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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Development of a Platform for High-Resolution Ion Mobility Separations Coupled with Messenger Tagging Infrared Spectroscopy for High-Precision Structural Characterizations

The ability to uniquely identify a compound requires highly precise and orthogonal measurements. Here we describe a newly developed analytical platform that integrates high resolution ion mobility and cryogenic vibrational ion spectroscopy for high-precision structural characterizations. This platform allows for the temporal separation of isomeric/isobaric ions and provides a highly sensitive description of the ion’s adopted geometry in the gas phase. The combination of these orthogonal structural measurements yields precise descriptors that can be used to resolve between and confidently identify highly similar ions. The unique benefits of our instrument, which integrates a structures for lossless ion manipulations ion mobility (SLIM IM) device with messenger tagging infrared spectroscopy, include the ability to perform high-resolution ion mobility separations and to record the IR spectra of all ions simultaneously. The SLIM IM device, with its 13 m separation path length, allows for multipass experiments to be performed for increased resolution as needed. It is integrated with an Agilent qTOF MS where the collision cell was replaced with a cryogenically held (30 K) TW-SLIM module. The cryo-SLIM is operated in a novel manner that allows ions to be streamed through the device and collisionally cooled to a temperature where they can form noncovalently bound N 2 complexes that are maintained as they exit the device and are detected by the TOF mass analyzer. The instrument can be operated in two modes: IMS+IR where the IR spectra for mobility-selected ions can be recorded and IR-only mode where the IR spectra for all mass-resolved ions can be recorded. In IR-only mode, IR spectra (400 cm –1 spectral range) can be recorded in as short as 2 s for high throughput measurements. Further, this work details the construction of the instrument and modes of operation. It provides initial benchmarking of CCS and IR measurements to demonstrate the utility of this instrument for targeted and untargeted approaches.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Comprehensive structural characterization of charged polymers involved in moisture-driven direct air capture

This study provides a comprehensive structural characterization of commercially available alkaline anion-exchange polymers (Fumasep FAA-3 and IRA 900) used in moisture-driven direct air capture (DAC) of carbon dioxide. Using X-ray diffraction, SAXS/WAXS, atomic force microscopy, FIB-SEM, and transmission electron microscopy, the authors identify nanoscale clustering, porosity, swelling behavior, and humidity-dependent structural changes that influence CO₂ adsorption and release. These findings establish structure–function relationships critical for designing more durable and energy-efficient DAC polymer materials.

36 MATERIALS SCIENCE↗
NASA NTRS2003

Synthesis,and structural characterization of [(CH3(C5H4N))Ga(SCH2(CO)O)]-[(4-MepyH)]+, a novel Ga(III) five coordinate complex.

The synthesis and structural characterization of a novel ionic Ga(III) five coordinate complex [{CH3(C5H4N)}Ga(SCH2(CO)O)2]-[(4-MepyH)]+, (4-Mepy = CH3(C5H5N)) from the reaction between Ga2Cl4 with sodium mercapto-acetic acid in 4-methylpyridine is described. Under basic reaction conditions the mercapto ligand is found to behave as a 2e- bidentate ligand. Single crystal X-ray diffraction studies show the complex to have a distorted square pyramidal geometry with the [(-SCH2(CO)CO-)] ligands in a trans conformation. The compound crystallizes in the P2(sub 1)/c (No. 14) space group with a = 7.7413(6) A, b = 16.744(2) A, c = 14.459(2) A, V = 1987.1(6) A(sup 3), R(F) = 0.032 and R(sub w) = 0.038.

Banger, Kulbinder K.↗
NASA NTRS2004

Synthesis and Structural Characterization of a Novel Indium Mercapto Derivative [clln(sch2(co)o)2]2-[(4-mepyh)2]2+

The synthesis and structural characterization of a novel In(III) complex is described. The reaction between InCl3 with sodium mercapto-acetic acid, (NaSCH2(CO)OH) in 4-methylpyridine, (CH3(C5H5N), (4-Mepy)) at 25 C affords [ClIn(SCH2(CO)O)2]2- [(4-MepyH)2]2+. X-ray diffraction studies show it to have a distorted square pyramidal geometry, with the [(-SCH2(CO)CO-)] ligands in a trans conformation. The compound crystallizes in the P(raised dash) 1 (No. 2) space group with a = 7.8624 Angstrom, b = 9.950 Angstrom, c = 13.793 Angstrom, alpha = 107.60 degrees, beta= 90.336 degrees, gamma = 98.983 degrees, V = 1014.3 Angstroms (sup 3), R(F(raised circle)) = 0.037, and R(sub w) = 0.048.

