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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Studying microbially induced corrosion on glass using ToF-SIMS

Microbially induced corrosion (MIC) is an emerging topic that has huge environmental impacts, such as long-term evaluation of microbial interactions with radioactive waste glass, environmental cleanup and disposal of radioactive material, and weathering effects of microbes. Time-of-flight secondary ion mass spectrometry (ToF-SIMS), a powerful mass spectral imaging technique with high surface sensitivity, mass resolution, and mass accuracy, can be used to study biofilm effects on different substrates. Understanding how to prepare biofilms on MIC susceptible substrates is critical for proper analysis via ToF-SIMS. We present here a step-by-step protocol for preparing bacterial biofilms for ToF-SIMS analysis, comparing three biofilm preparation techniques: no desalination, centrifugal spinning (CS), and water submersion (WS). Comparisons of two desalinating methods, CS and WS, show a decrease in the media peaks up to 99% using CS and 55% using WS, respectively. Proper desalination methods also can increase biological signals by over four times for fatty acids using WS, for example. ToF-SIMS spectral results show chemical compositional changes of the glass exposed in a Paenibacillus polymyxa SCE2 biofilm, indicating its capability to probe microbiologically induced corrosion of solid surfaces. This represents the proper desalination technique to use without significantly altering biofilm structure and substrate for ToF-SIMS analysis. ToF-SIMS spectral results showed chemical compositional changes of the glass exposed by a Paenibacillus bacterial biofilm over 3-month inoculation. Finally, possible MIC products include various phosphate phase molecules not observed in any control samples with the highest percent increases when experimental samples were compared with biofilm control samples.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Altering the solubility of metal–organic polyhedra via pendant functionalization of Cp 3 Zr 3 O(OH) 3 nodes

Here, the chemistry of zirconium-based metal-organic polyhedra (ZrMOPs) is often limited by their poor solubilities. Despite their attractive features—including high yielding and facile syntheses, predictable topologies, high stability, and tunability—problematic solubilities have caused ZrMOPs to be under-studied and under-applied. Although these cages have been synthesized with a wide variety of carboxylate-based bridging ligands, we explored a new method for ZrMOP functionalization via node-modification, which we hypothesized could influence solubility. Herein, we report ZrMOPs with benzyl-, vinylbenzyl-, and trifluoromethylbenzyl-pendant groups decorating cyclopentadienyl moieties. The series was characterized by 1 H/ 19 F NMR, high-resolution mass spectrometry, infrared spectroscopy, and single-crystal X-ray diffraction. The effects of node functionalities on ZrMOP solubility were quantified using inductively coupled plasma mass spectrometry. Substitution caused a decrease in water solubility, but for certain organic solvents, e.g. DMF, solubility could be enhanced by ~20×, from 16 μM for the unfunctionalized cage to 310 μM for the vinylbenzyl- and trifluoromethylbenzyl-cages.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Continuous measurements of volatile gases as detection of algae crop health

Wide adoption of algae cultivation to produce environmentally sustainable biofuels and fine chemicals is currently hampered by large losses (10 to 30%) incurred by grazer infections. We show the usage of real-time chemical ionization mass spectrometry to rapidly identify gaseous indicators of grazer infections in cyanobacteria cultures. Grazing was detected significantly faster (up to 3 d) using real-time mass spectrometry than the current methods of microscopy and qPCR. By employing this technology, cultivators may be empowered to treat grazer infestations sooner, thereby protecting the crop and enhancing profitability.

09 BIOMASS FUELS↗
DOE OSTI2023

malbacR: A Package for Standardized Implementation of Batch Correction Methods for Omics Data

Mass spectrometry is a powerful tool for identifying and analyzing small molecules, such as metabolites and lipids, in com-plex biological samples. Liquid chromatography and gas chromatography mass spectrometry studies quite commonly in-volve large numbers of samples, which can require significant time for sample preparation and analyses. To accommodate such studies, the samples are commonly split into batches. Inevitably, variations in sample handling, temperature fluctua-tion, imprecise timing, column degradation and other factors result in systematic errors or biases of the measured abundances between the batches. Numerous methods are available via R packages to assist with batch correction for small molecule om-ics data; however, since these methods were developed by different research teams, the algorithms are available in separate R packages, each with different data input and output formats. We introduce the malbacR package which consolidates eleven common batch effect correction methods for small molecule omics data into one place so users can easily implement and compare: pareto scaling, power scaling, range scaling, ComBat, EigenMS, NOMIS, RUV-random, QC-RLSC, WaveI-CA2.0, TIGER, and SERRF. The malbacR package standardizes data input and output formats across these batch correction methods. The package works in conjunction with the pmartR package, allowing users to seamlessly include batch effect cor-rection in a pmartR workflow without needing any additional data manipulation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

