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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Xenon Detection Using Double-Pulse Laser-Induced Breakdown Spectroscopy

Laser-induced breakdown spectroscopy has been proposed as a diagnostic tool for fuel failure monitoring in helium-cooled fast reactor designs. Here, we show preliminary results which indicate that using double-pulse laser induced breakdown spectroscopy, a sub-ppm sensitivity for xenon in a helium ambient can be achieved. We additionally propose future studies which could help elucidate the mechanisms which lead to the observed signal enhancement.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2025

Analysis of Off-Gas Streams from Small- and Large-Scale Sparging Salt Vessels using Laser-Induced Breakdown Spectroscopy

Laser-induced breakdown spectroscopy (LIBS) is being developed as an analytical monitoring tool for molten salt reactor (MSR) systems. A mobile LIBS platform was configured on a small-scale salt vessel (~100 g of salt) and then transported 0.6 km to successfully monitor an engineering-scale pumped salt loop (~100 kg of salt). Several studies on monitoring salt aerosols, hydrogen isotopes, and noble gases were performed on the small-scale system. All these studies were then implemented for monitoring various tests on the engineering-scale loop. Aerosolized salts from both the storage tank and pump bowl were monitored using LIBS to assess bulk salt analyte ratios (Mg, Na, K) and evaluate impurities (H, O, Ca). In addition to monitoring salt aerosols, LIBS was used in tandem with a residual gas analyzer (RGA) and a Raman spectroscopy system to detect hydrogen isotopes as they were sparged through and subsequently depleted from the loop storage tank. Lastly, a similar test with noble gases (100 ppm Kr, 1000 ppm Xe) was performed, in which LIBS demonstrated a faster response than the RGA used in-line. The tests and results are summarized in this report with detailed publications to follow. Key takeaways are listed in the conclusion of the report.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2025

Single particle trace element analysis of uranium oxide standards with laser-induced breakdown spectroscopy

Femtosecond Laser-Induced Breakdown Spectroscopy (LIBS) was used to analyze over 1000 individual particles of uranium oxide trace element standard CRM124. Intra-granular analysis showed elemental concentrations were consistent across different surface locations on each uranium grain. However, inter-granular comparison revealed large heterogeneity between different grains of the same sample. By comparing the distribution of elemental concentrations across the particle populations, we were able to correctly identify a manufacturing process involving wet chemistry, rather than a dry mixing of two powders to give an overall chemical average. In conclusion, this demonstrates the utility of LIBS as a large-scale single particle analysis tool for nuclear forensics.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Radiative transition probabilities of neutral and singly ionized Europium estimated by laser-induced breakdown spectroscopy (LIBS)

Laser-induced breakdown spectroscopy (LIBS) is a versatile technique for compositional analysis for solids, liquids, or gasses. LIBS is an asset for the quantitative or qualitative analysis of resource limited materials like actinides and rare earths because it is quasi-nondestructive. Two Eu 2 O 3 pellets were synthesized to be a test and validation set, respectively. Spectral lines identified from the National Institute of Standards and Technology database with fundamental data reported were used to form Saha-Boltzmann plots. The Saha-Boltzmann plots were used to determine the plasma temperatures and electron densities of the laser-induced plasmas for both samples. These Saha-Boltzmann plots were then used to calculate previously unreported transition probabilities associated with identified peaks. Additionally, the transition probabilities presented in this paper provide the capability for calibration free LIBS to be performed more readily on europium samples and the spectroscopic analysis of stellar bodies. Eight previously unreported transition probabilities are presented in this paper; five for Eu I and three for Eu II. The transition probabilities for Eu I ranged from 0.172 to 7.38 × 10 7 s -1 and those for Eu II ranged from 1.56 to 6.75 × 10 7 s -1 .

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

Neptunium transition probabilities estimated through laser induced breakdown spectroscopy (LIBS) measurements

in tis report calibration free–laser induced breakdown spectroscopy (CF-LIBS) approaches are promising for the analysis of radioactive materials; however, a lack of reported fundamental properties for these materials is an obstacle to implementation. Spectra of laser induced plasmas containing Np and Sr, along with Saha–Boltzmann methods, were used to estimate the first reported transition probabilities (TPs) of Np. These TPs enabled the first attempt at CF-LIBS analysis of radioactive samples to predict Np/Sr ratios with a mean error of 3.86%. The presented methodology of TP estimation will be applied to the study of other actinides and allow broader applications of CF-15 LIBS in the nuclear field.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2025

