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DOE OSTI2026

Coupling of high-resolution mass spectrometer and photosynthesis system for comprehensive leaf volatile metabolite profiling

Background Leaf-level biogenic volatile organic compounds (BVOCs) emissions represent a major source of organic gases in the atmosphere, influencing both climate and air quality. These emissions are strongly driven by environmental perturbations, which affect individual plant- to ecosystem-level processes. Uncovering all the BVOCs and understanding how their emissions respond to altered environmental conditions provide critical insights into vegetation-driven changes in atmospheric chemistry. We developed a tandem instrumentation setup that integrates a proton transfer reaction time-of-flight mass spectrometer (PTR-ToF-MS) with parts-per-trillion detection limits and a photosynthetic infrared gas exchange system for the untargeted survey of all the BVOCs. This novel system enables simultaneous, real-time monitoring of BVOC emissions and photosynthetic parameters at the leaf level, offering new opportunities to disentangle the physiological and environmental drivers of VOC release. Furthermore, we established the VOC Analysis and Processing Optimization Resource (VAPOR), an open-access software tool designed for rapid data post-processing and the analysis of the variability of hundreds of BVOCs. We assessed the performance of the tandem system under varying background conditions, using standard gas mixtures and a range of environmental factors. Results Blank emissions were substantially lower for major BVOCs (e.g., isoprene) compared to those observed in plant emissions. Despite this, the observation of background-level VOCs highlights the importance of routinely acquiring and accounting for blank measurements in analyses using the coupled instrumentation. Introduction of known VOC concentrations to the system demonstrated a linear response across different compounds with varying molecular compositions, indicating minimal gas loss regardless of chemical moieties within the coupled instrumentation. We applied the optimized system to investigate the physiological mechanisms driving BVOC emissions across different genotypes of poplar and pennycress. The high mass resolution capabilities of the PTR-ToF-MS, coupled with comprehensive VAPOR-driven data analysis, enabled the identification of several important BVOCs, including methanol and methanethiol; these BVOCs displayed substantial variation across pennycress genotypes and showed concentrations ~ 100–350% higher than the blank. Moreover, isoprene emissions varied significantly among poplar genotypes grown in different potting media. Conclusions Tandem instrumentation offers a powerful tool for profiling volatile molecular markers and elucidating their genetic and environmental underpinnings. This approach enhances our ability to predict BVOC emissions in response to genotype by environmental interactions and contributes to a deeper understanding of vegetation responses to environmental changes.

Biogenic volatile organic compounds↗

DOE OSTI2026

Polar primary aerosols across the ocean-sea ice-snow-atmosphere interface: From sources to impacts

Primary aerosols play a critical role in polar climate systems, influencing cloud formation, precipitation, radiative balance, and surface energy budgets. This paper provides a comprehensive synthesis of primary aerosol sources, transformation and removal processes, and broader atmospheric impacts in polar regions, emphasizing their links to ocean and sea ice biogeochemistry. These aerosols (including sea salt, primary organic aerosol, and primary biological aerosol particles) originate from marine and cryospheric environments and are emitted through physical processes, such as wave breaking, bubble bursting, and blowing snow. Emission sources include seawater, sea ice, snow, and freshwater from river discharge and glacial runoff. Once airborne, these particles can serve as a chemical reservoir, influencing atmospheric composition and reactivity, and as seeds for cloud droplet and ice crystal formation, influencing cloud microphysics and polar climate. Despite their importance, many of the processes governing primary aerosol emissions and transformations remain poorly constrained. The most pressing knowledge gaps pertain to emission processes, limited spatiotemporal observational coverage, instrumentation constraints, parameterization development, and the integration of interdisciplinary expertise. To improve our understanding of primary aerosol drivers and their response to climate, future research efforts should prioritize strategically coordinated and cross-disciplinary process studies, advancements in measurement technologies and coverage, and close collaboration between modelers and observational scientists to inform and refine model parameterizations. As polar regions continue to undergo profound changes marked by increased precipitation, reduced sea and land ice, freshening oceans, and shifting ecosystem dynamics, characterizing present-day primary aerosol populations is vital. Improved understanding will be essential for anticipating future changes in aerosol-radiation and aerosol-cloud interactions and their implications for polar and global climate systems.

