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At least 145 records · Page 8

Fungal elemental profiling unleashed through rapid laser-induced breakdown spectroscopy (LIBS)

Elemental profiling of fungal species as a phenotyping tool is an understudied topic and is typically performed to examine plant tissue or non-biological materials. Traditional analytical techniques such as inductively coupled plasma–optical emission spectroscopy (ICP-OES) and inductively coupled plasma–mass spectrometry (ICP-MS) have been used to identify elemental profiles of fungi; however, these techniques can be cumbersome due to the difficulty of preparing samples. Additionally, the instruments used for these techniques can be expensive to procure and operate. Laser-induced breakdown spectroscopy (LIBS) is an alternative elemental analytical technique—one that is sensitive across the periodic table, easy to use on various sample types, and is cost-effective in both procurement and operation. LIBS has not been used on axenic filamentous fungal isolates grown in substrate media. In this work, as a proof of concept, we used LIBS on two genetically distinct fungal species grown on a nutrient-rich and nutrient-poor substrate media to determine whether robust elemental profiles can be detected and whether differences between the fungal isolates can be identified. This data set contains the raw LIBS spectral data for the summarized results described inRush, et. al. 2024

elemental profiling↗

Fungal elemental profiling unleashed through rapid laser-induced breakdown spectroscopy (LIBS)

ABSTRACT Elemental profiling of fungal species as a phenotyping tool is an understudied topic and is typically performed to examine plant tissue or non-biological materials. Traditional analytical techniques such as inductively coupled plasma–optical emission spectroscopy (ICP-OES) and inductively coupled plasma–mass spectrometry (ICP-MS) have been used to identify elemental profiles of fungi; however, these techniques can be cumbersome due to the difficulty of preparing samples. Additionally, the instruments used for these techniques can be expensive to procure and operate. Laser-induced breakdown spectroscopy (LIBS) is an alternative elemental analytical technique—one that is sensitive across the periodic table, easy to use on various sample types, and is cost-effective in both procurement and operation. LIBS has not been used on axenic filamentous fungal isolates grown in substrate media. In this work, as a proof of concept, we used LIBS on two genetically distinct fungal species grown on a nutrient-rich and nutrient-poor substrate media to determine whether robust elemental profiles can be detected and whether differences between the fungal isolates can be identified. Our results demonstrate a distinct correlation between fungal species and their elemental profile, regardless of the substrate media, as the same strains shared a similar uptake of carbon, zinc, phosphorus, manganese, and magnesium, which could play a vital role in their survival and propagation. Independently, each fungal species exhibited a unique elemental profile. This work demonstrates a unique and valuable approach to rapidly phenotype fungi through optical spectroscopy, and this approach can be critical in understanding these fungi's behavior and interactions with the environment. IMPORTANCE Historically, ionomics, the elemental profiling of an organism or materials, has been used to understand the elemental composition in waste materials to identify and recycle heavy metals or rare earth elements, identify the soil composition in space exploration on the moon or Mars, or understand human disorders or disease. To our knowledge, ionomic profiling of microbes, particularly fungi, has not been investigated to answer applied and fundamental biological questions. The reason is that current ionomic analytical techniques can be laborious in sample preparation, fail to measure all potential elements accurately, are cost-prohibitive, or provide inconsistent results across replications. In our previous efforts, we explored whether laser-induced breakdown spectroscopy (LIBS) could be used in determining the elemental profiles of poplar tissue, which was successful. In this proof-of-concept endeavor, we undertook a transdisciplinary effort between applied and fundamental mycology and elemental analytical techniques to address the biological question of how LIBS can used for fungi grown axenically in a nutrient-rich and nutrient-poor environment.

