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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 271 records · Page 15
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Membrane Adsorbents Comprising Self-Assembled Inorganic Nanocages (SINCs) for Super-fast Direct Air Capture Enabled by Passive Cooling

The objectives of the proposed project were to develop highly porous membrane adsorbents comprising CO 2 -philic polymers and self-assembled inorganic nanocages (SINCs) for rapid temperature swing adsorption using electricity-free solar heating and radiative cooling, enabling an economically viable approach for direct air capture (DAC). Our core technical activities combine three key innovations. (1) Highly porous flat-sheet membrane adsorbents contain CO 2 -philic amines that can be easily produced using a phase inversion method. (2) CO 2 -philic SINCs can be easily dispersed in the polymers with great stability (compared with the metal-organic frameworks or MOFs). (3) The adsorption and desorption are integrated with solar heating and radiative cooling for rapid continuous operation, in contrast to traditional long-cycle separate operation. The membrane adsorbents containing amines, polymers, and SINCs were produced using a one-step industrial process. The porous membranes coupled with porous SINCs offer low resistance for gas flow and fast CO 2 sorption/desorption cycles, while the incorporation of the additional amine groups provides high CO 2 sorption capacity. The key achievements are summarized below. (1) Membrane adsorbents with high PEI loading (>40%), high porosity of >80%, and low gasflow resistance were prepared in one step using commercially available, low-cost materials. (2) Membrane adsorbents based on Solupor and PEI show CO 2 sorption capacity of >1.5 mmol/g using air containing 400 ppm at a relative humidity of 15%. (3) Effect of the adsorbent compositions (such as PEI type, PEI content, SINC content, porosity) on the CO 2 sorption was systematically investigated. (4) Effect of the processing conditions (such as CO 2 content, temperature, and relative humidity) on the CO 2 sorption was systematically investigated; (5) The stability of the membrane adsorption against many cycles of sorption and desorption was studied. The higher molecular weight of PEI (PEI25k) shows better stability than PEI800. (6) Advanced materials with radiative cooling were developed, which can decrease the temperature by 5-7 °C compared to the ambient temperature. (7) Preliminary techno-economic analysis shows that our process may achieve a capture cost of $1,343/tonne CO 2 with a total OPEX cost of $1,112/tonne CO 2 . The adsorbent replacement cost accounted for 52% of the total OPEX cost. Membrane adsorbents with lower costs and longer operation life can significantly decrease the cost. The proposed project directly addresses the requirement of DE-FOA-0002188, i.e., novel materials with CO 2 adsorption capacity for direct air capture with integrated solar heating and radiative cooling to reduce the cost of the DAC. Our future work will focus on the development of low-cost adsorbents that can be stable at the sorption and desorption conditions for long term.

14 SOLAR ENERGY↗
DOE OSTI2024

Bench-Scale Development of a Novel Direct Air Capture Technology Using High-Capacity Structured Sorbents

The work performed under this project has resulted into development of a DAC technology utilizing a structured sorbent to capture CO 2 from ambient air with a key innovation of direct Joule heating of the sorbent for CO 2 desorption. A working SMA, fully integrated with an electrically resistive heating layer, high surface area support, and high CO 2 capacity sorbent coated onto a commercial ceramic monolithic substrate, was successfully developed and demonstrated over >200 adsorption-desorption cycles in a high-fidelity bench test unit directly using ambient air. A cordierite-based monolith was selected as a substrate owing to its high surface area, low bulk density, low heat capacity, and commercial availability. Reaction kinetics study conducted during this project led to development of a promoter for the base Na 2 CO 3 sorbent that could be incorporated into the sorbent to enhance to achieve higher CO 2 adsorption/desorption rates, greater working capacity, and reduced regeneration temperature. An accelerated aging study was conducted in a TGA to determine sorbent stability and no degradation in the sorbent performance was observed even after 250 adsorption-desorption cycles. An electrically resistive heating layer was developed with tunable electrical properties. The heating layer was coated onto the selected cordierite substrate. Aging studies performed showed the electrical properties and heating performance was stable after 500 heating and cooling cycles. The collective findings on the selected cordierite substrate, robust heating layer, promoter and sorbent selection were used to synthesize a full, 6”x6” SMA for bench-scale testing. The bench-scale DAC system was constructed to test full size SMAs using real ambient air for adsorption and joule heating for regeneration. After completing shakedown and commissioning of the 1 kg/day of CO 2 capacity DAC bench unit, an extended operation was performed to complete over 230 cycles with the full size SMA. This testing showed no observable degradation in sorbent performance. A detailed process model, TEA and LCA were developed for a conceptual 100,000 TPY CO 2 removal DAC facility. The LCA results show the net CO 2 e emissions from the DAC system are highly dependent on the electricity source. All other factors, including SMA manufacturing, materials for facility enclosure, etc., are minor cost contributors compared to the energy consumption required for CO 2 removal. With the successful development and validation of the SMA for the sustained performance for CO 2 removal from ambient air with joule heated regeneration in this project, a fully integrated 1 TPY bench-scale DAC system is currently in development with the support of DOE/FECM (DE-FE0032243). The project objective is to demonstrate the engineering design of the DAC system to produce a continuous, high purity CO 2 stream from ambient air. This project will address and validate key engineering features of the DAC system including the gas sealing mechanism and panels, enclosure and air contactor design, and automation sequence to achieve continuous CO 2 production.