Aerosol-cloud↗

DOE OSTI2022

Materials properties characterization in the most extreme environments

Abstract There is an ever-increasing need for material systems to operate in the most extreme environments encountered in space exploration, energy production, and propulsion systems. To effectively design materials to reliably operate in extreme environments, we need an array of tools to both sustain lab-scale extreme conditions and then probe the materials properties across a variety of length and time scales. Within this article, we examine the state-of-the-art experimental systems for testing materials under extreme environments and highlight the limitations of these approaches. We focus on three areas: (1) extreme temperatures, (2) extreme mechanical testing, and (3) chemically hostile environments. Within these areas, we identify six opportunities for instrument and technique development that are poised to dramatically impact the further understanding and development of next-generation materials for extreme environments. Graphical abstract

Schreiber, Daniel K.↗

DOE OSTI2021

Supervisory control and health monitoring framework for large-scale additive manufacturing systems. Final CRADA report

ORNL worked with National Instruments (NI) to develop a large-scale, complex additive manufacturing (AM) systems framework for remote health monitoring and supervisory control. We found the framework, based on the Lincoln Electric Metal AM system located at ORNL’s MDF, capable of controlling the process, leading to improved part quality and digital twin creation.

42 ENGINEERING↗

DOE OSTI2021

Algorithms and file structures to enhance software workflows for ion mobility mass spectrometry (IM-MS): CRADA 410 (Final Report)

This document is the final report for CRADA 410 (Project No. 72496). The purpose of this project was supporting customizations of algorithms and raw data file structures to enhance software workflows for liquid chromatography (LC), mass spectrometry (MS) and ion mobility mass spectrometry (IM-MS)-based metabolite characterization. PNNL worked with Agilent to evaluate and improve the integration of ion mobility into existing MS data analysis methods of Agilent software tools. The project augmented PNNL’s capabilities to analyze complex omics samples. These capabilities are directly beneficial to DOE and PNNL efforts to characterize and analyze compounds in microbial and plant communities. The project assisted Agilent in further developing improved instrument-software solutions combining ion mobility with mass spectrometry for widespread applications in life sciences and other fields.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2023

Applications of Alternate Actinide Calibration on Inductively Coupled Plasma Mass Spectrometry (ICPMS) Analysis of H-Canyon Highly Enriched Uranium Legacy Material at the Savannah River Site (SRS)

The Savannah River National Laboratory (SRNL) uses Inductively Coupled Plasma Mass Spectrometry (ICPMS) to support numerous programs at the Savannah River Site (SRS). As part of an objective to prepare high assay low enriched uranium (HALEU), the SRS H-Canyon needed analysis of legacy uranyl nitrate that is stored at its Outside Facilities (HOF). With the application of a standard practice for alternate actinide calibration on ICP-MS, SRNL has successfully demonstrated its capability to characterize the uranium/actinide composition of the HOF tanks that are intended for consolidation prior to preparation of the HALEU. A comparison of the uranium analytical results between recently upgraded SRNL ICP-MS and Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) instrumentation shows the alternate actinide calibration is a valid complementary method when used in conjunction with other analytical techniques (Davies-Gray Potentiometric Titration). The methods, instrumentation, and ongoing developments on ICP-MS at SRNL will be discussed.

Jones, Mark A.↗

DOE OSTI2024

Lead tungstate calorimeters at Jefferson Lab and perspectives for the Electron–Ion Collider

Electromagnetic calorimeters based on PbWO4 scintillating crystals have a widespread applica- tion in experiments at different accelerator facilities such as CERN, FNAL, GSI, and Jefferson Lab. The unique properties of PbWO4 crystals, including a small radiation length and Molire radius, make them ideal for building high-granularity, radiation-hard detectors. This enables excellent spa- tial separation and energy resolution of reconstructed electromagnetic showers, making PbWO4 crystals the material of choice for numerous experiments. Lead tungstate calorimeters have been successfully used in several experiments at Jefferson Lab. Two large-scale detectors have been re- cently fabricated for future experiments : the Neutral Particle Spectrometer and the lead tungstate calorimeter of the GlueX detector. The future application of PbWO4 crystals in the ElectronIon Collider further highlights their ongoing importance in advancing experimental capabilities. In planning new experiments, the development of calorimeter instrumentation technologies becomes paramount. The integration of modern photodetectors, such as Silicon photomultipliers that are capable of operating in strong magnetic fields, and the implementation of streaming readout data acquisition systems, sophisticated shower reconstruction algorithms, and real-time data analysis are some examples of the continuously growing requirements of experimental setups. I will give an overview of the lead tungstate scintillating calorimeters and discuss some recent advancement in the calorimeter instrumentation.