Banger, Kulbinder K.↗
DOE OSTI2022

Reduced diffusion and enhanced retention of multiple radionuclides from pore structure characterization of barrier materials for enhanced repository performance

Fluid flow and chemical transport in porous media are the macroscopic consequences of pore structure, which integrates geometry (e.g., pore size and surface area, pore-size distribution) and topology (e.g., pore connectivity). Low-permeability geological media whose pores are poorly interconnected will exhibit the characteristics of anomalous diffusion and sample size-dependent effective porosity, which will strongly impact long-term net diffusion and retention of radionuclides in geological repository settings involving different host rocks and barrier materials. A suite of innovative and complementary experimental approaches is utilized to study the microscopic pore structure and macroscopic fluid flow & chemical transport for a range of host rocks and barrier materials, in addition to standard clay minerals and reference rocks. With a particular focus on quantifying the presence and magnitude of “isolated” pores for a reduced effective porosity in low-permeability geomedia, the integrated methodologies for basic properties and pore structure characterization of these geomedia include X-ray diffraction, thin section petrography, grain size distribution, water immersion porosimetry after vacuum-pulling for full saturation, mercury intrusion porosimetry, nitrogen physisorption, scanning electron microscopy, X-ray computed tomography, and (ultra-)small angle neutron (X-ray) scattering. In addition, custom-designed gas diffusion, tracer recipe involving a range of anionic and cationic chemicals with subsequent analyses by laser ablation and inductively coupled plasma-mass spectrometry, along with batch sorption, column transport, and imbibition tests were conducted for coupled effects of pore structure and chemical retention/transport. From the perspectives of pore structure in conjunction with multiple and complementary approaches to examining a range of sample sizes under different observational scales, we find that the poor pore connectivity is prevalent in low-permeability media (mudstone and crystalline rock) that is related to geological processes (e.g., compaction, diagenesis and thermal maturation). For example, the deep and organic matter-rich mudstones have a much smaller effective porosity than the total porosity (as a result of poor pore connectivity) and associated diffusion coefficient, and the effective porosity & diffusion coefficients are also dependent upon the sample sizes used in the measurement. Similarly, most of the pore space in the shallow mudstone is also controlled by pore-throat diameters in the 5-50 nm range of intergranular pore types from its fine-grained nature, but with an overall good pore connectivity. However, the nm-sized pore space (physically pore-network architecture) and strong sorption capacities (chemical retention from clay minerals) of both shallow and deep mudstones lead to the synergistic retention of cationic radionuclides and their utilities as effective host rocks and barrier materials. Our unique approaches of studying how the micro-scale pore structure affect macro-scale fluid flow, diffusion & retention, and chemical transport produce improved mechanistic understanding, and realistic quantification, of diffusion and retention of typical radionuclides in a range of generic host rocks and barrier materials (clay/shale, salt, crystalline rock, and tuff), with the overall results leading to scientifically-based understanding of enhanced isolation (from both diffusion and retention) of radionuclides and improved confidence on the long-term performance of geological repository to store high-level radioactive wastes. In addition to the training of 25 undergraduates, graduates, and postdocs of UTA, the scientists (organizations) involved in performing this work (e.g., discussion, sample sharing, and operation of SANS and SAXS instruments) include Ed Matteo, Yifeng Wang, and Kristopher Kuhlman (Sandia National Laboratories), Jens Birkholzer, Liange Zheng, Tim Kneafsey, and Sharon Borglin (Lawrence Berkeley National Laboratory), Mavrik Zavarin (Lawrence Livermore National Laboratory), Yukio Tachi and Yuta Fukatsu (Japan Atomic Energy Agency), Mieke de Craen (Euridice, Belgium), Markus Bleuel (NIST), Wei-Ren Chen, Gergely Nagy, Changwoo Do, William Heller, Larry Anovitz, and Kenneth Littrell (ORNL), as well as Jan Illvsky, Ivan Kuzmenko, Ju-Sang Park and Jon Almers (ANL). Key deliverables include a total of 13 peer-reviewed journal articles (nine published and three under review), 23 presentations at scientific conferences (AAPG, AAPG Southwest Section, AGU, Asian Clay Conference, GSA, GSA South-Central Section, IHLRWM, InterPore, International Conference on Chemistry and Migration Behavior of Actinides and Fission Products in the Geosphere, International Conference on Coupled Processes in Fractured Geological Media: Observation, Modeling and Application), and academic institutions (UTA, New Mexico State University; University of Poitiers, France; University of Helsinki, Finland; Uppsala University, Sweden; Istanbul Technical University, Turkey) and other organizations (Andra, France; Posiva Oy, Finland).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Multiscale Structural Characterization of a Smectic Liquid Crystalline Elastomer upon Mechanical Deformation Using Neutron Scattering