Rapid spatial analysis of surrogate TRISO fuel particles using laser-induced breakdown spectroscopy image analysis

Laser-induced breakdown spectroscopy (LIBS) mapping enables rapid elemental and spatial analysis of solid samples. In this work, surrogate TRi-structural ISOtropic (TRISO) particles with various layers consisting of Zr, W, C, and Si were used to demonstrate the use of a new thickness measurement tool developed to analyze elemental images generated from LIBS maps. Zr particles with varying outer-layer thicknesses ranging from 16 to 32 μm were measured with scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS) and LIBS with both a complementary metal-oxide-semiconductor (CMOS) detector and an intensified charged coupled device (ICCD) detector. LIBS maps of particles were completed using CMOS and ICCD spectrometers with effective spatial resolutions of 4 and 2 μm, respectively. The novel thickness measurement tool identified layer regions within a LIBS map and then identified the locations of the boundaries between these layers. The tool then generated up to 1000 random profiles stemming radially from the center region, which were used to measure the layer thickness/radius. This image analysis tool demonstrated LIBS's ability to provide values comparable with SEM-EDS (3.7% relative difference) along with a 95% reduction in measurement time. Furthermore, the precision of these measurements was on par with the SEM-EDS measurements at <15% relative standard deviation. Following the analysis of the Zr particles, W particles with increased complexity (e.g., five versus three layers) were analyzed using both the CMOS and ICCD spectrometers simultaneously. The spatial dimensions were extracted with an average relative difference of 2.7% and an average relative standard deviation of 9%.

Andrews, Hunter B. [Oak Ridge National Laboratory ↗
DOE OSTI2020

Evaluation of analytical performance of double pulse laser-induced breakdown spectroscopy for the detection of rare earth elements

Double pulse laser-induced breakdown spectroscopy (DP-LIBS) in collinear configuration was demonstrated to enhance the signal intensity of three rare earth elements (REEs), Eu, Gd, Pr, and Y (Yttrium is included because of its similar chemical properties and occurrence in similar deposits as REE). Significant enhancement in spectral signals of all elements was observed with an aid of second laser. Two laser pulses of 1064 nm wavelength were employed in collinear geometry on the Pr 2 O 3 , Eu 2 O 3 , Gd 2 O 3 , and Y 2 O 3 pellets to obtain emission spectra. For selected strong emission lines of Eu and Gd signal enhancement was found to be 3 to 7-fold and that for Y and Pr lines was observed to be 3 to 13-fold compared to single-pulse laser-induced breakdown spectroscopy (SP-LIBS). Role of inter-pulse delay between two pulses in DP-LIBS was found to be very crucial. Furthermore, while comparing selected ionic and neutral lines, ionic lines were found to have larger signal enhancement in DP-LIBS at the experimental conditions used in this study.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Uranium corrosion characterization by handheld laser-induced breakdown spectroscopy

In this study, a commercial-off-the-shelf handheld laser-induced breakdown spectroscopy system was modified, calibrated and tested for discrimination between uranium oxide and uranium hydride when assessing uranium corrosion products. Operating parameters, system modifications, and onboard data analysis were developed to accomplish the analytical task. This work represents the first laser-induced breakdown spectroscopy analysis of bulk uranium hydride, a pyrophoric material, within an inert glovebox. Finally, the work shown here illustrates a rapid identification technique for uranium corrosion types from pure UO 2 or U 3 O 8 to pure UH 3 .

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2021

Filament-induced breakdown spectroscopy signal enhancement using optical wavefront control

Filament-induced breakdown spectroscopy (FIBS) is an analytical method that holds significant promise for remote sensing. In FIBS, it is desirable to maximize the intensity and improve the reproducibility of a selected spectroscopic feature. Here, we demonstrate the use of wavefront control in conjunction with a genetic algorithm in FIBS of metallic copper and show that this approach can increase the efficacy of filament-induced breakdown signal production. Through wavefront optimization, we enhance the intensity of a chosen characteristic spectroscopic feature of copper by a factor of approximately 3 when performing filamentation over a 1-meter distance. The relative standard deviation of signal intensity is reduced from ~17% to ~12% after optimization. We find that modification of the wavefront by introduction of astigmatism and coma maximizes the signal intensity, and these aberrations appear in two distinct trials of the genetic algorithm. We compare these findings to previous work on multiple filament control and discuss the possible mechanisms that lead to signal enhancement associated with both the beam amplitude and phase profile. A broader use of wavefront control with feedback may improve the performance of FIBS in remote sensing applications.