Somov, Alexander↗

DOE OSTI2025

Algorithms and file structures to extend and enhance liquid chromatography and ion mobility mass spectrometry workflows (CRADA Final Report)

The purpose of this project was to continue supporting customizations of algorithms and raw data file structures to enhance software workflows for liquid chromatography (LC), mass spectrometry (MS) and ion mobility mass spectrometry (IM-MS)-based protein and metabolite characterization. PNNL worked with Agilent to design, implement, evaluate, and demonstrate new algorithms and integrated them as functionalities into the PNNL-PreProcessor software. The project augmented PNNL’s capabilities to analyze complex proteomics and metabolomics samples. These capabilities are directly beneficial to DOE and PNNL efforts to characterize and analyze these compounds in microbial and plant communities. The project assisted Agilent in further developing improved instrument-software solutions combining liquid chromatography and ion mobility with mass spectrometry for widespread applications in life sciences and other fields.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Postirradiation Examination of WIRE-21 Experiment Irradiated in the High Flux Isotope Reactor

Westinghouse Electric Company is developing wireless sensors to monitor the centerline temperature and internal pressure of commercial light-water reactor fuel rods during irradiation. Oak Ridge National Laboratory and Westinghouse Electric Company developed the Wireless Instrumented RB Experiment 2021 (WIRE-21) to test wireless temperature and pressure sensor technologies in a removable beryllium position in the High Flux Isotope Reactor. The experiment was irradiated for a total of 75 days, at temperatures ranging from approximately 150°C to 400°C, resulting in a peak fast (energy > 0.1 MeV) neutron fluence of about 3 × 10 21 n/cm 2 . The temperature was intentionally cycled multiple times to compare the response of the wireless temperature sensor to collocated thermocouples. Similarly, the pressure sensor was actuated in multiple steps to compare the response of the wireless measurement to excore pressure transducers (Petrie et al., 2023). After irradiation, the experiment was disassembled in the Irradiated Fuels Examination Laboratory (IFEL) hot cell at Oak Ridge National Laboratory with the intent to recover sensor and dosimetry components, document the as-irradiated condition of the hardware, and investigate possible causes of the sensor behavior observed during irradiation. The postirradiation examination successfully recovered and preserved key WIRE-21 components. After the housing was removed using a milling machine, the internal experiment sections were examined. All eight fiber-optic sensors were recovered, cut, and stored. The silicon carbide thermometry, temperature sensor, pressure sensor, lower spacer, and selected pressure and temperature cable sections were also removed and stored. The metal bellows of the pressure sensor was found to be plastically deformed, indicating that it had been properly pressurized during irradiation and generally behaved as expected. X-ray diffraction analysis of a section of one of the irradiated inductor cores within the pressure sensor was performed and confirmed the presence of phase-pure alpha ferrite (i.e., no unexpected phase transformations). Inductance testing was performed on the irradiated pressure sensor cores using an unirradiated test coil, and DC resistance measurements of the transceiver coils were also performed. The measurements with irradiated inductor cores assembled inside unirradiated coils showed slightly reduced inductance compared to measurements made with unirradiated cores, but the difference was not sufficient to explain the more significant reductions in inductance that were observed in-pile. Therefore, it is suspected that degradation of the inductor coils (specifically the wire wrapping) is responsible for the reduced inductance observed in-pile.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2023

Fiber Optic Temperature Sensor System Using Air-Filled Fabry–Pérot Cavity with Variable Pressure

