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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 OSTI2020

Universal liquid sample device and process for high resolution transmission electron microscope imaging and multimodal analyses of liquid sample materials

Liquid sample imaging devices and processes are disclosed for high resolution TEM imaging and multimodal analyses of liquid sample materials in situ under high vacuum that are compatible with standard type TEM chip membranes and TEM sample holders allowing TEM liquid sample imaging to be performed wherever a TEM instrument is accessible and at a substantially reduced cost compared to prior art systems and approaches.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Preliminary EDS Liquid Sample Adapter Design Assurance Testing

A new liquid sample adapter design for the Explosive Destruction Systems has been developed. The design features a semi-transparent fluoropolymer tube coupled to the vessel high pressure sample valve with a closing quick connect fitting. The sample tubes are the pressure-limiting component. The tubes were hydrostatically tested to establish failure characteristics and pressure limits at ambient and operational temperatures. A group of tubes from two manufacturing lots were tested to determine the consistency of the commercial part. An upper pressure limit was determined for typical operations.

42 ENGINEERING↗
DOE OSTI2023

3D-printed sheet jet for stable megahertz liquid sample delivery at X-ray free-electron lasers

X-ray free-electron lasers (XFELs) can probe chemical and biological reactions as they unfold with unprecedented spatial and temporal resolution. A principal challenge in this pursuit involves the delivery of samples to the X-ray interaction point in such a way that produces data of the highest possible quality and with maximal efficiency. This is hampered by intrinsic constraints posed by the light source and operation within a beamline environment. For liquid samples, the solution typically involves some form of high-speed liquid jet, capable of keeping up with the rate of X-ray pulses. However, conventional jets are not ideal because of radiation-induced explosions of the jet, as well as their cylindrical geometry combined with the X-ray pointing instability of many beamlines which causes the interaction volume to differ for every pulse. This complicates data analysis and contributes to measurement errors. An alternative geometry is a liquid sheet jet which, with its constant thickness over large areas, eliminates the problems related to X-ray pointing. Since liquid sheets can be made very thin, the radiation-induced explosion is reduced, boosting their stability. These are especially attractive for experiments which benefit from small interaction volumes such as fluctuation X-ray scattering and several types of spectroscopy. Although their use has increased for soft X-ray applications in recent years, there has not yet been wide-scale adoption at XFELs. Here, gas-accelerated liquid sheet jet sample injection is demonstrated at the European XFEL SPB/SFX nano focus beamline. Its performance relative to a conventional liquid jet is evaluated and superior performance across several key factors has been found. This includes a thickness profile ranging from hundreds of nanometres to 60 nm, a fourfold increase in background stability and favorable radiation-induced explosion dynamics at high repetition rates up to 1.13 MHz. Its minute thickness also suggests that ultrafast single-particle solution scattering is a possibility.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Advanced Test Reactor Loop Activity Report: Gamma-Ray Emitting Radionuclides Concentrations and Decontamination Factors of ATR Loop Liquid Samples Cycle 173C-1

The gamma-ray emitting radionuclide concentration and decontamination factor results from gamma-ray spectrometry measurements of ATR loop liquid samples by the Radiation Measurements Laboratory (RML) are contained in this report for ATR Cycle 173C-1 from November 22, 2024, to January 21, 2025.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Gamma-Ray Emitting Radionuclides Concentrations and Decontamination Factors of ATR Loop Liquid Samples Cycle 171B

This report contains the gamma-ray emitting radionuclides concentration and decontamination factor results from gamma-ray spectrometry measurements of ATR loop liquid samples by the Radiation Measurements Laboratory (RML) for ATR Cycle 171B Jun. 20, 2023, to Sep. 27, 2023. This report consists of five subsections, one for each loop. Each subsection contains the results for each sampling of the loop along with the date and time of sampling, spectral data identifications, sample type, and reactor power (MW). The results are reported in units of disintegrations per minute per milliliter of sample. The results are obtained with the gamma-ray spectral data analysis routines of the RML computer. Some of this report is also generated by RML data storage and handling routines.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Gamma-Ray Emitting Radionuclides Concentrations and Decontamination Factors of ATR Loop Liquid Samples: Cycle 172A