Liquid crystalline elastomers (LCEs) exhibit unique shape memory behavior due to the combination of liquid crystalline orientation and rubber elasticity. Multiscale structural characterization of these materials upon deformation is crucial to understanding their structure–property relationships. In this work, the structure evolution of an epoxy-based, main-chain LCE with deuterated flexible spacers upon uniaxial mechanical deformation is investigated at different length scales. Wide-angle and small-angle X-ray scattering (WAXS/SAXS) reveal the presence of smectic polymorphism and rotations of the smectic domains upon mechanical stretching, which is also confirmed by small-angle neutron scattering (SANS). Importantly, the selective deuteration enables an improved neutron scattering contrast between the smectic and amorphous domains. SANS patterns of the deformed, deuterated LCE exhibit strong scattering streaks that are not observed in SAXS or SANS of hydrogenated LCE, indicating the presence of highly aligned amorphous domains. The macroscopic orientation also results in the formation of structures in the micrometer scale revealed by the ultrasmall-angle neutron scattering (USANS) experiment.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Multielectrode electrochemical cell for in situ structural characterization of amorphous thin-film catalysts using high-energy X-ray scattering

A multielectrode-based electrochemical cell allows the structural characterization of an amorphous thin-film water oxidation catalyst under various electrochemical potentials using high-energy X-ray scattering and atomic pair distribution function (PDF) techniques. A multielectrode with five electrodes provides a sufficiently low background signal to enable high-energy X-ray scattering (HEXS) measurements and amplifies the extremely low HEXS signals from samples for high-resolution PDF analysis of in situ data from thin-film catalysts. Glassy carbon (GC) creates a relatively low intensity HEXS pattern and is used as a working electrode. Instead of a three-dimensional (3D) porous electrode architecture, the flat geometry of the electrode enables various deposition techniques to be used for the preparation of a highly conductive metal oxide layer. PDF analysis demonstrates high spatial resolution for a 230 nm thick amorphous iridium oxide film deposited on two roughened 60 µm thick GC electrodes. The PDF analysis resolves the domain size and distinguishes changes in fine structure which are directly correlated with the structure and function of the catalysts. In conclusion, the results bring the opportunity to analyze the structure of nanometre-scale amorphous thin-film catalysts in an electrolyte-compatible and compact 3D-printed electrochemical cell in a three-electrode configuration.

36 MATERIALS SCIENCE↗
NASA NTRS1992

Structural characterization of an articulated-truss joint

A first generation space crane articulated-truss joint was statically and dynamically characterized in a configuration which approximated an operational environment. The articulated-truss joint was integrated into a test bed for structural characterization. Static characterization was performed by applying known loads and measuring the corresponding deflections to obtain load-deflection curves. Dynamic characterization was performed using modal testing to experimentally determine the first six mode shapes, frequencies, and modal damping values. The static and dynamic characteristics were also determined for a reference truss, which served as a characterization baseline. Load-deflection curves are presented for the reference truss, and the articulated-truss joint mounted in the test bed. The static and dynamic experimental results are compared to analytical predictions obtained from finite element analyses. The load-deflection response is also presented for one of the linear actuators used in the articulated-truss joint. Finally, an assessment is presented for the predictability of the truss hardware used in the reference truss and articulated-truss joint based upon hardware stiffness properties which were previously obtained during the Precision Segmented Reflector (PSR) Technology Development Program.

