the observed non-linearity and achieved high accuracy and precision, improving on linear fits. Colorimetry showed the weakest direct relationship with ash content for the tested samples but improved performance when included in multi-signal models. At pre-selected 3.5% decision threshold, calibrated and ML approaches yielded near-perfect classification (Matthews correlation coefficient ˜ 1), suggesting strong practical operability for field screening. Additionally, field-analog tests highlighted the role of endmembers—accuracy declined without access to end-member measurements but was largely recovered by collecting a minimal labeled pair for local recalibration. With end members, accuracy remained high. Globally trained models performed well on three operational unknowns; however, series-specific refits provided the most accurate predictions. Overall, these results highlight the potential of combining rapid geophysics and minimal local calibration for improved coal-ash delineation.

Peshtani, Klaudio↗

DOE OSTI2021

Chemically Inert Hydrocarbon-Based Slurries for Rapid Laser Sintering of Thin Proton-Conducting Ceramics

The process of rapid laser sintering of thin BaZrO 3 –BaCeO 3 -based proton-conducting electrolytes is being developed for easy fabrication of ceramic fuel cells and electrolyzers. However, cracks on the electrolytes caused by volume change due to chemical reactions between the basic ceramic constituents and the polar solvents during wet processing has been problematic. In order to address this issue, the use of chemically inert saturated-hydrocarbon-based slurries comprised of hexadecane, polybutene, and a long-chain saturated fatty acid were investigated in this work. By optimizing slurry composition and laser sintering conditions, a 20 mm long, 4 mm wide, 13.5-μm-thick and 97%-dense BaCe 0.7 Zr 0.1 Y 0.07 Sm 0.13 O 3-d membrane showing proton conductivity on the order of 10 –4 S•cm –1 at 600 °C was successfully prepared in just three seconds by laser sintering. As a result, the use of saturated-hydrocarbon-based slurries will facilitate wet processing and rapid laser sintering of proton-conducting ceramic electrolytes.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Inactivation of multiple human pathogens by Fathhome's dry sanitizer device: Rapid and eco-friendly ozone-based disinfection

SARS-CoV-2 spread rapidly, causing millions of deaths across the globe. As a result, demand for medical supplies and personal protective equipment (PPE) surged and supplies dwindled. Separate entirely, hospital-acquired infections have become commonplace and challenging to treat. To explore the potential of novel sterilization techniques, this study evaluated the disinfection efficacy of Fathhome's ozone-based, dry-sanitizing device by dose and time response. Inactivation of human pathogens was tested on non-porous (plastic) surfaces. 95.42-100% inactivation was observed across all types of vegetative microorganisms and 27.36% inactivation of bacterial endospores tested, with no residual ozone detectable after completion. These results strongly support the hypothesis that Fathhome's commercial implementation of gas-based disinfection is suitable for rapid decontamination of a wide variety of pathogens on PPE and other industrially relevant materials.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2026

Rapid neutron and gamma-ray source localization using machine learning

Rapid localization of radiation sources is critical for applications including nuclear emergency response, safeguards, and security. However, conventional imaging systems such as neutron scatter cameras and Compton cameras depend on rare coincidence events, which often result in long acquisition times. In this work, we address the challenge of rapid source localization by developing a machine learning approach to predict the direction of a single radiation source using only count rates from an array of neutron and gamma-ray detectors. The proposed model is a fully connected neural network (FCNN) trained using Monte Carlo simulation data from a 252 Cf source. The model hyperparameters are optimized with a small set of routine 252 Cf measurements. We benchmarked the performance of the trained and optimized machine learning model using additional 252 Cf , 137 Cs , and PuBe measurements under laboratory conditions with varying source-detector configurations. For these measurements, the machine learning model achieved a mean localization error smaller than 30° with 3 x 10 3 system counts, corresponding to 8 s measurement time for the imaging system used in this work. In this low-statistics regime, the method outperformed traditional scatter-based imaging by more than 75% in localization accuracy for the evaluated measurement configurations. These results demonstrate that a machine learning-based approach can significantly reduce the time required for accurate single-source localization, providing a robust and computationally efficient alternative to traditional imaging systems in time-critical nuclear security and emergency response scenarios.