We report a high-resolution fiber optic temperature sensor system based on an air-filled Fabry–Pérot (FP) cavity, whose spectral fringes shift due to a precise pressure variation in the cavity. The absolute temperature can be deduced from the spectral shift and the pressure variation. For fabrication, a fused-silica tube is spliced with a single-mode fiber at one end and a side-hole fiber at the other to form the FP cavity. The pressure in the cavity can be changed by passing air through the side-hole fiber, causing the spectral shift. We analyzed the effect of sensor wavelength resolution and pressure fluctuation on the temperature measurement resolution. A computer-controlled pressure system and sensor interrogation system were developed with miniaturized instruments for the system operation. Experimental results show that the sensor had a high wavelength resolution (<0.2 pm) with minimal pressure fluctuation (~0.015 kPa), resulting in high-resolution (±0.32 ℃) temperature measurement. It shows good stability from the thermal cycle testing with the maximum testing temperature reaching 800 ℃.

47 OTHER INSTRUMENTATION↗

DOE OSTI2020

Helium Ion Microscopy

Nanotechnology research led to the development of various instruments to be used for imaging or fabrication. The helium ion microscope (HIM) became available in 2006 but quickly gained popularity. Its unique gas field ion source enables high-resolution imaging, nanofabrication, direct write, and the recent combination with a secondary ion mass spectrometer offers chemical imaging with ~15 nm resolution. Particularly attractive are the small interaction volume of He and Ne (the two gases offered), small beam spot size, and a moderate sputtering rate. Additionally, the HIM is an excellent imaging tool for insulating samples in soft, polymeric, and biological materials. It can be expected that helium ion microscopy will continue to have a strong influence on broad range of scientific disciplines, including chemistry, materials science, and biology.This chapter aims at providing an overview of the current status of HIM for imaging, analysis, and nanofabrication. It introduces the reader to key components of the instrument, theoretical background, and latest results in the areas of imaging, material fabrication, and chemical analysis capabilities of helium ion microscopy.

Belianinov, Alex↗

DOE OSTI2023

Book Chapter: Small Modular Reactors

Small Modular Reactors (SMRs) have been a very promising development in nuclear power over the last two decades. SMRs are defined as nuclear reactors with a power output of less than 300 MWe. This is in comparison to gigawatt-size reactors, which can have electrical output of 1000–1500 MWe or more. This chapter will consist of two major sections. The first will be a detailed summary of the small modular reactor designs being proposed around the world. This section will focus on those that are the furthest along in their development, but will also include some information about the wide variety of proposed designs that require significant research and development. The second part will be a discussion of the remaining challenges to the adoption of SMRs as a major energy source. SMRs are not a new concept, but they do represent a new vision for an older concept. These reactors have the potential to become a major source of energy in the near future. The development of small, modular designs can help promote the adoption of nuclear energy by reducing upfront costs, reducing the financial risk associated with nuclear power, and the barriers to entry. However, the adoption of SMRs is not without challenges. Regulatory and licensing changes to address the unique benefits and concerns associated with SMRs will continue to be a challenge as regulators adapt to the unique features emerging from the design process. The development of new instrumentation and control systems is an ongoing issue. And economics is possibly the most significant challenge, with high construction costs, cheap natural gas, and government subsidies, combining to result in significant financial risk associated with adopting nuclear generation.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2023

Study of Different Piezoelectric Material Stroke Displacement at Different Temperatures Using an SRF Cavity

Piezoelectric actuators are used for resonance control in superconducting linacs. The level of frequency compensation depends on the piezoelectric stroke displacement. In this study, the stroke displacement will be measured with a 1.3 GHz SRF cavity by measuring the frequency shift with respect to the voltage applied. The entire system was submerged in liquid helium. This study characterizes the PZT piezoelectric actuator (P-844K093) and a lithium niobate (P-844B0005) piezoelectric actuator. All these actuators were developed at Physik Instrumente (PI). The piezoelectric displacement was measured at different temperatures.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2020