Sutter, Thomas R.↗
NASA NTRS1992

Structural characterization of a first-generation articulated-truss joint for space crane application

A first-generation space crane articulated-truss joint was statically and dynamically characterized in a configuration that approximated an operational environment. The articulated-truss joint was integrated into a test-bed for structural characterization. Static characterization was performed by applying known loads and measuring the corresponding deflections to obtain load-deflection curves. Dynamic characterization was performed using modal testing to experimentally determine the first six mode shapes, frequencies, and modal damping values. Static and dynamic characteristics were also determined for a reference truss that served as a characterization baseline. Load-deflection curves and experimental frequency response functions are presented for the reference truss and the articulated-truss joint mounted in the test-bed. The static and dynamic experimental results are compared with analytical predictions obtained from finite element analyses. Load-deflection response is also presented for one of the linear actuators used in the articulated-truss joint. Finally, an assessment is presented for the predictability of the truss hardware used in the reference truss and articulated-truss joint based upon hardware stiffness properties that were previously obtained during the Precision Segmented Reflector (PSR) Technology Development Program.

Sutter, Thomas R.↗
DOE OSTI2022

Structural characterization of a soil viral auxiliary metabolic gene product – a functional chitosanase

Metagenomics is unearthing the previously hidden world of soil viruses. Many soil viral sequences in metagenomes contain putative auxiliary metabolic genes (AMGs) that are not associated with viral replication. Here, we establish that AMGs on soil viruses actually produce functional, active proteins. We focus on AMGs that potentially encode chitosanase enzymes that metabolize chitin – a common carbon polymer. We express and functionally screen several chitosanase genes identified from environmental metagenomes. One expressed protein showing endo-chitosanase activity (V-Csn) is crystalized and structurally characterized at ultra-high resolution, thus representing the structure of a soil viral AMG product. This structure provides details about the active site, and together with structure models determined using AlphaFold, facilitates understanding of substrate specificity and enzyme mechanism. Our findings support the hypothesis that soil viruses contribute auxiliary functions to their hosts.

59 BASIC BIOLOGICAL SCIENCES↗
NASA NTRS1988

Some instrumentation requirement issues for the Space Station structural characterization experiment

The Space Station will provide unique opportunities to the research and technology community as a national in-space research facility. Opportunities will exist for technology experiments in a variety of disciplines, including dynamics and control of large space structures (LSS). The Space Station Structural Characterization Experiment (SSSCE) is an early space station technology experiment now under development. The objective of the experiment is to instrument and use the Space Station as a generic research test article, in support of research and technology activities in the areas of structural dynamics and control/structure interaction (CSI). Tests will be conducted, potentially, on each assembly flight configuration, as well as on the phase 1 configuration. Structural dynamic response data will be measured and transferred to the ground for analysis. These measurements will support the development and in-space verification of system identification and analytical modeling techniques for future LSS, including the evolutionary Space Station. The paper begins by restating the principal objective of SSSCE, along with the basic approach that will be used. The body of the paper deals with instrumentation requirement issues. The paper closes with several questions concerning modal-testing objectives and limitations, a brief review of a previous on-orbit experiment, the Solar Array Flight Experiment, and concluding remarks.

Pappa, Richard S.↗
DOE OSTI2025

Hydrogen bonding to the formate ligand: Structural characterization of 2,2′:6′,2″-terpyridine zinc formate·H 2 O

Here, two polymorphs of the 2,2’:6’,2”-terpyridine zinc formate compound (terpy)Zn(O 2 CH) 2 •H 2 O have been structurally characterized by X-ray diffraction. In each case, the formate ligands coordinate via a K 1 -monodentate coordination mode and participate in hydrogen bonding interactions with water molecules. Despite this similarity, however, the polymorphs exhibit different hydrogen bonding motifs. Specifically, while one polymorph forms chains in which water molecules link adjacent (terpy)Zn(O 2 CH) 2 molecules, the other polymorph consists of discrete tetranuclear [(terpy)Zn(O 2 CH) 2 •H 2 O] 4 moieties.

