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All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Lead Isotope Fingerprinting of Nanoscale Mineral Particles via Single Particle Inductively Coupled Plasma Mass Spectrometry

Determining lead (Pb) isotopic ratios is of broad interest across chemical disciplines for source tracing and age determinations, but the technique is inherently limited when multiple sources of Pb are present in a single sample. Single particle methods offer a solution to directly resolve multiple distinct isotopic ratios within individual samples. In this study, single particle inductively coupled plasma-mass spectrometry (spICP-MS) was performed using time-of-flight (TOF) and multicollector (MC)-based platforms to measure the Pb isotopic composition of individual nanoscale particles. Distinct Pb isotope ratios were measured in particles from four powdered galena samples of different origins (average single-particle 206Pb/207Pb ratios ranging from 0.91 to 1.28) using both the TOF and the MC-based platforms. Differentiation of galena particles in a mixture (liberated grains and those hosted in a silicate matrix) was possible due to detecting their unique multielemental fingerprints. The differing behavior of the two galena samples during digestion was investigated; undigested galena particles trapped within silicate minerals were detected using spICP-MS, which has implications for Pb recovery in bulk-scale isotopic analysis. The multinuclide detection capability of the ICP-TOF-MS instrument allowed for the simultaneous detection of secondary constituent elements within the nanoparticles and the identification of multiple populations of isotopically distinct Pb-bearing particles in a copper ore sample, whereas the increased sensitivity of the MC instrument enabled quantification of 204Pb, allowing differentiation using multiple isotopic ratios. A single particle isotope ratio analysis module was developed within an open-source spICP-TOF-MS data processing platform, enabling its adoption across chemical disciplines.

Goodman, Aaron J. [University of Montreal, Quebec,↗
DOE OSTI2026

Single particle – MC-ICP-MS for isotopic analysis of uranium particles

Single particle – multi-collector – inductively coupled plasma – mass spectrometry (SP-MC-ICP-MS) was employed to measure a suspension of 1 µm U3O8 particles (∼1.3 pg total U/particle) to determine their individual isotopic compositions of 234U/238U, 235U/238U, and 236U/238U. The effects of different detector combinations for 235U and 238U, including secondary electron multipliers (SEM) and Faraday detectors (1011 and 1013 Ω amplifiers), were explored for accuracy and precision optimization on the observed 235U/238U. The minor isotopic ratios (i.e., 234U/238U and 236U/238U) were analyzed such that the 234U and 236U were monitored on SEM detectors and the 238U was monitored on a Faraday (1011 Ω) detector. Various integration times (5, 10, 25, and 50 ms) were investigated in all detector configurations to gain a better understanding of their impact on sensitivity, accuracy, and precision. For 235U/238U ratios of 1 µm U3O8 particles, a dual Faraday detector measurement with 1011 Ω was the optimal choice; measurement of 1021 particles yielded an average 235U/238U ratio of 0.00170 (14), a −1.8% relative difference (% RD) from the reference value. The minor isotopic compositions were determined to be 0.0000070 (14) and 0.0000758 (48) for the 234U/238U and 236U/238U, respectively. These measurements correspond to <8% and <1% RD from their reference value for the 234U/238U and 236U/238U, respectively. SP-MC-ICP-MS was also able to provide insight into measurement sensitivity. In these individual particles, merely 15 and 165 atto-grams (ag) of 234U and 236U were present (calculated). Initial limits of detection for SP-MC-ICP-MS were determined to be ∼1.0 ag (when measured via SEM detectors). This valuable approach is applicable to areas including nuclear forensics, nuclear safeguards, and geochemical analysis, which require high-precision measurements of uranium within micron-sized particles.