59 BASIC BIOLOGICAL SCIENCES↗

Measurement of Magnetic Field using Doppler-Free Saturation Spectroscopy (DFSS) in C-2W FRC Plasma

The Cooperative Research and Development Agreement (CRADA) between Oak Ridge National Laboratory (ORNL) and TAE Technologies (TAE) focused on implementing an existing mobile Doppler-free saturation spectroscopy (DFSS) diagnostic to determine the direction of the equilibrium magnetic field within TAE’s C-2W field-reversed configuration (FRC) fusion device. Non-perturbative measurements of magnetic fields in the core of FRCs can provide critical information needed to constrain equilibrium models and for the continued advancement of the fusion research program at TAE. DFSS is a well-established, laser-based absorption spectroscopy technique used to suppress inhomogeneous (Doppler) broadening and reveal the Zeeman fine structure of the target emission lines. The collaboration involved the use of ORNL’s recently constructed mobile DFSS diagnostic. The DFSS diagnostic was shipped and installed on C- 2W in February 2023. TAE’s expertise was used to design and construct the mechanic support structures required to mount the optical hardware on C-2W. Additionally TAE provide critical input to minimize the noise imposed on the DFSS signal by vibrations of the mechanic support structure during operations. DFSS data was obtained for over 500 C-2W shots and will continue until the expiration of this CRADA on September 30 th 2023. Over the course of this work, significant progress was made to maximize the signal to noise (SNR) ratio. Analysis of recently acquired data is on-going, however, initial indications are highly suggestive that a DFSS signal above background has been successfully acquired in C-2W.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Structural features of early fuel cycle taggant incorporation for intentional nuclear forensics

To develop strategies for incorporating transition metal taggants (Fe, Cr, and Ni) into oxide fuels and to understand how these taggant candidates persist through early fuel cycle processes, synthetic procedures are modified from established production routes to yield intentionally tagged early fuel cycle intermediates including uranyl nitrate hexahydrate (UNH, UO 2 (NO 3 ) 2 ·6H 2 O), uranyl peroxide tetrahydrate (studtite, UO 2 O 2 ·4H 2 O), and uranyl peroxide dihydrate (metastudtite, UO 2 O 2 ·2H 2 O). First, Fe, Cr, and Ni nitrate solutions are introduced to an aqueous solution of UNH followed by precipitation to produce tagged UNH. Then, studtite is precipitated from UNH followed by dehydration to metastudtite. Structural influences of taggant incorporation within all synthesized phases are investigated using powder X-ray diffraction (PXRD) and Raman spectroscopy to provide insight into crystallographic modifications resulting from the addition of tags to these early fuel cycle materials and elucidate the chemical form of taggants introduced at these stages. The possibility of segregation of taggant species into discrete phases within U matrices was examined using scanning electron microscopy with energy dispersive X-ray spectroscopy. Taggant concentrations in solid-phase materials were determined using inductively coupled plasma-optical emission spectroscopy. Observations from Raman spectroscopy and PXRD indicate that introducing transition metal tags during uranyl nitrate precipitation results in potential impurity phase segregation in UNH, but transition metal incorporation is suggested by results for tagged uranyl peroxide materials. Further, results from this study will inform strategies for optimizing taggant incorporation in UO 2 .

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Characterization of an imploding cylindrical plasma for electron transport studies using x-ray emission spectroscopy

We report here on the characterization of the conditions of an imploding cylindrical plasma by time-resolved x-ray emission spectroscopy. Knowledge about this implosion platform can be applied to studies of particle transport for inertial confinement fusion schemes or to astrophysical plasmas. A cylindrical Cl-doped CH foam within a tube of solid CH was irradiated by 36 beams (I total ~5×10 14 W/cm 2 , 1.5ns square pulse, and E total ~ 16.2kJ) of the OMEGA-60 laser to radially compress the CH toward the axis. The analysis of the time-resolved spectra showed that the compression can be described by four distinct phases, each presenting different plasma conditions. First the ablation of the cylinder is dominant; second, the foam is heated and induces a significant jump in emission intensities; third, the temperature and density of the foam reaches a maximum; and finally, the plasma expands. Ranges for the plasma temperature were inferred with the atomic physics code SCRAM (Spectroscopic Collisional-Radiative Atomic Model) and the experimental data have been compared to hydrodynamic simulations performed with the 2D code FLASH, which showed a similar implosion dynamic over time.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Supramolecular Assembly of Multielement Ribbon-like Structures Derived from Halide Perovskites