Gamma-ray imaging↗

DOE OSTI2021

Inclusive heavy-flavour production at central and forward rapidity in Xe–Xe collisions at $\sqrt{s_{NN}}$ = 5.44 TeV

The first measurements of the production of muons and electrons from heavy-flavour hadron decays in Xe–Xe collisions at $\sqrt{s_{NN}}$ =5.44 TeV, using the ALICE detector at the LHC, are reported. The measurement of the nuclear modification factor R AA is performed as a function of transverse momentum p T in several centrality classes at forward rapidity (2.5 < y < 4) and midrapidity (|y| < 0.8) for muons and electrons from heavy-flavour hadron decays, respectively. A suppression by a factor up to about 2.5 compared to the binary-scaled pp reference is observed in central collisions at both central and forward rapidities. The R AA of muons from heavy-flavour hadron decays is compared to previous measurements in Pb–Pb collisions at $\sqrt{s_{NN}}$ = 5.02 TeV. When the nuclear modification factors are compared in the centrality classes 0–10% for Xe–Xe collisions and 10–20% for Pb–Pb collisions, which have similar charged-particle multiplicity density, a similar suppression, with R AA ~ 0.4 in the p T interval 4 < p T < 8 GeV/c, is observed. The comparison of the measured R AA values in the two collision systems brings new insights on the properties of the quark-gluon plasma by investigating the system-size and geometry dependence of medium-induced parton energy loss. The results of muons and electrons from heavy-flavour hadron decays provide new constraints to model calculations.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2023

Measurements of azimuthal anisotropies at forward and backward rapidity with muons in high-multiplicity p–Pb collisions at $\sqrt{s_{NN}} = 8.16$ TeV

The study of the azimuthal anisotropy of inclusive muons produced in p–Pb collisions at $\sqrt{s_{NN}}$ = 8.16 TeV, using the ALICE detector at the LHC is reported. The measurement of the second-order Fourier coefficient of the particle azimuthal distribution, v 2 , is performed as a function of transverse momentum p T in the 0–20% high-multiplicity interval at both forward (2.03 < y CMS < 3.53) and backward (-4.46 < y CMS < -2.96) rapidities over a wide pT range, 0.5 < p T < 10 GeV/c, in which a dominant contribution of muons from heavy-flavour hadron decays is expected at p T > 2 GeV/c. The v 2 coefficient of inclusive muons is extracted using two different techniques, namely two-particle cumulants, used for the first time for heavy-flavour measurements, and forward–central two-particle correlations. Both techniques give compatible results. A positive v 2 is measured at both forward and backward rapidities with a significance larger than 4.7σ and 7.6σ, respectively, in the interval 2 < p T < 6 GeV/c. Comparisons with previous measurements in p–Pb collisions at $\sqrt{s_{NN}}$ = 5.02 TeV, and with AMPT and CGC-based theoretical calculations are discussed. The findings impose new constraints on the theoretical interpretations of the origin of the collective behaviour in small collision systems

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2023

A data analysis method to rapidly characterize gallium concentration in plutonium matrices using LIBS

The processing of actinide samples is a complex and costly endeavor that requires compositional analysis at various stages. Laser-induced breakdown spectroscopy (LIBS) has been used to analyze actinide-containing samples in many nuclear applications including waste management, fuel processing and forensics. The LIBS spectrum obtained from actinide materials are generally extremely complex, exhibiting many thousands of strong emission lines. This makes it difficult to identify other elements within the sample of interest, given the rich and dominant actinide spectrum. Here, in this article, we describe a recent effort to identify and quantify impurities and alloying constituents in plutonium matrices using a hand-held LIBS instrument that is used to rapidly and efficiently measure an emission spectrum from a material sample. We tabulate the emission line positions and intensities of plutonium. We report the development of machine-learning software that can identify gallium and quantify its concentration in plutonium matrices. This work has the potential to provide a rapid and nearly non-destructive technique that allows more confidence in characterizing the composition of materials that are present within complex actinide associated targets. We describe how our LIBS measurements and data analysis methods have successfully quantified the gallium concentration in a variety of samples.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Rapid characterization and failure analysis of 6276 rooftop-harvested photovoltaic connectors

Photovoltaic (PV) connectors, which link modules in series and connect PV strings in parallel, have increasingly been recognized as a primary contributor to PV system failures and a source of numerous fire incidents. However, publicly available data on the rates and types of connector failures are scarce, primarily due to the proprietary nature of the information and the need for comprehensive analysis. This study represents the first large-scale investigation of harvested PV connectors, drawing from a dataset of 6276 connectors from residential rooftop solar systems across the United States. The outcome of this work is twofold: 1) we have established a rapid characterization method for large populations of harvested connectors, incorporating visual inspection, resistance measurements, and X-ray imaging; and 2) the analysis made possible by our rapid-processing method has revealed, for a population of connector models provided by a single rooftop installer, failure statistics and insights for various connector makes and models, installation practices, operating currents, and internal component displacements. This research identifies common failure modes that could be considered in future connector designs standards, and operations and maintenance practices, to ultimately improve the reliability of this vital component of PV infrastructure.