Manard, Benjamin [ORNL] (ORCID:0000000207400627)↗
DOE OSTI2025

Isotopic analysis of Nd nanoparticles using single particle MC-ICP-MS: A comparative study with single particle-ICP-TOF-MS

Single particle - inductively coupled plasma - mass spectrometry (SP-ICP-MS) is a powerful technique for characterization of the elemental and isotopic composition of individual particles. In this work, the capabilities of the newest generation of MC-ICP-MS with acquisition rates down to 50 ms were evaluated for single particle analysis, with a focus on isotopic precision achievable on a single-particle level. Nd (NdVO 4 ) nanoparticles (~120 nm in diameter) were used as case study and were first characterized in terms of mass (respective size) and particle number concentration by SP-ICP-TOF-MS and then by SP-MC-ICP-MS for isotopic precision. For the isotopic ratio measurements, the MC-ICP-MS performance was compared to the ICP-TOF-MS and it was found that the isotope ratio precision was increased (R 2 between 0.98 and 0.99) compared to ICP-TOF-MS (R 2 between 0.88 and 0.97). The accuracy attained on a single particle level, was compared to bulk digestion followed by MC-ICP-MS analysis, and the SP-MC-ICP-MS technique was able to determine the particle population average to be <4 %, percent relative differences for the 142 Nd/ 144 Nd, 143 Nd/ 144 Nd, 145 Nd/ 144 Nd, 146 Nd/ 144 Nd, and 148 Nd/ 144 Nd ratios The detection limit for the SP-MC-ICP-MS approach was also assessed. Here, when utilizing an all Faraday-cup based detection scheme the determined LOD for the measurements was 0.2fg for Nd, per particle. Based on these results, the newest generation of MC-ICP-MS has demonstrated its utility for performing SP measurement, particularly when high precision isotopic determination is warranted.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Towards an understanding of particle-scale flaws and microstructure evolution in cold spray via accumulation of single particle impacts

Cold spray coatings are the sum of countless individual bonding events between single particles impacting on top of one another at high velocities. Thus, the collective behavior of microparticles must be considered to elucidate the origins of coating flaws at the scale of the particles and larger, or the dynamic evolution of the overall coating microstructure. Laser-induced particle impact testing (LIPIT) has been extensively used to study single-particle impacts, and in this work is adapted to study the accumulation of numerous particles with knowledge of each individual particle's impact parameters (particle size, velocity). The method reproducibly deposits stacks of gold particles (>20 particles) with different characteristic spectra of impact velocity. The observation of impact-induced erosion lets us define a critical velocity for material-build-up that is higher than that for single-particle bonding. The quantitative single-particle data are analyzed in a correlative manner to the structure and flaws in the resulting stacks, providing some first statistical connections between, e.g., strain and recrystallization, or aberrant particle characteristics and defects. The results highlight opportunities for the study of many-particle phenomena in microparticle impact—from interaction of particles in cold spray to multi-step erosion processes—with a quantitative view of the behavior of single particles.

Erosion↗
DOE OSTI2024

Enhanced Detection of Primary Biological Aerosol Particles Using Machine Learning and Single-Particle Measurement

Accurately identifying primary biological aerosol particles (PBAPs) using analytical techniques poses inherent challenges due to their resemblance to other atmospheric carbonaceous particles. Here, we present a study of an enhanced method for detecting PBAPs by combining single-particle measurement with advanced supervised machine learning (SML) techniques. We analyzed ambient particles from a variety of environments and lab-generated standards, focusing on chemical composition for traditional rule-based and clustering approaches and incorporating morphological features into the SML approaches, neural networks and XGBoost, for improved accuracy. This study demonstrates that SML methods outperform traditional methods in quantifying PBAPs, achieving significant improvements in precision, recall, F1-score, and accuracy, leading to an increased number of detected PBAPs by at least 19%. The adaptability of the proposed XGBoost-based SML model is showcased in comparison to traditional methods in categorizing PBAPs for blind data sets from different geographical locations. Two field case studies were investigated, over agricultural land and Amazonia rain forest, representing relatively low and high concentrations of PBAPs, respectively, where XGBoost consistently detected up to 3.5 times more PBAPs than traditional methods. Precise detection of PBAPs in the atmosphere could significantly improve the prediction of climatic impacts by them.