Current Status of the Synroc Waste Treatment Facility - 20263

Construction of the Synroc Waste Treatment Facility is well underway at ANSTO. This plant has been designed to treat intermediate level liquid waste arising from the production of Mo-99 within the newly constructed ANSTO Nuclear Medicine (ANM) precinct [1]. The facility utilises ANSTO Synroc technology that has been tailored to the chemical, physical, and radiological properties of the waste. The result is a highly durable wasteform with a significant reduction in the final volume of the treated waste. This paper presents the construction status of the Synroc Waste Treatment Facility and the status of the associated technology maturation plan. Construction of the building is scheduled for completion in late 2020 followed by process installation and commissioning. A key component of the technology maturation plan has been the construction of an Inactive Engineering Demonstrator [2]. This has aided in the mitigation of risks with respect to technology selection, process integration, and process nuclearisation. Furthermore, the demonstration facility has provided an environment for the design and development of the instrumentation and control philosophy resulting in a seamlessly integrated plant control system. Successful demonstration of the technology by the inactive engineering demonstrator has significantly reduced the associated risks. Details of the Synroc Waste Treatment Facility project progress will also be presented. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

DICER: A new instrument at LANSCE to constrain neutron capture rates on radionuclides

. With very few exceptions, direct measurements of neutron capture rates on radionuclides have not been possible. A number of indirect methods have been pursued such as the surrogate method, the γ-ray strength function method, the Oslo method and the β-Oslo method. Substantial effort has been devoted to quantify the usually large systematic errors that accompany the results from these techniques. A new instrument has been developed at the Los Alamos Neutron Science Center (LANSCE) to provide more accu rate data on several radionuclides relevant to nuclear criticality safety, radiochemical diagnostics, astrophysics, nuclear forensics and nuclear security, by measuring the transmission of neutrons through radioactive samples and studying resonance properties. The Device for Indirect Capture on Radionuclides (DICER) and as sociated radionuclide production at the Isotope Production Facility (IPF), both at LANSCE, as well radioactive sample fabrication, have been under development the last few years. A description of the new apparatus, data on a few mid-weight stable isotopes and efforts on radionuclide measurements will be presented.

Nuclear Criticality Safety Program (NCSP)↗

DOE OSTI2024

GAMPix: a novel fine-grained, low-noise and ultra-low power pixelated charge readout for TPCs

Here, we report on the development of a novel pixel charge readout system, Grid Activated Multi-scale pixel readout (GAMPix), which is under development for use in the GammaTPC gamma ray instrument concept. GammaTPC is being developed to optimize the use of liquid argon time projection chamber technology for gamma ray astrophysics, for which a fine grained low power charge readout is essential. GAMPix uses a new architecture with coarse and fine scale instrumented electrodes to solve the twin problems of loss of measured charge after diffusion, and high readout power. Fundamentally, it enables low noise and ultra low power charge readout at the spatial scale limited by diffusion in a time projection chamber, and has other possibly applications, including future DUNE modules.

Shutt, Tom↗

DOE OSTI2023

Cyber Framework for Steering and Measurements Collection Over Instrument-Computing Ecosystems

We propose a framework to develop cyber solutions to support the remote steering of science instruments and measurements collection over instrument-computing ecosystems. It is based on provisioning separate data and control connections at the network level, and developing software modules consisting of Python wrappers for instrument commands and Pyro server-client codes that make them available across the ecosystem network. We demonstrate automated measurement transfers and remote steering operations in a microscopy use case for materials research over an ecosystem of Nion microscopes and computing platforms connected over site networks. The proposed framework is currently under further refinement and being adopted to science workflows with automated remote experiments steering for autonomous chemistry laboratories and smart energy grid simulations.

Al Najjar, Anees↗

DOE OSTI2026

INL CRMO XRF Special Report No. 3: INL CRMO XRF Calibration Methods for the Analysis of Ceramics and Brick

This report details the analytical methods used by the Idaho National Laboratory Cultural Resource Management Office to characterize ceramic and brick artifacts using X-ray fluorescence spectrometry. More specifically, this report provides details on instrumentation, analysis times, and matrix-specific calibration protocols for ceramic materials. Calibration curves were developed to adjust raw instrumental output for 13 elements using a suite of reference standards made from historic brick borrowed from the Yale Peabody Museum. Calibration curves were validated by plotting predicted values against published reference values for the calibration set as well as a certified soil reference standard (SRM 2711a).

36 MATERIALS SCIENCE↗