This report contains the gamma-ray emitting radionuclides concentration and decontamination factor results from gamma-ray spectrometry measurements of ATR loop liquid samples by the Radiation Measurements Laboratory (RML) for ATR Cycle 172A running March 2, 2024, to March 16, 2024. This report consists of five subsections, one for each loop. Each subsection contains the results for each sampling of the loop along with the date and time of sampling, spectral data identifications, sample type, and reactor power (MW). The results are reported in units of disintegrations per minute per milliliter of sample. The results are obtained with the gamma-ray spectral data analysis routines of the RML computer. Some of this report is also generated by RML data storage and handling routines.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

Advanced Test Reactor Loop Activity Report: Gamma-Ray Emitting Radionuclides Concentrations and Decontamination Factors of ATR Loop Liquid Samples for ATR Cycle 175B-1

The gamma-ray emitting radionuclide concentration and decontamination factor results from gamma-ray spectrometry measurements of ATR loop liquid samples by the Radiation Measurements Laboratory (RML) are contained in this report for ATR Cycle 175B-1 from August 4, 2025 to October 6, 2025.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Gamma-Ray Emitting Radionuclides Concentrations and Decontamination Factors of ATR Loop Liquid Samples Cycle 173A Revision 0

This report contains the gamma-ray emitting radionuclides concentration and decontamination factor results from gamma-ray spectrometry measurements of ATR loop liquid samples by the Radiation Measurements Laboratory (RML) for ATR Cycle 173A running May 3, 2024, to July 6, 2024. This report consists of five subsections, one for each loop. Each subsection contains the results for each sampling of the loop along with the date and time of sampling, spectral data identifications, sample type, and reactor power (MW). The results are reported in units of disintegrations per minute per milliliter of sample. The results are obtained with the gamma-ray spectral data analysis routines of the RML computer. Some of this report is also generated by RML data storage and handling routines.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Complete resolution across the neodymium/samarium isotopic envelope with a liquid sampling‐atmospheric pressure glow discharge — Orbitrap mass spectrometer

Rationale Nd and Sm isotope ratios play an important role in geological dating and as nuclear forensic signatures; however, the overlap of the respective 144, 148, 150 Nd/Sm isobars requires prior separations to be performed before analysis on typical MS platforms. The work presented here overcomes these isobaric interferences using ultrahigh‐mass resolution to alleviate interference without prior chemical separations. Methods A liquid sampling‐atmospheric pressure glow discharge ion source was coupled to a standard, QExactive Focus Orbitrap mass spectrometer, providing a mass resolution of ~80 k. A Spectroswiss FTMS booster X2 data acquisition package was used to collect extended transients, providing much higher mass resolution; ~230 k and ~600 k are employed here for Nd and Sm isotopes. Results While the standard Orbitrap resolution is far greater than typical “atomic” MS platforms, it was insufficient to alleviate all isobars. The use of a resolution of ~230 k resulted in baseline separation across the entire isotopic envelope for both Nd and Sm. Isotope ratios obtained from Nd:Sm mixtures using high‐resolution were equivalent to those found for individual‐element solutions, while isotope ratios obtained at a resolution of ~80 k (standard for the OEM data system) showed large deviations. Conclusions Use of ultrahigh‐resolution is an attractive alternative to extensive chemical separations to alleviate severe isobaric interferences. Sufficient mass resolution greatly reduces/eliminates the need for sample manipulations (separations) before analysis while reducing costs and total analysis times.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Preliminary investigation of an uncertainty budget for uranium isotope ratio analysis using a liquid sampling—atmospheric pressure glow discharge—orbitrap mass spectrometer system