MC4↗

DOE OSTI2021

Oestrogen regulates SOX9 bioavailability by rapidly activating ERK1/2 and stabilising microtubules in a human testis-derived cell line

Highlights: • Brief oestrogen treatment causes the cytoplasmic retention of the testis factor SOX9. • The cytoplasmic retention of SOX9 by oestrogen is associated with the rapid stabilisation of microtubules. • ERK1/2 is required for the stabilisation of microtubules by activated oestrogen receptors. • Oestrogen can act on both a non-genomic and genomic level to impact gonad somatic cell fate. Nuclear SOX9 is essential for Sertoli cell differentiation and the development of a testis. Exposure of Sertoli cells to exogenous oestrogen causes cytoplasmic retention of SOX9, inhibiting testis development and promoting ovarian development. The cytoplasmic localisation of SOX9 requires a stabilised microtubule network and a key MAPK complex, ERK1/2, is responsive to oestrogen and known to affect the microtubule network. We hypothesised that oestrogen could stabilise microtubules through the activation of ERK1/2 to promote the cytoplasmic retention of SOX9. Treatment of human testis-derived NT2/D1 cells for 30 min with oestrogen rapidly activated ERK1/2, stabilised the microtubule network and increased cytoplasmic localisation of SOX9. The effects of oestrogen on SOX9 and tubulin were blocked by the ERK1/2 inhibitor U0126, demonstrating that ERK1/2 mediates the stabilisation of microtubules and cytoplasmic retention of SOX9 by oestrogen. Together, these data revealed a previously unknown mechanism for oestrogen in impacting MAPK signalling to block SOX9 bioavailability and the differentiation of Sertoli cells.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2021

Boundary zonal flows in rapidly rotating turbulent thermal convection

Recently, in Zhang et al. ( Phys. Rev. Lett. , vol. 124, 2020, 084505), it was found that, in rapidly rotating turbulent Rayleigh–Bénard convection in slender cylindrical containers (with diameter-to-height aspect ratio $\varGamma =1/2$ ) filled with a small-Prandtl-number fluid ( ${Pr}\approx 0.8$ ), the large-scale circulation is suppressed and a boundary zonal flow (BZF) develops near the sidewall, characterized by a bimodal probability density function of the temperature, cyclonic fluid motion and anticyclonic drift of the flow pattern (with respect to the rotating frame). This BZF carries a disproportionate amount ( ${>}60\,\%$ ) of the total heat transport for ${Pr} < 1$ , but decreases rather abruptly for larger ${Pr}$ to approximately $35\,\%$ . In this work, we show that the BZF is robust and appears in rapidly rotating turbulent Rayleigh–Bénard convection in containers of different $\varGamma$ and over a broad range of ${Pr}$ and ${Ra}$ . Furthermore, tirect numerical simulations for Prandtl number $0.1 \leq {\textit {Pr}} \leq 12.3$ , Rayleigh number $10^7 \leq {Ra} \leq 5\times 10^{9}$ , inverse Ekman number $10^{5} \leq 1/{\textit {Ek}} \leq 10^{7}$ and $\varGamma = 1/3$ , 1/2, 3/4, 1 and 2 show that the BZF width $\delta _0$ scales with the Rayleigh number ${Ra}$ and Ekman number ${\textit {Ek}}$ as $\delta _0/H \sim \varGamma ^{0} Pr^{\{-1/4, 0\}} {Ra}^{1/4} {\textit {Ek}}^{2/3}$ ( $\{{\textit {Pr}}<1, {\textit {Pr}}>1\}$ ) and with the drift frequency scales as $\omega /\varOmega \sim \varGamma ^{0} Pr^{-4/3} {Ra}\,{\textit {Ek}}^{5/3}$ , where $H$ is the cell height and $\varOmega$ the angular rotation rate. The mode number of the BZF is 1 for $\varGamma \lesssim 1$ and $2 \varGamma$ for $\varGamma = \{1,2\}$ independent of ${Ra}$ and ${Pr}$ . The BZF is quite reminiscent of wall mode states in rotating convection.