42 ENGINEERING↗
DOE OSTI2025

Impact of gas background on XFEL single-particle imaging

Abstract Single-particle imaging (SPI) using X-ray free-electron Lasers (XFELs) offers the potential to determine protein structures at high spatial and temporal resolutions without the need for crystallization or vitrification. However, the technique faces challenges due to weak diffraction signals from single proteins and significant background scattering from gases used for sample delivery. A recent observation of a diffraction pattern from an isolated GroEL protein complex Ekeberg T et al. (Light Sci Appl 13:15, 2024.https://doi.org/10.1038/274s41377-023-01352-7) had similar numbers of signal and background photons. Ongoing efforts aim to reduce the background created by sample delivery, with one approach replacing most of the used gas with helium Yenupuri T et al. (Sci Rep 14:4401, 2024.https://doi.org/10.1038/s41598-024-54605-9). In this study, we investigate the effects of a reduced background on the resolution limits for SPI of isolated proteins under different experiment conditions. As a test case, we used GroEL, and we used experimentally derived parameters for our simulations. We observe that background significantly impacts the achievable resolution, particularly when the signal strength is comparable to the background. This is best exemplified at 6.0 keV, where a background reduction by a factor of 10 leads to a resolution improvement from 1.9 to 1.2 nm, for a dataset of$$10^4$$patterns.

Science & Technology - Other Topics↗
DOE OSTI2024

Quantifying the Diversity of an Atmospheric Aerosol Population in an Arctic Oil Field on a Single‐Particle Level

As the Arctic rapidly warms, sea ice extent is decreasing and oil and gas extraction activities are expanding. Local combustion emissions affect the Arctic atmospheric aerosol chemical mixing state (the distribution of chemical species across the aerosol population), which impacts climate-relevant properties. Bulk and single-particle measurements of submicron aerosols were conducted at Oliktok Point, Alaska within the North Slope of Alaska oil fields. In this work, we quantify aerosol diversity using online single-particle mass spectrometry data (32,880 individual particles), offline single-particle microscopy data (20,912 individual particles), and online bulk aerosol mass spectrometry and aethalometer data. This method was used to derive individual particle mass fractions for both refractory and non-refractory material within distinct particle types. Single-particle, average single-particle, and bulk population diversities (D i , D α , D γ , respectively) and mixing state indices (χ) were calculated for the data set. Calculated D i values were generally low (2.2 ± 0.6), as individual particle masses were dominated by a few chemical species of interest. Aged aerosol particles (those internally mixed with nitrate and/or sulfate) exhibited higher D i values (>3) compared to recently emitted (fresh) aerosol particles. During oil field plume periods, D α values approached three due to the abundance of diesel combustion particles, which were rich in sulfate, black carbon, and organic aerosol. Overall, the submicron aerosol population within the Arctic oil fields was found to be relatively externally mixed (χ < 50%), due to the constant local emissions within oil fields combining with background aerosol and locally emitted sea spray aerosol at the coastal site.

Wu, J.↗
DOE OSTI2025

Particle signal considerations for isotope ratio analysis with single particle multi-collector inductively coupled plasma mass spectrometry

Particle analysis has benefitted from the advent of single particle inductively coupled plasma-mass spectrometry (spICP-MS) due to its robustness, sensitivity, and high-throughput nature. Previous methods of spICP-MS have typically utilized quadrupole or time-of-flight mass analyzers and therefore employ electron multiplier-based detectors (such as secondary electron multipliers or microchannel plates). However, to obtain precise measurements on elemental or isotopic ratios within individual particles, multi-collector ICP-MS (MC-ICP-MS) can be used. Here, we investigate Ce isotope ratios, specifically 142 Ce/ 140 Ce, by spMC-ICP-MS using an all-Faraday cup collector array. Using 1 μm (diameter) cerium dioxide particles, integration times of the Faraday cup detectors were varied from 50–500 ms. The signal from the cerium isotopes in the particles was used to determine isotope ratios, which closely matched the expected natural isotopic abundances. Due to the signal decay response from the Faraday cups, the signal from particles lasts much longer than the expected 1–2 ms (up to 100 s of ms). To explore this effect on isotope ratio analysis, multiple ratio analysis methods were used to determine how to obtain optimal precision and accuracy. Relative differences were around 2% for methods that calculated isotope ratios from summing the total signal of an individual particle before calculating the ratio (rather than using every data point individually). It was found that summing all data points per particle, or integrating under the signal peak, yielded both accurate and precise isotope ratios within the particle population. Particles were also sampled off a solid substrate via microextraction, and isotope ratios were determined with relative differences of 0.13% to 9%. This demonstrates the ability to use spMC-ICP-MS to obtain isotope ratios on particles, with little to no relative difference in comparison to the expected ratio, even when operating Faraday detectors at fast 50 ms integration times.