42 ENGINEERING↗
DOE OSTI2022

Determination of fluorine distribution in shark teeth by laser-induced breakdown spectroscopy

Quantifying the chemical composition of fast-growing hard tissues in the environment can shed valuable information in terms of understanding ecosystems both prehistoric and current. Changes in chemical composition can be correlated with environmental conditions and can provide information about the organism's life. Sharks can lose 0.1 to 1.1 teeth/day, depending on species, which offers a unique opportunity to record environmental changes over a short duration of time. Shark teeth contain a biomineral phase that is made up of fluorapatite [Ca 5 (PO 4 ) 3 F], and the F distribution within the tooth can be correlated to tooth hardness. Typically, this is determined by bulk acid digestion, energy-dispersive X-ray spectroscopy (EDS), or wavelength-dispersive spectroscopy. Here we present laser-induced breakdown spectroscopy (LIBS) as an alternative and faster approach for determining F distribution within shark teeth. Using a two-volume laser ablation chamber (TwoVol3) with innovative embedded collection optics for LIBS, shark teeth were investigated from sand tiger (Carcharias Taurus), tiger (Galeocerdo Cuvier), and hammerhead sharks (Sphyrnidae). Fluorine distribution was mapped using the CaF 603 nm band (CaF, Β 2 Σ + → X 2 Σ + ) and quantified using apatite reference materials. In addition, F measurements were cross referenced with EDS analyses to validate the findings. Distributions of F (603 nm), Na (589 nm), and H (656 nm) within the tooth correlate well with the expected biomineral composition and expected tooth hardness. This rapid methodology could transform the current means of determining F distribution, particularly when large sample specimens (350 mm 2 , presented here) and large quantities of specimens are of interest.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Application of deep learning to single-shot gas-phase laser-induced breakdown spectroscopy

Single-shot fs laser-induced breakdown spectroscopy (LIBS) has the potential to capture ns-scale electrode desorption phenomena in pulsed power fusion drivers. However, the successful implementation of the diagnostic for this purpose is challenging, as it requires interpreting single-shot measurements collected from low-density gas mixtures. In this work, we demonstrate the efficacy of a Bayesian-optimized convolutional neural network (CNN) to interpret these measurements. We generated 256 distinct measurement conditions at relevant gas pressures ranging from 80–530 mTorr by mixing 100–250 sccm H 2 and 50–200 sccm CH 4 in increments of 10 sccm. Despite the considerable overlap between signals separated by 20 sccm, the CNN is able to predict the H 2 flow rate with a root-mean-square error (RMSE) of 15.9 sccm and the CH 4 flow rate with an RMSE of 12.0 sccm. The average relative prediction error is <9% for each gas and largely remains below or near 10%.

Brown, Nathan Parnell [Sandia National Lab. (SNL-N↗
DOE OSTI2025

Single-shot femtosecond laser-induced breakdown spectroscopy in low-density gases

Single-shot fs laser-induced breakdown spectroscopy (LIBS) has been used to interrogate low-density gases of H 2 ⁠, CH 4 ⁠, CO 2 ⁠, and H 2 O ranging from 0.5 × 10 15 to 9.1 × 10 15 cm −3 (15–275 mTorr). Strong spectral signatures were observed above the noise baseline for each test gas at all densities considered. Unique molecular signatures were observed for both CH 4 and CO 2 along with atomic features for each gas. The LIBS intensity response with respect to density was determined for each species using Voigt lineshape fitting or numerical integration. Finally, the collection and analysis of LIBS spectra of composite mixtures of CH 4 –CO 2 and CH 4 –H 2 demonstrates that the extraction of individual densities from gas mixtures is feasible at low densities.

Artificial neural networks↗
DOE OSTI2025

Geochemistry of Mars with Laser-Induced Breakdown Spectroscopy (LIBS): ChemCam, SuperCam, and MarSCoDe

Laser-induced breakdown spectroscopy (LIBS) has been used to explore the chemistry of three regions of Mars on respective missions by NASA and CNSA, with CNES contributions. All three LIBS instruments use ~100 mm diameter telescopes projecting pulsed infrared laser beams of 10–14 mJ to enable LIBS at 2–10 m distances, eliminating the need to position the rover and instrument directly onto targets. Over 1.3 million LIBS spectra have been used to provide routine compositions for eight major elements and several minor and trace elements on >3000 targets on Mars. Onboard calibration targets common to all three instruments allow careful intercomparison of results. Operating over thirteen years, ChemCam on Curiosity has explored lacustrine sediments and diagenetic features in Gale crater, which was a long-lasting (>1 My) lake during Mars’ Hesperian period. SuperCam on Perseverance is exploring the ultramafic igneous floor, fluvial–deltaic features, and the rim of Jezero crater. MarSCoDe on the Zhurong rover investigated for one year the local blocks, soils, and transverse aeolian ridges of Utopia Planitia. The pioneering work of these three stand-off LIBS instruments paves the way for future space exploration with LIBS, where advantages of light-element (H, C, N, O) quantification can be used on icy regions.