42 ENGINEERING↗
DOE OSTI2024

Ultrafast Surface Phosphor Thermometry for Pulsed-power and Hostile Environments

Modern concepts for next generation pulsed power (NGPP) are slated to deliver up to ten times the energy of Z today. An increase of this magnitude is concerning insofar that Z currently exhibits sizable amounts of inner magnetically insulated transmission line (MITL) loss current on the order of 5-10%. Loss phenomenon in these systems are complex and electrode heating and subsequent thermal desorption are a leading cause. Rapid heat-driven thermal desorption of contaminants scales as the square of the current. Therefore, even a modest doubling of drive current would yield an ~ 4X in non-linear surface electrode heating, quickening thermal desorption-based current loss. Exacerbating these physics is a current inability to measure ultra fast heating rates (>20°C/ns), which are paramount to benchmarking and code validation critical to NGPP design – as an empirical approach is not viable. Therefore, Ultrafast Photoluminescent Surface Heating Optical Thermometry (UP-SHOT) was developed as a new diagnostic for measurement of GHz-scale electrode heating. The discovery of UP-SHOT leveraged expertise in Engineering Science, Material Science, Pulsed-Power, and the Center for Integrated Nanotechnologies. This report includes information on: 1) The preparation of zinc oxide (ZnO) films, characterization, post-deposition treatments 2) Time-resolved photoluminescence at elevated temperatures and thermographic sensitivity

36 MATERIALS SCIENCE↗
DOE OSTI2024

Preparation and Characterization of Materials for Low- to Intermediate-Temperature CO2 Adsorption

Global carbon dioxide emissions are rising and the use of fossil fuels in several sectors are the leading causes. As global population and economies continue to grow significantly, the most practical method of lowering such emissions is to capture CO2. Although other technologies are more developed, adsorption is very promising and has attracted much attention. To ensure this technology’s success, it is essential to have suitable CO2 adsorbent materials. In this work, several new hydrotalcites (HTs) with different initial concentrations of ion precursors were prepared for the first time by the co-precipitation method—it was possible to verify that the ion concentrations influence the characteristics of the materials. The prepared HTs were characterized by thermogravimetric analysis (TG), X-Ray diffraction (XRD), surface area measurements and temperature-programmed desorption of CO2 (TPD-CO2) to relate their CO2 capture capacity to their physicochemical properties; the CO2 adsorption equilibrium isotherms were determined at 35 and 300 °C for the prepared samples, as well as for some commercial materials: magnesium oxide, calcium oxide, aluminium oxide and Zeolite 13X. After determining which materials present the best CO2 adsorption capacity, these were submitted to adsorption-desorption cycles to study their stability. The main objective of the work was to prepare and study different CO2 adsorbents for processes that are carried out at low and intermediate temperatures. From the experimental results, it was possible to conclude that the Zeolite 13X showed the best capacity at 35 °C, 3.38 mmol·g−1 (@ pCO2 = 1 bar), and a prepared calcined HT (c-HT2) was the best at 300 °C, 0.97 mmol·g−1 (@ pCO2 = 1 bar). Moreover, it seems there is an optimum initial concentration of the ions’ solutions for the tested HTs, which depends on the final application—c-HT1 showed a better capacity at 35 °C and c-HT2 at 300 °C. From the adsorption-desorption cycles—performed at 35 and 300 °C with the best materials using a magnetic suspension microbalance at 1 bar of CO2 partial pressure —, a working cyclic capacity of 2.69 mmol∙g−1 was achieved by the Zeolite at 35 °C; in turn, c-HT2 showed a working cyclic capacity of 0.79 mmol∙g−1 at 300 °C.