Halide perovskites are crucial materials with broad applications owing to their exceptional optoelectronic properties. Vacancy-ordered double perovskites, featuring highly tunable transition metal sites, enable controllable optoelectronic properties through multielement compositional design. Here, in this study, we introduced 18-crown-6 into the vacancy-ordered double perovskites system and developed two-dimensional ribbon-like single crystals (18C6@K) 2 {PtSnTeIrRe} 1 Cl 6 via an antisolvent supramolecular assembly method, demonstrating morphology modulation through multielement composition design. The crystals crystallize in the centrosymmetric space group $P\bar{1}$. The dumbbell-shaped structural units (crown ether@A)2MX6 pack along a and b axes to form a 2-dimensional (2D) monolayer, and these monolayers further stack along the c axis to generate the ribbon-like single crystals. Energy-dispersive X-ray spectroscopy (EDX) qualitatively confirmed the uniform distribution of the five transition metals throughout the crystal, while inductively coupled plasma atomic emission spectroscopy (ICP–AES) quantitatively verified their atomic ratios. We further investigated the origin of the morphology, distinct from the previously reported cube-like single crystals with the $R\bar{3}$ space group. When acetonitrile was used as the solvent, three-dimensional crystals with $R\bar{3}$ symmetry were obtained, whereas dimethylformamide (DMF) was essential for forming two-dimensional ribbon-like single crystals. The essential role of DMF could be ascribed to its capability to maintain a higher concentration of the building blocks. Moreover, Ir 4+ and Pt 4+ cations also played critical roles in inducing the two-dimensional ribbon-like morphology. The three-element (18C6@K) 2 {PtSnTe}1Cl 6 single crystals exhibited bright yellow emission under 375 nm laser excitation, demonstrating the tunability of optoelectronic properties of this class of material.

Zhu, Heqing [University of California, Berkeley, C↗

Effects of solvent formulations in electrolytes on fast charging of Li-ion cells

Improving the fast charging performance of lithium ion batteries (LIBs) has the promise to increase the widespread adoption of electric vehicles (EVs). Electrolyte development plays an important role in enabling fast charging. In this study, fast charging performance of LIBs is studied with different electrolytes of 1.2 M LiPF 6 in Ethylene Carbonate (EC)/Ethyl Methyl Carbonate (EMC)/co-solvents at 30/50/20 wt%. The co-solvents are methyl acetate (MA), ethyl acetate (EA), ethyl formate (EF), dimethyl carbonate (DMC) and EMC. Long term cycling performance under fast charging shows different capacity retention behaviors for different co-solvents. The structural changes in the electrode material are studied by X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD). The molarity changes in electrolyte is investigated by inductively coupled plasma-optical emission spectroscopy (ICP-OES). The electrode/electrolyte interfaces before and after fast charging are analyzed by X-ray photoemission spectroscopy (XPS). The characterization results are in good agreement with the long-term cycling performance. DMC shows the highest fast-charging capability among the five studied co-solvents due to its increased conductivity, improved electrode/electrolyte interface and stable electrode structural integrity.

25 ENERGY STORAGE↗

Core-flood Effluent and Shale Surface Chemistries in Predicting Interaction between Shale, Brine, and Reactive Fluid