42 ENGINEERING↗

DOE OSTI2025

Rapid High-Resolution Analysis of Polysaccharide-Lignin Interactions in Secondary Plant Cell Walls Using Proton-Detected Solid-State NMR

The plant secondary cell wall, a complex matrix composed of cellulose, hemicellulose, and lignin, is crucial for the mechanical strength and water-proofing properties of plant tissues, and serves as a primary source of biomass for biorenewable energy and biomaterials. Structural analysis of these polymers and their interactions within the secondary cell wall has been heavily relying on 13 C-based solid-state NMR techniques. In this study, we explore the application of 1 H-detected solid-state NMR techniques for rapid, high-resolution structural characterization of polysaccharides and lignin, demonstrated on the stems of hardwood eucalyptus. We explored the use of synthesized 2D spectra to resolve central 1 H resonances and the combined application of 3D hCCH and hCHH experiments for complete resonance assignment and unambiguous identification of lignin-carbohydrate interactions. Our findings emphasize the central role of acetylated three-fold xylan conformers, rather than two-fold, in stabilizing the carbohydrate-lignin interface, with glucuronic acid sidechains in eucalyptus glucuronoxylan colocalizing with lignin, revised cellulose-lignin interactions involving uncoated microfibril surfaces, and pectin-lignin interactions indicative of early-stage lignification. These results present a novel approach for rapid structural analysis of lignocellulosic biomaterials without the need for solubilization or extraction.

09 BIOMASS FUELS↗

DOE OSTI2025

A Method for Rapid and Precise Triple Oxygen Isotope Measurements via High-Temperature Conversion to CO Followed by Nickel-Catalyzed CO to CO 2 Conversion and Laser Spectroscopy

Triple oxygen isotopic compositions ( 16 O, 17 O, 18 O) have conventionally been measured via isotope ratio mass spectrometry using O 2 as an analyte. Conversion of sample oxygen to O 2 typically utilizes fluorination chemistry or catalytic equilibration between CO 2 and O 2 . Recently, laser spectroscopy has become a viable alternative for triple oxygen isotope (Δ' 17 O) measurements due to its ease and rapid throughput. Laser spectrometers are currently available for Δ' 17 O analysis of either H 2 O or CO 2 as the analyte gas. So far, these instruments have been used to measure Δ' 17 O of water, carbonate (CO 2 liberated by acid digestion), and atmospheric CO 2 samples. Here, we present a new method for high-precision Δ' 17 O analysis of CO 2 via tunable infrared laser direct absorption spectroscopy that is compatible with a wider range of geochemically important materials. This approach involves converting sample oxygen to CO 2 in two steps. First, the sample oxygen is liberated and reduced to CO by high-temperature conversion at 1450 °C in the presence of excess elemental carbon. Then, CO is catalytically converted to CO 2 over hot nickel at 350 °C. The conversion process is rapid (10 to 30 min) and quantitative. Spectroscopic Δ' 17 O analysis of the resulting CO 2 takes approximately 45 min. By measuring several oxygen isotope standards, we demonstrate that the method is precise (1σ = 12 per meg for procedural replicates) and accurate (within 11 per meg of previously reported values). The method can be applied to most pyrolytic materials where quantitative oxygen conversion is attainable, such as sulfate, phosphate, nitrate, and oxide minerals, water, and organic molecules.

Ellis, Nicholas M. [University of California, Berk↗

DOE OSTI2020

Rapid and Simultaneous Characterization of Drug Conjugation in Heavy and Light Chains of a Monoclonal Antibody Revealed by High-Resolution Ion Mobility Separations in SLIM

Antibody-drug conjugates (ADCs) have recently gained traction in the biomedical community due to their promise for human therapeutics and an alternative to chemotherapy for cancer. Crucial metrics for ADC efficacy, safety, and selectivity are their drug-antibody ratios (DARs). However, DAR characterization (i.e., determining the average number of conjugated drugs on the antibody) through analytical methods remains challenging due to the heterogeneity of drug conjugation as well as the numerous post-translational modifications possible in the monoclonal antibody. In this work, we report on the use of high-resolution ion mobility spectrometry separations in our structures for lossless ion manipulations coupled to mass spectrometry (SLIM IMS-MS) platform for the rapid and simultaneous characterization of the drug load profile (i.e., stoichiometric distribution of the number of conjugated drugs present on the mAb), determination of the weighted average DAR in both the heavy and light chains of a model antibody-drug conjugate, and calculation of the overall DAR of the ADC. After chemical reduction of the ADC and a subsequent 31.5 meter SLIM IMS separation the various drug bound antibody species could be well resolved for both chains. Furthermore, we also show that higher resolution separations were possible with SLIM IMS as compared to ones performed on a commercially available (~1 meter) drift tube IMS-MS platform. Interestingly, additional gas-phase substructures become evident with longer path length SLIM IMS, potentially providing insight related to how drug conjugation may alter the structural properties of a monoclonal antibody and thus affect its overall potency and/or selectivity for a given antigen. We expect high-resolution SLIM IMS separations will augment the existing toolbox for ADC characterization, particularly for structural confirmation to enable the rapid optimization of DAR for a given ADC and thus better understand its potential toxicity and potency.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Selective Sorbent Design: CaS Aerogel for Rapid Remediation of Aqueous Pb (II)