US-DOE and Republic of South Africa Uranium Benchmarking: Results From Los Alamos National Laboratory (Study Report)

This report details work performed at Los Alamos National Laboratory (LANL) in support of an interlaboratory uranium (U) benchmarking collaboration between LANL, Lawrence Livermore National Laboratory (LLNL), and South African Nuclear Energy Corporation (Necsa). The goal of this interlaboratory benchmarking exercise is to compare analytical methods and data obtained on uranium reference materials CUP-2 and New Brunswick Laboratory (NBL) certified reference material (CRM) 124-2. The LANL commitments for this project include performing microwave digestion of fresh CUP-2 and CRM 124-2 powders, measuring the U isotope composition of CUP-2 and CRM 124-2 by both single-collector and multi-collector inductively coupled plasma mass spectrometry (SC-ICP-MS and MC-ICP-MS, respectively), and determining trace-element abundances in CUP-2 and CRM 124-2 by inductively coupled plasma mass spectrometry (ICP-MS). This report details the methods employed by LANL in support of these objectives and presents the data obtained during this collaborative exercise.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2026

Unveiling the High‐Voltage Reactivity and Gas Evolution With Aluminum‐Based Chloride and Oxychloride Catholytes in Solid‐State Sodium Batteries

All-solid-state sodium batteries (ASSBs) employing halide solid electrolytes (SEs) offer a cost-effective and energy-dense alternative to conventional liquid electrolyte systems. However, their high voltage (>4 V vs. Na/Na + ) performance remains limited by interfacial instability between the cathode active material (CAM) and the SE. We present here the electrochemical and interfacial behaviors of crystalline NaAlCl 4 and amorphous sodium–aluminum–oxychloride (NACO) SEs when combined with NaNi 0.5 Mn 0.5 O 2 cathode. While oxygen incorporation in NACO enhances ionic conductivity by nearly three orders of magnitude relative to NaAlCl 4 , it does not improve high-voltage cycling stability. Cells employing NACO exhibit accelerated capacity fade, increased cell impedance growth, and intrinsic oxygen evolution above 4.5 V vs. Na 3 Sn, as revealed by operando electrochemical mass spectrometry. In contrast, the NaAlCl 4 -based cells show no detectable gas release, underscoring their superior high-voltage stability and safety. Time-of-flight secondary-ion mass spectrometry confirms the formation of Al─O and Ni/Mn─Cl species, respectively, in the SE and CAM, indicating redox-driven anion exchange that contributes to kinetic hindrance of high-voltage phase transitions. The findings establish that while oxygen incorporation enhances ionic transport, it can compromise interfacial stability, suggesting pure chloride SEs may offer a more robust and intrinsically safer pathway for developing high-energy ASSBs.

25 ENERGY STORAGE↗
NASA NTRS1990

Development of microchannel plates in advanced wind-tunnel instrumentation

Microchannel plate (MCP) electron multiplier dynamic range has been increased 3 to 4 orders of magnitude at ambient temperatures, through enhanced input count rate capability and reduced background or 'dark' noise. The previous upper limit of roughly 10(exp 7) - 10(exp 8) cm(exp -2)s(exp -1) at ambient has been extended to levels approach 10(exp 10) cm(exp -2)s(exp -1) under continuous dc operation. The lower limit, previously set by an irreducible background component (approximately 0.6 cm(exp -2)s(exp -1)), has been lowered to the cosmic ray limit of .01 cm(exp -2)s(exp -1). The high end improvement was achieved by conductively cooling a very low resistance MCP by bonding it to a heat sink, while maintaining pulse-counting operation with multianode readouts. The low-end improvement was achieved by removing all radioisotopes from the MCP matrix glass. The detectors will benefit optical and mass spectrometry, flow visualization, plasma diagnostics, magnetometry, and other high signal flux applications. Very low MCP background noise will benefit X-ray and UV astronomy, medical imaging, trace isotope mass spectrometry, and other applications where the signal flux is often extremely low.