Figueiredo, Anabela↗
DOE OSTI2025

Fiber-Coupled Multipass NIR Sensor for In Situ, Real-Time Water Vapor Outgassing Monitoring

This work presents the recent development of a fiber-coupled multipass near-infrared (NIR) gas sensor used to monitor water vapor desorption of small material coupons. The gas sensor design employs a White cell topology to maximize the optical path length over a compact, hand-size footprint. Water vapor concentrations are quantified over a large dynamic range by simultaneously applying wavelength modulation and tunable diode laser absorption spectroscopy techniques. A custom headspace optimized for material desorption experiments is assembled using commercially available vacuum chamber components. We provide in situ measurements of water vapor desorption from two geometries of the industrially important silicone elastomer Sylgard-184 as a case study for sensor viability. To corroborate the results, the gas sensor data are compared to numerical simulations based on a triple-mode diffusion–sorption model, consisting of Henry, Langmuir, and Pooling modes.

gas sensor↗
NASA NTRS1972

Physical electronics and surface physics

Current analytical and experimental investigations of the influence of surface processes on the rate of permeation of gases through solids are summarized. A brief description is presented of an analytical model that provides an approximate prediction of the dependence of the permeation rate on the rates of surface processes relative to the rate of the diffusion process. Results of experiments indicate that the desorption process of hydrogen from various materials is influenced by surface impurities to the degree that substantial changes in the spatial distribution of the desorbed molecules are observed when the impurities are varied. Except possibly for H-Nb, the permeation measurements indicate that the desorption process is not influenced to the degree that detectable changes in the permeation rates are observed when the impurities and temperatures are varied. On the basis of analysis, it is unlikely that the desorption process will be the rate-controlling step under the conditions of the present experiments.

Stickney, R. E.↗
NASA NTRS1977

The development and testing of a regenerable CO2 and humidity control system for Shuttle

A regenerable CO2 and humidity control system is presently being developed for potential use on Shuttle as an alternate to the baseline lithium hydroxide (LiOH) system. The system utilizes a sorbent material (designated 'HS-C') to adsorb CO2 and water vapor from the cabin atmosphere and desorb the CO2 and water vapor overboard when exposed to a space vacuum. Continuous operation is achieved by utilizing two beds which are alternately cycled between adsorption and desorption. This paper presents the significant hardware development and test accomplishments of the past year. A half-size breadboard system utilizing a flight configuration canister was successfully performance tested in simulated Shuttle missions. A vacuum desorption test provided considerable insight into the desorption phenomena and allowed a significant reduction of the Shuttle vacuum duct size. The fabrication and testing of a flight prototype canister and flight prototype vacuum valves have proven the feasibility of these full-size, flight-weight components.

Boehm, A. M.↗
NASA NTRS1982

Chemisorption of CO on particulate deposits of platinum

Morphology and CO chemisorption properties are studied as a function of particle size for the case of particulate Pt films, vapor-deposited onto ultrahigh vacuum-cleaved and heat-treated mica surfaces at a 200 C substrate temperature. The particles were found to be mostly irregular in shape and randomly-oriented, with two desorption peaks after CO absorption at 60 C: (1) an alpha peak, at 120 C, attributed to smooth particle surfaces, and (2) a beta peak, at about 175 C, attributed to particle edges and steps. Transmission electron microscopy showed that major changes occur in particle morphology during absorption-desorption cycling, so that the decrease in CO desorption flux may be interpreted as due to particle restructuring, rather than contamination by CO decomposition as in the cases of Ni or Pd on mica. Auger electron spectroscopy corroborates the lack of CO decomposition, even for the case of very small Pt particles.