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

Synthesis and structural characterization of 2,2′:6′,2″-terpyridine zinc formate: Hydroboration and hydrosilylation of CO 2 and carbonyl compounds

The zinc formate compound (terpy)Zn(O 2 CH) 2 is obtained via the reaction of Zn(O 2 CH) 2 with 2,2′:6′,2″-terpyridine (terpy) and has been structurally characterized by X-ray diffraction as possessing formate ligands that coordinate via a κ 1 -monodentate coordination mode, which is in accord with IR spectroscopic studies. In terms of reactivity, (terpy)Zn(O 2 CH) 2 participates in catalytic transformations involving CO 2 and carbonyl compounds via hydrosilylation and hydroboration reactions. For example, (terpy)Zn(O 2 CH) 2 achieves hydroboration of Me 2 CO and Ph 2 CO by HBpin to afford R 2 C(H)OBpin, and triple insertion of Ph 2 CO, PhC(O)Me, Me 2 CO and PhCHO into the Si–H bonds of PhSiH 3 to afford PhSi[OCH(R)R’] 3 . In addition, CO 2 also undergoes hydroboration and hydrosilylation by HBpin and (MeO) 3 SiH in the presence of (terpy)Zn(O 2 CH) 2 to afford HCO 2 Bpin and HCO 2 Si(OMe) 3 , respectively.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2016

Synthesis, Structure, Characterization, and Decomposition of Nickel Dithiocarbamates: Effect of Precursor Structure and Processing Conditions on Solid-State Products

Single-crystal X-ray structures of four nickel dithiocarbamate complexes, the homoleptic mixed-organic bis-dithiocarbamates Ni[S2CN(isopropyl)(benzyl)]2, Ni[S2CN(ethyl)(n-butyl)]2, and Ni[S2CN(phenyl)(benzyl)]2, as well as the heteroleptic mixed-ligand complex NiCl[P(phenyl)3][(S2CN(phenyl)(benzyl)], were determined. Synthetic, spectroscopic, structural, thermal, and sulfide materials studies are discussed in light of prior literature. The spectroscopic results are routine. A slightly distorted square-planar nickel coordination environment was observed for all four complexes. The organic residues adopt conformations to minimize steric interactions. Steric effects also may determine puckering, if any, about the nickel and nitrogen atoms, both of which are planar or nearly so. A trans-influence affects the Ni-S bond distances. Nitrogen atoms interact with the CS2 carbons with a bond order of about 1.5, and the other substituents on nitrogen display transoid conformations. There are no strong intermolecular interactions, consistent with prior observations of the volatility of nickel dithiocarbamate complexes. Thermogravimetric analysis of the homoleptic species under inert atmosphere is consistent with production of 1:1 nickel sulfide phases. Thermolysis of nickel dithiocarbamates under flowing nitrogen produced hexagonal or -NiS as the major phase; thermolysis under flowing forming gas produced millerite (-NiS) at 300 C, godlevskite (Ni9S8) at 325 and 350 C, and heazlewoodite (Ni3S2) at 400 and 450 C. Failure to exclude oxygen results in production of nickel oxide. Nickel sulfide phases produced seem to be primarily influenced by processing conditions, in agreement with prior literature. Nickel dithiocarbamate complexes demonstrate significant promise to serve as single-source precursors to nickel sulfides, a quite interesting family of materials with numerous potential applications.

microscopy↗
DOE OSTI2024

Structural Characterization of Deployed Thermoplastic and Thermoset Composite Tidal Turbine Blades