We report field and laboratory observations to date indicate that the efficiency of hydraulic fracturing, as it relates to hydrocarbon recovery, depends significantly on geochemical alterations to rock surfaces that diminish accessibility by partial or total plugging of the pore and fracture networks. This is caused by mineral scale deposition such as coating of fracture surfaces with precipitates, particle migration, and/or crack closure due to dissolution under stress. In reactive flow-through experiments, mineral reactions in response to acidic fluid injection significantly reduced system porosity and core permeability. The present study focuses on changes to fluid chemistry and shale surfaces (inlet and fracture walls) resulting from shale-fluid interactions and integrating these findings for an improved estimate of transport-related consequences. The reacted shale surfaces were examined by spatially-resolved scanning electron microscopy - energy dispersive spectroscopy (SEM-EDS) analysis. Importantly, inductively coupled plasma - mass spectrometry/optical emission spectroscopy (ICP-MS/OES) was utilized to probe the chemical evolution of the core-flood effluents. The three study cores selected from the Marcellus formation represent different mineralogies and structural features. In flow-through experiments, lab-generated brine and HCl-based fracture fluid (pH=2) were injected sequentially under effective stress (up to 500 psi) at reservoir temperature (80°C). SEM-EDS results confirmed by the ICP concentration trends showed significant Fe hydroxide precipitates in clay- and pyrite-rich outcrop samples due to partial oxidation of Fe-bearing phases in the case of intrusion of low salinity water-based fluids. Porosity reduction in the MSEEL (Marcellus Shale Energy and Environmental Laboratory) carbonate-rich sample is related to compaction of cores under stress due to matrix softening with substantial dissolution, and pore-filling by hydroxides, as well as barite and salts. Despite the same fluid compositions and experimental conditions used for both MSEEL samples, barite precipitation was much more intense in the MSEEL clay-rich sample due to its greater sorption capacity and additional sulfate source as well as fissile nature with multiple lengthwise cracks. ICP tests revealed time-resolved concentration trends in produced brine and reactive fluids that in turn complemented the pre-/post-reaction SEM-EDS observations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

First field test of a novel optical gas analyser in the exhaust of Wendelstein 7-X

A novel optical gas analyser, designed for isotope-resolved exhaust composition measurement, was field-tested at Wendelstein 7-X (W7-X) to validate its laboratory-proven concept under operational fusion experiment conditions. The system, Optix, comprises a cold cathode remote plasma generator and a high-resolution Fabry–Perot spectrometer and was deployed in the exhaust line of W7-X during the OP2.3 campaign. The injection of 3 He and 4 He for minority ion-cyclotron heating provided a test case for helium isotope discrimination. Despite limitations due to background gas and low partial pressures of the target species, isotope-resolved spectral signatures were successfully observed, demonstrating the fundamental viability of the Optix approach. Additionally, the spectrometer was evaluated for plasma emission measurements from both core and edge sightlines. While helium line emission was detectable, interpretation was hindered by complex background signals, highlighting the benefits of controlled remote plasma generators for spectroscopy. This first deployment provides critical insight into pressure requirements, spectral resolution, and operational constraints, informing future applications of optical exhaust diagnostics in fusion devices.

magnetic confinement fusion↗

Real-time monitoring of trace noble gases using laser-induced breakdown spectroscopy—An investigation of the impact of bulk gas on plasma properties and sensitivity

The impact of Ar and He bulk gases on laser-induced breakdown spectroscopy (LIBS) real-time monitoring of trace Xe and Kr was assessed. LIBS is being developed as a monitoring tool for measuring noble gas transport in molten salt systems, in which traditional sensors may face challenges associated with radiation, corrosive materials, and/or mixed phases. The plasma temperature and electron densities of LIBS plasmas were measured in both static and various flowing Ar and He streams (0–5 L min −1 ). The use of an Ar bulk gas resulted in higher plasma temperature, greater electron densities by an order of magnitude, and extended plasma lifetime compared with when He bulk gas was used. Gas flow rate was found to have little impact on plasma temperature; however, its effect on electron density was significant, indicating the need to consider flow rate–specific models. Matrix effects on emission peaks were reported for both bulk gases. Due to these matrix effects, multivariate models were developed for Xe and Kr ranging from 0 to 700 ppm in both bulk gases. Although the predictive behavior was similar (root mean square error of prediction ranging from 11.1 to 20.6 ppm), the limits of detection were superior in He (Xe: 22.9 ppm, Kr: 30.4 ppm). Furthermore, these models were employed in demonstrative real-time tests (>1 h), which showed strong predictive precision (relative standard deviation <5 %) regardless of the bulk gas. Ultimately, this study provides a guide for the considerations required when developing gaseous LIBS models for real-time monitoring.