Feller, W. Bruce↗
NASA NTRSDate not supplied

Investigating Commercial Off-The-Shelf (COTS) Glovebox and Support Components Compared to Custom Curatorial Laboratories

There is a need envisioned to investigate the application of commercial off-the-shelf (COTS) systems as tools that could be used within commercial preliminary curation as the expected space economy is supported and begins to take flight. NASA is involved with supporting and developing the space economy [1] and therefore it’s feasible that at some point, a commercial space company would bring back materials and either store initially, or permanently, within COTS equipment as a stand-in for custom curation laboratories. While utilizing opportunities to explore this capability at NASA-Johnson Space Center (JSC) during the establishment of other laboratories [2] it was realized that cleanliness and/or other properties could be evaluated for these COTS systems during their installation in advanced research facilities that are not ISO-class rated clean rooms. Several aspects of a COTS-Curation system were explored including various gloves for curation manipulation within a negative pressure glovebox (Fig.1), Balazs organic and inorganic contaminant levels testing prior to glovebox ever being used, mode swapping comparison of recirculation vs. single pass, constant monitoring of oxygen (O2) and moisture (H2O) levels in various conditions, etc. To acquire inorganic and organic compound loads inside the glovebox, Balazs wafer testing and gas sampling were implemented. These are standardized analytical tests provided by Balazs™ NanoAnalysis, a division of Air Liquide USA. Deployment of 8-inch silicon wafer witness plates for 24-hours in an undisturbed environment capture the organic compound load and inorganic trace metal contents which can be obtained by Vapor Phase Decomposition Inductively Coupled Plasma Mass Spectrometry (VPD ICP-MS). Balazs gas sample analysis was also performed for better measurements of volatile organic compounds (VOC) in glovebox air analyzed by Thermal Desorption Gas Chromatography Mass Spectrometry (TD GC-MS). These analytical testings were carried out in a controlled ultra high pure (UHP) gaseous nitrogen (N2)-purged environment where oxygen and moisture contents were continuously monitored at certain temperature and pressure. The preliminary outcomes of these testings are promising. The COTS systems appear to maintain the steady-state controlled environment for days, if not weeks, with uninterrupted gaseous N2-supply which was operated from a standard medium pressure LN2 250L 230L dewar, exchanged as needed. The outgassing load can be maintained by selecting the glove materials that have the least outgassing and particle shedding performances. Further experiments will be considered to validate the preliminary findings. While this project is exploratory, it is not intended as an endorsement by NASA Curation for approved materials or usage for advanced curatorial activities. NASA does not endorse nor promote any one particular product or company. References: [1] McCubbin F. M. et al. (2019) Space Science Reviews 215:A48. [2] Lewis, E.K. et. al (2024) LPSC LV, Abstract #2457.

Curation↗
DOE OSTI2025

C136A and C138A Report of Analysis

In this work the isotopic ratios and weight percentages of 238 Pu, 239 Pu, 240 Pu, 241 Pu and 242 Pu were determined using Isotope Dilution Mass Spectrometry. Two samples of C136A and C138A were sent to the Analytical Research laboratories by the National Nuclear Security Administration Nuclear Reference Material Program. The four samples were dissolved in concentrated hydrochloric acid. From the parent solutions, eight aliquots were taken, diluted, spiked with 244 Pu and submitted to separations. After the samples were separated, they were analyzed using Multicollector Inductively Coupled Plasma Mass Spectrometry. Along with the samples, two C126A Quality Control Samples were analyzed each day. Mass bias standards were also analyzed at the beginning, during and at the end of the analysis. GUM Workbench Pro software Version 2.4.1.406 was used to calculate the isotopic ratios relative to 239 Pu, and total Pu mass and the correlated expanded uncertainties.

37 - INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL C↗
NASA NTRS1990

Application of reversal electron attachment for ultrasensitive detection of thermal electron-attaching molecules - CCl4 and C6H5O2

A standard gas-dilution method was used to determine the selective response of the reversal electron attachment detector to carbon tetrachloride concentrations in nitrogen. Data are provided that determine the lowest concentration of sample detectable with the present instrumental configuration as being below 1.0 part per trillion by volume. The incorporation of a 90-deg electrostatic deflector with the quadrupole mass spectrometer is shown to be vital, and with it, negative-ion quadrupole mass spectrometry is used to characterize the ionization process. Observations are also made of the reversal electron attachment response to nitrobenzene. The analytical potential of reversal electron capture negative-ion mass spectrometry is examined, and areas for future development are discussed.