The National Renewable Energy Laboratory worked with Verdant Power to manufacture, and characterize, novel thermoplastic composite blades on their Gen5d 5 m diameter turbines at the Roosevelt Island Tidal Energy (RITE) site in the East River in N.Y. to demonstrate a low-cost manufacturing process for marine energy structures. Verdant had designed, manufactured, and deployed epoxy thermoset composite blades on three Gen5d turbines in October 2020. At a maintenance cycle in May 2021, a Gen5d turbine equipped with the NREL thermoplastic blades was deployed and retrieved in October 2021. Modal, static and fatigue structural characterization was performed on both blade types before and after the deployment. The static and modal test results showed that the thermoplastic blades were slightly stiffer than the epoxy blades both dry and after the deployment. The epoxy blades had about 8% increase in strain at the applied load after the deployment, whereas the thermoplastic blade strains were not changed significantly. Ultimately the thermoplastic blade failed during fatigue testing due to a crack which is thought to have initiated between the internal foam and the laminate at the location of the internal instrumentation. The Verdant Power Gen5d epoxy blades did not have this internal instrumentation and did not have this failure, performing adequately through the operational period. A lack of design information and fatigue data for both the thermoplastic laminates and the adhesive used means that further work is needed to fully understand his failure and the root cause analysis is ongoing. This paper provides details on the thermoplastic blade manufacturing, materials, test methodology and results.

17 WIND ENERGY↗
DOE OSTI2025

Molecular and structural characterization of a Bacillus cereus strain producing an anthrax-like capsule

Bacillus cereus is a ubiquitous Gram-positive, spore-forming, rod-shaped saprophytic bacterium, occasionally reported to cause food-borne illnesses. However, instances of B. cereus strains harboring anthrax toxin and capsule genes have elevated certain strains as formidable pathogens and biothreats. This study focuses on the genomic analysis and the structural characterization of capsular material produced by the virulent B. cereus PATH2418 strain, isolated from the wound of a traumatic open fracture patient. The genome was sequenced using Nanopore MinION sequencing, revealing a chromosome of 5,270,283 bp and three plasmids. One plasmid, pATH1, was found to encode an operon for the biosynthesis of a bacterial capsule. This operon had sequence homology to the Bacillus anthracis capBCADE operon, which encodes the poly-γ-D-glutamate (PDGA) capsule. The capsule production in B. cereus PATH2418 was influenced by temperature and CO 2 levels. Structural analysis of the capsular material using a combined approach of nuclear magnetic resonance (NMR) and high-performance liquid chromatography (HPLC) techniques confirmed the presence of a high-molecular-weight poly-γ-glutamate capsule, with an enantiomeric composition of approximately 67% D-glutamic acid and 33% L-glutamic acid, matching that of B. anthracis.

Bacillus cereus↗
DOE OSTI2024

Structural characterization of strawberry pomace

Strawberries are a nutrient dense food rich in vitamins, minerals, non-nutrient antioxidant phenolics, and fibers. Strawberry fiber bioactive structures are not well characterized and limited information is available about the interaction between strawberry fiber and phenolics. Therefore, we analyzed commercial strawberry pomace in order to provide a detailed carbohydrate structural characterization, and to associate structures with functions. The pomace fraction, which remained after strawberry commercial juice extraction, contained mostly insoluble (49.1 % vs. 5.6 % soluble dietary fiber) dietary fiber, with pectin, xyloglucan, xylan, β-glucan and glucomannan polysaccharides; glucose, fructose, xylose, arabinose, galactose, fucose and galacturonic acid free carbohydrates; protein (15.6 %), fat (8.34 %), and pelargonidin 3-glucoside (562 μg/g). Oligosaccharides from fucogalacto-xyloglucan, methyl-esterified rhamnogalacturonan I with branched arabinogalacto-side chains, rhamnogalacturonan II, homogalacturonan and β-glucan were detected by MALDI-TOF MS, NMR and glycosyl-linkage analysis. Previous reports suggest that these oligosaccharide and polysaccharide structures have prebiotic, bacterial pathogen anti-adhesion, and cholesterol-lowering activity, while anthocyanins are well-known antioxidants. A strawberry pomace microwave acid-extracted (10 min, 80 °C) fraction had high molar mass (2376 kDa) and viscosity (3.75 dL/g), with an extended rod shape. A random coil shape, that was reported previously to bind to phenolic compounds, was observed for other strawberry microwave-extracted fractions. These strawberry fiber structural details suggest that they can thicken foods, while the polysaccharide and polyphenol interaction indicates great potential as a multiple-function bioactive food ingredient important for gut and metabolic health.

59 BASIC BIOLOGICAL SCIENCES↗