Gas flow effects↗

Molecular Iodine Interactions with Fe, Ni, Cr, and Stainless Steel Alloys

The adsorption behavior of molecular iodine is important for understanding the spread of radioiodine in a nuclear accident. Prior experiments indicate that, in addition to the interaction with Fe, molecular iodine [i.e., I 2(g) ] also interacts with the next most abundant components of austenitic stainless steel (i.e., Ni, and Cr) at room temperature. Here, we investigate iodine adsorption on Fe, Ni, and Cr while focusing on understanding the variables affecting adsorption as well as the iodine compounds that are formed during adsorption. Scanning electron microscopy and energy-dispersive X-ray spectroscopy were used to characterize the surfaces of exposed metal particles and aid in the understanding of the morphology and chemistry of iodine interactions with the substrates. Inductively coupled plasma optical emission spectroscopy was used to detect low levels of metal iodides and X-ray photoelectron spectroscopy was used to confirm the formation of the metal iodides. The role of environmental factors (e.g., humidity and oxygen content) for iodine adsorption on metal substrates is addressed. The individual metals demonstrated formation of metal iodides for Fe and Ni particles from interaction with I 2(g) . The formation of metal iodides may indicate the affinity of iodine for the respective metal. In this study, the iodine affinities ranked Fe > Ni > Cr as determined by the quantity of chemisorbed iodine. This trend is also supported by the distributions and proportions of metals in the corrosion product of the stainless steels. The exposures without oxygen and humidity indicate the potential of a multistep iodine adsorption process where iodine first attacks the oxide layer and then chemisorbs to the exposed metal.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Pulsed contact glow discharge electrification for online material quantification

Real-time elemental analysis of liquids in extreme environments remains a significant challenge for sensor development, particularly in applications such as advanced nuclear reactors. Plasma-based optical emission spectroscopy offers a promising solution. In this study, we investigate pulsed contact glow discharge electrolysis (CGDE) as an alternative plasma generation method for emission-based material quantification. Using aqueous NaCl solutions, we examine the role of discharge polarity on plasma behavior, emission characteristics, and spectral output. Our results demonstrate that cathodic discharges generate more energetic plasmas, enabling the detection of ionic species such as cerium, while anodic discharges favor atomic emission. These findings reveal a potential dual-mode sensing capability controlled by circuit configuration rather than hardware changes. Through synchronized measurements of emission, current, bubble, and spectral dynamics, we present a model in which electron emission and ohmic heating drive plasma formation. This model enhances our understanding of pulsed-CGDE and supports its potential as a versatile, adaptable platform for future deployment in high-temperature liquids such as molten salts.

98 - NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL↗

Ionization and temperature measurements in warm dense copper using x-ray absorption spectroscopy

We detail experimental results inferring ionization and temperature for warm dense copper plasmas at several times solid density (15–25 g/cm 3 ) and temperatures of 10–21 eV. Experiments performed at the OMEGA Laser Facility generate uniform warm dense matter conditions via symmetric shock compression of a buried copper layer. The plasma is probed with a laser-generated x-ray source to collect the K-shell x-ray absorption spectrum. Fitting bound-bound absorption contributions from constituent charge states of copper provides an estimated $\overline{Z}$ of approximately 4–7 for these warm dense copper plasmas. We find that these partially ionized plasmas have K-edge shifts of 12–30 eV and bound-bound resonance 1s → 3p absorption shifts of 4–26 eV with respect to the cold K edge. This study provides necessary experimental data to improve ionization and opacity models in the warm dense matter regime.

42 ENGINEERING↗

The influence of laser energy on deuterium emission characteristics from a Zircaloy-4 plasma