Bernius, Mark T.↗
DOE OSTI2022

Assessing Long-Term Cycling Stability of Single-Crystal Versus Polycrystalline Nickel-Rich NCM in Pouch Cells with 6 mAh cm -2 Electrodes

Lithium-ion batteries based on single-crystal LiNi1-x-yCoxMnyO2 (NCM, 1-x-y ≥ 0.6) cathode materials are gaining increasing attention due to their improved structural stability resulting in superior cycle life compared to batteries based on polycrystalline NCM. However, an in-depth understanding of the less pronounced degradation mechanism of single-crystal NCM is still lacking. Here, a detailed postmortem study is presented, comparing pouch cells with single-crystal versus polycrystalline LiNi 0.60 Co 0.20 Mn 0.20 O 2 (NCM622) cathodes after 1375 dis-/charge cycles against graphite anodes. The thickness of the cation-disordered layer forming in the near-surface region of the cathode particles does not differ significantly between single-crystal and polycrystalline particles, while cracking is pronounced for polycrystalline particles, but practically absent for single-crystal particles. Transition metal dissolution as quantified by time-of-flight mass spectrometry on the surface of the cycled graphite anode is much reduced for single-crystal NCM622. Similarly, CO 2 gas evolution during the first two cycles as quantified by electrochemical mass spectrometry is much reduced for single-crystal NCM622. Benefitting from these advantages, graphite/single-crystal NMC622 pouch cells are demonstrated with a cathode areal capacity of 6 mAh cm -2 with an excellent capacity retention of 83% after 3000 cycles to 4.2 V, emphasizing the potential of single-crystalline NCM622 as cathode material for next-generation lithium-ion batteries.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Highlighting the Importance of Authentic Reference Chemicals in the Unambiguous Identification of Unknowns during Routine Sample Analysis─An OPCW Proficiency Test Case

The unequivocal identification of unknown chemicals during routine sample analysis is a constant occurrence in the field of analytical chemistry. The process can be painstakingly tedious, particularly in situations where a tentatively identified unknown may possess isomeric counterparts yielding identical accurate mass values and very similar mass spectra. In this work, we present the experimental process involved in the correct identification of 1,4-oxathiane 4,4-dioxide and differentiation from its constitutional isomer, 2-hydroxyethyl vinyl sulfone, when present in a silica gel matrix featured in the 54th Environmental Organisation for the Prohibition of Chemical Weapons (OPCW) proficiency test. After discovering that the library-generated mass spectrum for 2-hydroxyethyl vinyl sulfone in a preliminary gas chromatography–mass spectrometry (GC-MS) analysis did not match the one from an authentic reference chemical, we embarked on an unknown structure determination campaign involving GC-MS, liquid chromatography-tandem mass spectrometry (LC-MS-MS), and nuclear magnetic resonance (NMR) spectroscopy. All of the information obtained, coupled to the synthesis of an authentic reference chemical, was used to determine the identity of the unknown as 1,4-oxathiane 4,4-dioxide. The process described in this work highlights the important role played by authentic reference chemicals in the identification of unknown chemicals during routine sample analysis.

Chemistry↗
DOE OSTI2021

Huntingtin structure is orchestrated by HAP40 and shows a polyglutamine expansion-specific interaction with exon 1

Huntington’s disease results from expansion of a glutamine-coding CAG tract in the huntingtin (HTT) gene, producing an aberrantly functioning form of HTT. Both wildtype and disease-state HTT form a hetero-dimer with HAP40 of unknown functional relevance. Here, we demonstrate in vivo and in cell models that HTT and HAP40 cellular abundance are coupled. Integrating data from a 2.6 Å cryo-electron microscopy structure, cross-linking mass spectrometry, small-angle X-ray scattering, and modeling, we provide a near-atomic-level view of HTT, its molecular interaction surfaces and compacted domain architecture, orchestrated by HAP40. Native mass spectrometry reveals a remarkably stable hetero-dimer, potentially explaining the cellular inter-dependence of HTT and HAP40. The exon 1 region of HTT is dynamic but shows greater conformational variety in the polyglutamine expanded mutant than wildtype exon 1. Our data provide a foundation for future functional and drug discovery studies targeting Huntington’s disease and illuminate the structural consequences of HTT polyglutamine expansion.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

R-Value Measurements Performed on Uranium Targets Irradiated with Fission Spectrum Neutrons FY 2021 for F2019 Project