Heavy metals are a persistent environmental problem due to their high toxicity, even at very low concentrations (parts per billion, ppb). The removal of such diluted heavy metals is challenging because of the competition the counterions (Ca 2+ , Na + , Mg 2+ , etc.) present in natural water bodies. The design of sorbents capable of removing ions below the action limit (15 ppb for Pb 2+ ) requires a strong driving force for selective uptake and rapid removal. In this work, we report the synthesis of porous CaS aerogels (surface area = 143.6 m 2 /g) by oxidative assembly of CaS nanoparticles and describe their use in selective Pb 2+ ion remediation from water. Despite the presence of amorphous CaCO 3 (up to 50 wt %) in the gel network, the gels demonstrated a capacity of 17.1 mmol Pb/g aerogel (3543 mg/g), and this could be augmented to 22.5 mmol Pb/g aerogel (4593 mg/g) by modifying the synthesis to reduce CaCO 3 content to ca. 15 wt %. Moreover, the selectivity of CaS aerogels toward Pb 2+ ions is high, as evidenced by little-to-no change in the distribution constant (K d ∼ 10 4 ) in the presence of competing ions (1 M) such as Na + , Mg 2+ , and Ca 2+ . During remediation with low concentrations (100 ppb) of Pb 2+ with CaS aerogels, the level of Pb 2+ dropped to 5.4 ppb (below the 15 ppb EPA limit) within 1 h with a 95.4% removal efficiency. In contrast to the CO 2 supercritically dried aerogels, lower surface area ambient dried gels (xerogels) only remove 40% of the lead ions from a 100 ppb solution, saturating within 1 h. The efficiency and rapidity of selective Pb 2+ uptake using CdS aerogels arise from a combination of a strong thermodynamic driving force for cation exchange (K eq = 2.5 × 10 27 ) and chemisorption along with favorable kinetics associated with the high surface area porous architecture. These results show that formation of high surface area metal chalcogenide aerogels by oxidative assembly to form nanocrystalline architectures, as previously demonstrated for II−VI and IV−VI semiconductors, can be extended to the more highly ionic alkaline earth sulfides.

Aerogels↗

DOE OSTI2023

Rapid Quantification of 237 U Specific Activity for Nuclear Forensics

In the event of an unattributed nuclear explosion, rapid assessment of the short-lived uranium isotope activity and mass can provide valuable information for subsequent forensic analysis. Rapid analysis in the field is enabled by using microfluidic chemistry and deployable instrumentation. Here, this work presents a flow chemistry system, controlled in LabVIEW, that integrates three functionalities: (1) selective extraction of uranium from the sample matrix via a 3D-printed supported liquid membrane module; (2) UV–visible absorbance spectrophotometry to measure the total uranium concentration in the strip flow; and (3) a portable CdTe γ-ray spectrometer coupled to a 3D-printed flow cell to measure 237 U activity concentration in the strip solution. The system was calibrated using standard solutions, and its functionality was demonstrated using a solution of depleted uranium spiked with 237 U. Uranium concentrations of 40–5000 μg/mL were directly quantified online using a 100 mm optical flow cell, while concentrations of 0.5–10 μg/mL were quantified online using a colorimetric reagent. The mass concentration measurement takes approximately 60 min while the activity concentration via γ-ray spectrometry varies depending on the activity of 237 U, with 1 kBq/mL requiring about 30 min of acquisition time to obtain <10% uncertainty at 1σ. This platform provides a fieldable approach for quantifying uranium mass and radioactivity relevant to postdetonation nuclear debris.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

A Rapid Microfluidic Neptunium Extraction Using a Supported Liquid Membrane Module

Extraction of neptunium from acidic matrices is important for its quantification, but its complex redox chemistry can cause variable yields. This study develops a microfluidic redox extraction for rapidly separating neptunium from submilliliter samples, achieving up to 90% process yield in less than 10 min for samples as small as 100 μL, with over 97% steady-state yield achieved after 20 min. It uses a supported liquid membrane module loaded with 30 vol % tributyl phosphate in n-dodecane, which performs forward- and back-extractions in a single, continuous step. Neptunium is first oxidized to +6 for extraction and then reduced during stripping. Bromate was selected as an oxidant over permanganate for its greater compatibility with the organic phase, achieving complete oxidation in under 30 s. Ascorbic acid and hydrogen peroxide were both effective reductants. Finally, the system’s high yield and rapid kinetics make it promising for future separations from complex mixtures.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