Laser-produced plasma coupled with optical emission spectroscopy (OES) is a promising technique for detecting certain isotopes, with unique capabilities such as standoff and rapid detection and minimal to no sample preparation requirements. The key figure-of-merit for isotopic analysis using optical spectroscopy tools is the linewidth relative to the isotope shift. Although the isotopes of hydrogen (1H, 2H, and 3H) possess large isotopic shifts (1H–2H ≈ 180 pm, 1H–3H ≈ 240 pm), being a light element, the H transitions are susceptible to various broadening mechanisms in the plasma environment. One of the critical parameters that influence the linewidth of a transition in an LPP is the incident laser energy. In the present study, we evaluated the role of laser energy on plume expansion dynamics, deuterium emission intensity, and linewidth in a nanosecond laser-produced Zircaloy-4 plasma. The changes in 2Hα emission intensity and linewidth were investigated for varying laser fluence and time after plasma onset. Spatially resolved and spatially integrated OES were performed and compared to investigate the emission spectral features and linewidth of 2Hα. Monochromatic two-dimensional time-resolved imaging was also performed to understand the morphology of the deuterium and protium emission relative to all species in the plume. Our results showed that 1Hα and 2Hα emissions predominantly occur closer to the target. Measurements of 2Hα linewidth approached similar values at later times of plasma evolution regardless of the laser energy. The linewidths of the 2Hα transition showed insignificant differences between spatially resolved and spatially integrated measurements.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Implementation of a Doppler-Free Saturation Spectroscopy (DFSS) Diagnostic for Helicon Wave Electric Field Vector Measurement in Edge Plasma in DIII-D

A laser-based technique known as Doppler-free saturation spectroscopy (DFSS) has been designed, fabricated, and installed on the DIII-D National Fusion Facility to measure the helicon wave electric field vector in the edge plasma. These experimental measurements quantify phenomena resulting in decreased current drive efficiency due to wave/edge plasma interactions. This implementation of DFSS on DIII-D is the first of its kind on a tokamak and thus presents unique engineering challenges, including integration of the system onto an existing multidiagnostic port flange without impacts to system serviceability, as well as maintaining precise laser alignment over a 2-m distance during disruptions and thermal drift of the vessel. Further, these challenges were resolved using innovative design approaches such as a novel decoupled shutter system to facilitate serviceability of the in-vessel mirror assemblies without the need for personnel vessel entry, as well as an ex-vessel piezo-mirror-based optical system for laser beam shaping and real-time steering of the measurement location. The solutions to these engineering challenges were demonstrated during the successful installation and operation of these diagnostic components during the 2022 DIII-D vent and subsequent experimental campaign.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Ground state rotational and kinetic temperatures of C 2 molecules in a laser-produced plasma

This study presents an experimental comparison between rotational and kinetic temperatures of molecular species in a laser-produced plasma, utilizing tunable laser absorption spectroscopy. We analyzed high-resolution and time-resolved absorption spectra of 31 rotational transitions within the Phillips A 1 II u –X 1 Σ g 3-0 band of the C 2 molecule, measured from a laser-produced graphite plasma in ~2 Torr argon, within the 771–781 nm spectral range. Spectral fitting provided quantitative state column densities of C 2 rotational energy levels in the ground electronic and vibrational states. Boltzmann analysis revealed thermalized rotational distributions showing rotational temperatures decreasing from 3000 to 600 K within 5–500 μs following the onset of the laser plasma. The measured kinetic and rotational temperatures of C 2 molecules are comparable, suggesting that collisional processes in the laser-produced plasma are sufficient to maintain thermal equilibrium between the C 2 molecules and the Ar background gas.

Absorption spectroscopy↗

Synthesis and Functionalization of Coal Fly Ash-Derived Zeolites for Boron Removal From Wastewater

There are hundreds of both active and unused surface impoundments in the United States containing coal combustion residuals (CCRs) produced by coal-fired power plants which can leach toxic elements into surface and groundwater. Therefore, the development of efficient means for both the clean-up of surface impoundments and for deriving economically viable products from CCRs are urgent tasks for researchers. Herein, a microwave-assisted strategy is presented for converting a common coal combustion residual, coal fly ash (CFA), into zeolite-based sorbents for boron (B) removal from wastewater. Specifically, CFA constitutes the main source of Si and Al ions to produce zeolite type-A and the resulting sorbent subsequently undergoes simple cation exchange with Ca to enhance its B adsorption capacity. Structure and composition of the sorbents were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), inductively coupled plasma (ICP)-mass spectrometry (MS), and ICP-optical emission spectroscopy (OES). The Ca-modified zeolite sorbent derived from CFA exhibits comparable B removal capacity with similar commercial zeolites.

Muldoon, Patrick↗