The liquid sampling-atmospheric pressure glow discharge (LS-APGD) ionization source has proven to be an effective analysis tool for making uranium isotope ratio measurements when coupled to high-resolution mass spectrometers, such as the Orbitrap. While previous studies have shown the capabilities of the LS-APGD for isotope ratio determination, a systematic evaluation of the measurement uncertainty of the technique has not been conducted. To this end, the International Standards Organizations (ISO) guidelines to the expression of uncertainty in measurement (GUM analysis) have been applied to generate an uncertainty budget. For this work, a preliminary assessment derived from the GUM analysis was performed. The uncertainty in the instrument blank determination has been identified as a primary factor contributing to measurement uncertainty for the LS-APGD-Orbitrap method. These findings for the specific test case of uranium isotopic analysis will be invaluable in applications across the breadth of isotope ratio mass spectrometry performed on this unique instrumental platform.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2023

Coupling of the Liquid Sampling–Atmospheric Pressure Glow Discharge to Orbitrap Mass Analyzers for Uranium Isotope Ratio Analysis: Evolution of the Methodology and Implications to the Field

Just over a decade ago, a truly outside-of-the-box approach to isotope ratio mass spectrometry (IRMS) was undertaken between research groups at Clemson University and the Pacific Northwest National Laboratory. The original motivation dealt with projections as to whether or not microplasmas could be developed into practical elemental ionization sources, perhaps for transportable analysis applications. In particular, the use of the liquid sampling–atmospheric pressure glow discharge (LS-APGD) was pursued. Its interfacing to an ultra-high resolution Orbitrap platform, proved not only facile, but opened up a wealth of potential applications. Here, we lay out a historical, tutorial description of the interfacing and the evolution of the methodology regarding IRMS of uranium. Practical challenges and opportunities are described, which hopefully provide guidance to further applications in high resolution IRMS. It is hoped that, while detailed and lengthy, the didactic nature of the presentation provides experimental insights and tips, and also serves as an homage to our very good friend, Professor Gary M. Hieftje, whose scientific inspiration and comradery have been immeasurably important in our own careers.

Koppenaal, David W.↗
DOE OSTI2025

Detection of Br and I as atomic anions using liquid sampling – atmospheric pressure glow discharge/Orbitrap mass spectrometry

The quantification and determination of halogen isotope composition is essential in many fields including geochemistry and nuclear forensics. Detection of the halogen elements is commonly attempted with inductively coupled plasma mass spectrometry (ICP-MS) however, there are multiple challenges faced. Most significantly this includes very poor ionization efficiency and the potential for isobaric interferences from either matrix or plasma species. Thus, sensitivity and accuracy are often limiting issues. Here a liquid sampling-atmospheric pressure glow discharge (LS-APGD) ionization source is coupled with an ultrahigh resolution Orbitrap MS to perform halogen detection of bromine and iodine as initial analytes. This facilitates simple and sensitive detection of these elements as atomic anions from simple aqueous salt solutions. Collision-induced dissociation (CID) and higher-energy collisional dissociation (HCD) energies were optimized to produce the maximum response of Br − and I − . The LS-APGD conditions were optimized using a design of experiments (DOE) approach for Br − and I − concurrently. Response curves for Br − and I − solutions determined limit of detection (LOD) values of 50 pg and 5 pg, respectively, in 20 μL aliquots. The curves indicated response factors of 0.67 for 79 Br − and 0.90 for 127 I − . Br isotope ratios were determined with precision between 0.7 and 7.3% RSD, with the isotope ratios determined with precision 0.8% RSD at concentrations above the limit of quantification. Preliminary tests were conducted to evaluate the effect of different cations (Na + , K + , and Mg 2+ ) on Br − responses, with no discernible impacts observed on the halogen signal responses. This study demonstrates the potential use of the LS-APGD-Orbitrap-MS for the detection of multiple halogens while avoiding interferences, minimizing sample preparation, and overcoming ionization barriers.

Lang, Dehlia A. [Clemson University, SC (United St↗