Szakas, Sarah E. [Oak Ridge National Laboratory (O↗
DOE OSTI2024

Measurement report: The Fifth International Workshop on Ice Nucleation phase 1 (FIN-01): intercomparison of single-particle mass spectrometers

Knowledge of the chemical composition and mixing state of aerosols at a single-particle level is critical for gaining insights into atmospheric processes. One common tool to make these measurements is single-particle mass spectrometry. There remains a need to compare the performance of different single-particle mass spectrometers (SPMSs). An intercomparison of SPMSs was conducted at the Aerosol Interaction and Dynamics in the Atmosphere (AIDA) chamber at the Karlsruhe Institute of Technology (KIT) in November 2014, as part of the first phase of the Fifth International Workshop on Ice Nucleation (FIN-01). In this paper we compare size distributions and mass spectra of atmospherically relevant particle types measured by five SPMSs. These include different minerals, desert and soil dusts, soot, bioaerosol (Snomax; protein granule), secondary organic aerosol (SOA), and SOA-coated mineral particles. Most SPMSs reported similar vacuum aerodynamic diameter (d va ) within typical instrumental ranges from ~100–200 nm (lower limit) to ~2–3 µm (upper limit). In general, all SPMSs exhibited a wide dynamic range (up to ~10 3 ) and high signal-to-noise ratio (up to ~10 4 ) in mass spectra. Common spectral features with small diversities in mass spectra were found with high average Pearson's correlation coefficients, i.e., for average positive spectra r avg-pos =0.74 ± 0.12 and average negative spectra r avg-neg =0.67 ± 0.22. We found that instrument-specific detection efficiency (DE) was more dependent on particle size than particle type, and particle identification favored the use of bipolar, rather than monopolar, instruments. Particle classification from “blind experiments” showed that all instruments differentiated SOA, soot, and soil dust and detected subtle changes in the particle internal mixing but had difficulties differentiating among specific mineral types and dusts. This study helps to further understand the capabilities and limitations of the single-particle mass spectrometry technique in general and the specific performance of the instrument in characterizing atmospheric aerosol particles.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2024

Detecting Multipartite Entanglement Patterns Using Single-Particle Green’s Functions

Here, we present a protocol for detecting multipartite entanglement in itinerant many-body electronic systems using single-particle Green’s functions. To achieve this, we first establish a connection between the quantum Fisher information and single-particle Green’s functions by constructing a set of witness operators built out of single electron creation and destruction operators in a doubled system. This set of witness operators is indexed by a momentum k. We compute the quantum Fisher information for these witness operators and show that for thermal ensembles it can be expressed as an autoconvolution of the single-particle spectral function. We then apply our framework to a one-dimensional fermionic system to showcase its effectiveness in detecting entanglement in itinerant electron models. We observe that the detected entanglement level is sensitive to the wave vector associated with witness operator. Our protocol will permit detecting entanglement in many-body systems using scanning tunneling microscopy and angle-resolved photoemission spectroscopy, two spectroscopies that measure the single-particle Green’s function. It offers the prospect of the experimental detection of entanglement through spectroscopies beyond the established route of measuring the dynamical spin response.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Scalable 3D reconstruction for X-ray single particle imaging with online machine learning

X-ray free-electron lasers offer unique capabilities for measuring the structure and dynamics of biomolecules, helping us understand the basic building blocks of life. Notably, high-repetition-rate free-electron lasers enable single particle imaging, where individual, weakly scattering biomolecules are imaged under near-physiological conditions with the opportunity to access fleeting states that cannot be captured in cryogenic or crystallized conditions. Existing X-ray single particle reconstruction algorithms, which estimate the particle orientation for each image independently, are slow and memory-intensive when handling the massive datasets generated by emerging free-electron lasers. Here, we introduce X-RAI (X-Ray single particle imaging with Amortized Inference), an online reconstruction framework that estimates the structure of 3D macromolecules from large X-ray single particle datasets. X-RAI consists of a convolutional encoder, which amortizes pose estimation over large datasets, as well as a physics-based decoder, which employs an implicit neural representation to enable high-quality 3D reconstruction in an end-to-end, self-supervised manner. We demonstrate that X-RAI achieves state-of-the-art performance for small-scale datasets in simulation and challenging experimental settings and demonstrate its unprecedented ability to process large datasets containing millions of diffraction images in an online fashion. These abilities signify a paradigm shift in X-ray single particle imaging towards real-time reconstruction.