47 OTHER INSTRUMENTATION↗
DOE OSTI2022

Monitoring Noble Gases (Xe and Kr) and Aerosols (Cs and Rb) in a Molten Salt Reactor Surrogate Off-Gas Stream Using Laser-Induced Breakdown Spectroscopy (LIBS)

In this study with surrogate materials we show that laser-induced breakdown spectroscopy (LIBS) is a robust tool with promising capability toward monitoring gaseous (Xe and Kr) and aerosol (Cs and Rb) species in an off-gas stream from a molten salt reactor (MSR). MSRs will continually evolve fission products into the cover gas flowing across the reactor headspace. The cover gas entrains Xe and Kr gases, along with aerosol particles, before passing into an off-gas treatment system. Univariate models of Xe and Kr peaks showed a strong correlation to concentration indicated by their coefficients of determination of 0.983 and 0.997, respectively. Multivariate models were built for all four analytes using partial least squares regression coupled with preprocessing steps including normalization, trimming, and/or genetic algorithm derived filters. The models were evaluated by predicting the concentrations of the analytes in four validation samples, in which all calibration models were successfully validated at a confidence interval of 99.9%. Finally, pressure controllers were used to regulate the mass flow rate of Kr flowing into the measurement cell in sinusoidal and stepwise waveforms to test the real-time monitoring capabilities of the regression models. Both univariate and partial least squares Kr models were able to successfully quantify the gas concentration in the real-time evaluation. The root mean squared error of prediction (RMSEP) values for these real-time tests were calculated to be 0.051, 0.060, and 0.121 mol% demonstrating the measurement systems’ capability to perform online monitoring with acceptable accuracy.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2023

Concept for an irradiation experiment to test a laser-induced breakdown spectroscopy off-gas sensor for molten salt systems

This paper focuses on laser-induced breakdown spectroscopy (LIBS) as an off-gas sensor and details a conceptual irradiation experiment to evaluate its performance in an environment that is more realistic of an operational molten salt reactor (MSR). MSRs are a promising advanced nuclear design that use high-temperature liquid salts as the coolant, fuel, or a combination of both. They will generate and subsequently evolve fission products into the reactor headspace during operation. These evolved fission products will necessitate an online off-gas system to treat the reactor cover gas before recycling it to the core. Such a system, especially during the early deployment phase, will benefit from online sensors to inform operators of the treatment system’s performance. Optical spectroscopy is well-suited to fit this task as it can be remotely deployed using fiber-optics and can detect most species at high frequencies. LIBS can detect nearly every element on the Periodic Table, stable or radioactive, making it an ideal candidate. The provided conceptual experiment discusses the facility requirements, salt capsule design, and detailed testing campaigns with corresponding simulated LIBS spectra.

47 OTHER INSTRUMENTATION↗
DOE OSTI2024

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↗
DOE OSTI2023

Elemental fractionation in aerosol laser-induced breakdown spectroscopy with nanosecond and femtosecond laser ablation

For the purpose of realizing atmospheric radiation plume tracking, laser-induced breakdown spectroscopy (LIBS) was performed to characterize Cs atomic emissions from airborne nanoparticles in a binary particle matrix using nanosecond and femtosecond laser ablation. As a surrogate to multi-element nuclear fallout particulates, both Cs and Na solutions were mixed with Cu at a 1:1.45 M concentration ratio and aerosolized to study elemental fractionation in atomic emissions, revealing Na I resonance emissions are enhanced whereas Cs I resonance emissions are reduced with Cu present despite sharing similar electronic and chemical properties. Femtosecond laser ablation reduced elemental fractionation effects by more than 50% while retaining the same temporal fractionation trends for Cs and Na. The origin of elemental fractionation in aerosol LIBS was further investigated using Al and Ti aerosols which revealed that the particle matrix induces changes to the local plasma temperature, population of atomic states, and subsequent molecular association and emission.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