The separation and characterization of two irradiated uranium targets, a depleted uranium (DU) and a highly enriched uranium (HEU) target, was conducted in April of 2021. The two targets were assembled at Los Alamos National Laboratory (LANL) and irradiated using the critical assembly at the National Criticality Experiments Research Center (NCERC). Splits of the dissolved targets were received by Pacific Northwest National Laboratory (PNNL) after which the PNNL and LANL teams chemically separated the solutions using independent separation schemes and analyzed the separated fractions for short lived actinides and fission products. Chemical separations at PNNL were traced with stable or radioactive tracers to allow for the determination of chemical yields, analyzing using either inductively coupled plasma optical emission spectroscopy (ICP-OES), inductively coupled plasma mass spectrometry (ICP-MS) or gamma emission analysis (GEA) depending on the nature of the tracer. Several other analytical techniques were used by PNNL including kinetic phosphorescence analysis (KPA) and thermal ionization mass spectrometry (TIMS) depending on the analyte’s need. Comparisons were made between current and historical PNNL and LANL, as well as literature values. Overall, there was agreement between the two laboratories for the bulk of analytes, with some notable exceptions such as 111 Ag, and 141,143,144 Ce. Included in these comparisons were the short-lived actinides 237 U, 239 Np, the fission products 89 Sr, 91 Y, 95/97 Zr, 99 Mo, 111 Ag, 115/115 mCd, 136/137 Cs, 140 Ba, 141/143/144 Ce, 147 Nd, 153 Sm, 156 Eu, and 161 Tb, providing both total atoms as well as the R-values. The data presented in this report represents the sixth NCERC irradiation of HEU and DU (FY13, FY14, FY15, FY17, FY18, FY21), and their subsequent separation and analysis.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1995

Analytical pyrolysis experiments of Titan aerosol analogues in preparation for the Cassini Huygens mission

Comparative pyrolysis mass spectrometric data of Titan aerosol analogs, called 'tholins', are presented. The Titan tholins were produced in the laboratory at Cornell by irradiation of simulated Titan atmospheres with high energy electrons in plasma discharge. Mass-spectrometry measurements were performed at FOM of the solid phase of various tholins by Curie-point pyrolysis Gas-Chromatography/Mass-Spectrometry (GCMS) and by temperature resolved in-source Pyrolysis Mass-Spectrometry to reveal the composition and evolution temperature of the dissociation products. The results presented here are used to further define the ACP (Aerosol Collector Pyrolyser)-GCMS experiment and provide a basis for modelling of aerosol composition on Titan and for the iterpretation of Titan atmosphere data from the Huygens probe in the future.

Ehrenfreund, P.↗
NASA NTRS1989

Arc jet diagnostics tests

Two objectives were addressed during a 10 week 1988 NASA/ASEE summer faculty fellowship at the Johnson Space Center Atmospheric Reentry Materials Structures Evaluation Facility (ARMSEF). These objectives were the evaluation of mass spectrometry for the measurement of atomic and molecular species in an arc jet environment, and the determination of atomic recombination coefficients for reaction cured glass (RCG) coated high temperature surface insulation (HRSI) materials subjected to simulated reentry conditions. Evaluation of mass spectrometry for the measurement of atomic and molecular species provided some of the first measurements of point compositions in arc jet tunnel environments. A major objective of this project centered around the sampling residence time. A three staged vacuum sampling system pulled the molecules and atoms from the arc jet to a quadrupole ionization mass spectrometer in 400 milliseconds. Conditions investigated included a composition survey across the nozzle exit at 3 cm z-distance from the nozzle exit for 3 different currents. Also, a point composition survey was taken around a shock created by the presence of a blunt body.

Willey, Ronald J.↗
DOE OSTI2021

Revealing functional insights into ER proteostasis through proteomics and interactomics

The endoplasmic reticulum (ER), responsible for processing approximately one-third of the human proteome including most secreted and membrane proteins, plays a pivotal role in protein homeostasis (proteostasis). Dysregulation of ER proteostasis has been implicated in a number of disease states. As such, continued efforts are directed at elucidating mechanisms of ER protein quality control which are mediated by transient and dynamic protein-protein interactions with molecular chaperones, co-chaperones, protein folding and trafficking factors that take place in and around the ER. Technological advances in mass spectrometry have played a pivotal role in characterizing and understanding these protein-protein interactions that dictate protein quality control mechanisms. Here, we highlight the recent progress from mass spectrometry-based investigation of ER protein quality control in revealing the topological arrangement of the proteostasis network, stress response mechanisms that adjust the ER proteostasis capacity, and disease specific changes in proteostasis network engagement. We close by providing a brief outlook on underexplored areas of ER proteostasis where mass spectrometry is a tool uniquely primed to further expand our understanding of the regulation and coordination of protein quality control processes in diverse diseases.

60 APPLIED LIFE SCIENCES↗