Computer science↗
DOE OSTI2026

Development of a Flow-through Cell for Ultrasonic Extraction (UE)─Single Particle (SP)─ICP-MS─an Approach for Nano/Microparticle Elemental and Isotopic Analysis

Nanotechnology is a salient part of the scientific landscape, and analytical approaches are rapidly evolving to enable small-scale characterization of nano- and microparticle compositions and impurities. Here, a flow-through sonicating cell was developed for direct particle extraction from a silicon wafer and integrated with an inductively coupled plasma–mass spectrometer (ICP-MS) for subsequent elemental and isotopic characterization of the released particles. Ultrasonic extraction (UE)─single particle (SP)─ICP-MS offers controlled particle mobilization from solid substrates and allows for increased sample throughput by eliminating the need for pre-extraction of particles and decreasing sample preparation steps. Coupling this device to an ICP-MS with a time-of-flight (TOF) mass analyzer, it is possible to distinguish unique isotopic compositions of the particles. Both tungsten and nickel isotopically tagged particles, which were deposited on Si wafers, are presented here with analysis via UE─SP─ICP-MS. This approach could support efforts in the fields of particle synthesis, nuclear safeguards and forensics, environmental monitoring, and semiconductor industries in which the detection of particles from substrates and wafers is critical.

Paul, Molly [ORNL] (ORCID:0009000009672055)↗
DOE OSTI2025

Chemical Interface Damping Revealed by Single-Particle Absorption Spectroscopy

Plasmon-induced interfacial charge separation is a promising way to efficiently extract energetic carriers through direct plasmon decay. This mechanism of charge transfer has been investigated by single-particle scattering spectroscopy, which measures the homogeneous plasmon line width. The line width is broadened by charge transfer, generally known as chemical interface damping. However, conflicting reports exist regarding the effect of chemical interface damping on the corresponding single-particle absorption spectrum, which is needed to accurately determine absolute light conversion efficiencies. This work aims to resolve this question by directly correlating absorption and scattering spectra of individual gold nanorods in the presence and absence of a charge-accepting interface. We find that for TiO 2 coated nanorods, the absorption line width is indeed broadened due to chemical interface damping but is overall narrower than the scattering line width. Here, chemical interface damping is furthermore found to increase with larger resonance energies. The observed differences in line widths between absorption and scattering are elucidated within the context of an analytically tractable model describing the lowest energy optically bright and higher-order optically dark plasmon modes of the nanorod, including bulk, radiative, and chemical interface damping effects. Taken together, these results establish that single-particle absorption spectroscopy is capable of revealing interfacial charge injection by direct plasmon decay.

absorption↗
DOE OSTI2026

Integrating Flow Imaging Analysis and Single-Particle ICP-TOFMS for Comprehensive Micro- and Nanoplastic Characterization

Flow imaging analysis (FIA), provides composition-agnostic morphological characterization. These measurements of particle size and shape are valuable to mass-based analysis, such as single particle inductively coupled plasma time-of-flight mass spectrometry (sp-ICP-TOFMS), which provides quantitative data on elements within particles. Using these two methods together enables informed use of geometric assumptions required by sp-ICP-TOFMS, as particle mass is typically converted to a particle diameter using assumed-spherical geometry. To validate this concept, parallel measurements to determine particle diameters were performed by FIA and sp-ICP-TOFMS on four particle suspensions: 300 nm polystyrene Eu-doped nanoparticles, 1 μm Fe-rich beads, 3 μm four element calibration polystyrene beads and 5 μm polystyrene beads. The Fe-particles obtained the highest percent difference from the manufacturer’s nominal diameter, as the mean diameter obtained by FIA was overestimated by 21% and sp-ICP-TOFMS underestimated the mean diameter by 20.7%. Two types of particles were selected to test the effect of varying the particle number concentrations (PNC) on sizing accuracy, and both methods accurately sized each particle population at the PNC expected. Single particle analysis of carbon has continued to be a popular research topic, with direct applications to environmental pollutants in terms of nano- and micro- plastics. Real-world plastic particles were studied, and FIA’s measured circularity values demonstrated that the particles deviated from spherical geometries, therefore sp-ICP-TOFMS data should be interpreted as mass-based rather than size-based. Combining these techniques enables improved interpretation of particle populations and evaluation of particle sizes.

Szakas, Sarah [ORNL] (ORCID:0000000241332197)↗
DOE OSTI2026

Single-Particle Insights Into the Electronic Structure and Enhanced Stability of CsPbBr 3 /FAPbBr 3 Core/Crown Nanoplatelets at the Nanometer Scale

Colloidal perovskite nanoplatelets (NPLs), despite their exceptional optoelectronic properties, face significant challenges due to their intrinsic instability and trap-assisted non-radiative recombination. Although many studies employing surface engineering, such as selecting ligands or coating to passivate defects, have demonstrated improved optoelectronic properties, these enhancements are typically inferred from bulk-ensemble measurements; the effects at the single-particle level remain elusive. Here, we conduct single-particle-level studies using scanning tunneling spectroscopy (STS) on a unique core–crown system, CsPbBr 3 @FAPbBr 3 NPLs, where the lateral surfaces of the CsPbBr 3 core are coated with an FAPbBr 3 crown. Experimental density-of-states (DOS) analysis reveals a 47% reduction in deep-trap states in core-crown NPLs compared to core-only NPLs, consistent with nearly two-fold enhancements in photoluminescence quantum yields. Progressive I–V sweep measurements demonstrate superior electrical stability in core-crown NPLs, preserving band structure with minimal degradation, while core-only NPLs exhibit rapid bandgap shrinkage and trap formation. Density functional theory (DFT) calculations indicate that FA incorporation distorts Pb octahedral lattice, widening the bandgap. This study elucidates how surface engineering modulates charge localization, passivates defects, and enhances stability at the single-particle level. Moreover, by uncovering bias-induced trap states in single unpassivated NPLs, this study establishes a precise, robust approach for characterizing emerging perovskite nanocrystals.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2025

Quantifying Impacts of Biomass Pelletization on Fast Pyrolysis Using a Single-Particle Reactor, X-ray Computed Tomography, and Computational Modeling

The pore structure and density of lignocellulosic feedstocks dictate intraparticle transport phenomena and thereby play an important role in thermochemical conversion processes such as fast pyrolysis for biofuel and biochemical production. Variations in microstructure are inherent from different biomass species and can be introduced by preprocessing techniques such as cutting and pelletization. Morphological changes also occur during conversion and lead to vastly different pore structures and behavior during pyrolysis, which impact required conversion times and product distributions. The current work presents a comprehensive comparison of fast pyrolysis of neat and pelletized pine feedstocks, which includes single-particle experiments, modeling, and 3D imaging by X-ray computed tomography (XCT). The particle-scale model included anisotropic heat and mass transport in a shrinking particle with pyrolysis reactions based on the CRECK mechanism with boundary conditions informed by reactor-scale simulations of the single-particle reactor. The models were validated by measurements of the temperature and mass loss from single-particle pyrolysis experiments of neat and pelletized pine. Quantitative analysis of XCT geometries revealed that pyrolytic conversion yielded chars with increased porosity and permeability compared to the unpyrolyzed materials, along with decreased tortuosity and anisotropy. Pelletization of the pine feedstock resulted in a much denser, less permeable material, which converted slower and produced more residual char after pyrolysis compared to neat pine. The results from particle modeling revealed that accounting for the dynamic and anisotropic heat and mass transport caused by differences in pore structure is critical to achieving agreement with experimental results. Overall, this study highlights the dramatic differences in conversion behavior imparted by pelletization and the importance of capturing microstructural attributes in computational models to guide the design and optimization of pyrolysis processes for specific biomass feedstocks.

09 BIOMASS FUELS↗