Doering, D. L.↗
NASA NTRS1987

The role of electronic mechanisms in surface erosion and glow phenomena

Experimental studies of desorption induced by electronic transitions (DIET) are described. Such studies are producing an increasingly complete picture of the dynamical pathways through which incident electronic energy is absorbed and rechanneled to produce macroscopic erosion and glow. These mechanistic studies can determine rate constants for erosion and glow processes in model materials and provide valuable guidance in materials selection and development. Extensive experiments with electron, photon, and heavy particle irradiation of alkali halides and other simple model materials have produced evidence showing that: (1) surface erosion, consisting primarily in the ejection or desorption of ground-state neutral atoms, occurs with large efficiencies for all irradiated species; (2) surface glow, resulting from the radiative decay of desorbed atoms, likewise occurs for all irradiating species; (3) the typical mechanism for ground-state neutral desorption is exciton formation, followed by relaxation to a permanent, mobile electronic defect which is the precursor to bond-breaking in the surface or near-surface bulk of the material; and (4) the mechanisms for excited atom formation may include curve crossing in atomic collisions, interactions with surface defect or impurity states, or defect diffusion.

Haglund, Richard F., Jr.↗
NASA NTRS1994

Real refractive indices of infrared-characterized nitric-acid/ice films: Implications for optical measurements of polar stratospheric clouds

The infrared spectra of nitric-acid/ice films representative of polar stratospheric clouds (PSCs) were collected with simultaneous optical interference measurements to determine the real refractive indices at lambda = 632 nm. Ice and amphorous nitric-acid/ice films were prepared by condensation of water and nitric acid vapors onto a wedged Al2O3 substrate. The real refractive indices of these films were determined from the optical interference of a reflected helium-neon laser during film growth. The indices of the amphorous films varied smoothly from n = 1.30 for ice to n = 1.49 for nitric acid, similar to observations in previous work. We were unable to obtain the refractive index of crystlline films during adsorption because of optical scattering caused by surface roughness. Therefore crystlline nitric acid hydrate films were prepared by annealing amphorous nitric-acid/ice films. Further heating caused desorption of the crystalline hydrate films. During desorption, the refractive indices for ice, NAM (nitric acid monohydrate), alpha- and beta-NAT (nitric acid trihydrate) films were measured using the optical interference technique. In agreement with earlier data, the real refractive indices for ice and NAM determined in desorption were n = 1.30 +/- 0.01 and n = 1.53 +/- 0.03, respectively. The real refractive indices for alpha- and beta-NAT were found to be n = 1.51 +/- 0.01 and n greater than or equal to 1.46, respectively. Our measurements also suggest that the shape of crystalline nitric acid particles may depend on whether they nucleate from the liquid or by vapor deposition. If confirmed by future studies, this observation may provide a means of distinguishing the nucleation mechanism of crystalline PSCs.

Middlebrook, Ann M.↗
NASA NTRS2001

Chemical and Isotopic Analysis of Trace Organic Matter on Meteorites and Interstellar Dust Using a Laser Microprobe Instrument

Polycyclic Aromatic Hydrocarbons (PAHs) are of considerable interest today because they are ubiquitous on Earth and in the interstellar medium (ISM). In fact, about 20% of cosmic carbon in the galaxy is estimated to be in the form of PAHs. Investigation of these species has obvious uses for determining the cosmochemistry of the solar system. Work in this laboratory has focused on four main areas: 1) Mapping the spatial distribution of PAHs in a variety of meteoritic samples and comparing this distribution with mineralogical features of the meteorite to determine whether a correlation exists between the two. 2) Developing a method for detection of fullerenes in extraterrestrial samples using microprobe Laser Desorption Ionization Mass Spectroscopy and utilizing this technique to investigate fullerene presence, while exploring the possibility of spatially mapping the fullerene distribution in these samples through in situ detection. 3) Investigating a possible formation pathway for meteoritic and ancient terrestrial kerogen involving the photochemical reactions of PAHs with alkanes under prebiotic and astrophysically relevant conditions. 4) Studying reaction pathways and identifying the photoproducts generated during the photochemical evolution of PAH-containing interstellar ice analogs as part of an ongoing collaboration with researchers at the Astrochemistry Lab at NASA Ames. All areas involve elucidation of the solar system formation and chemistry using microprobe Laser Desorption Laser Ionization Mass Spectrometry. A brief description of microprobe Laser Desorption Ionization Mass Spectroscopy, which allows selective investigation of subattomole levels of organic species on the surface of a sample at 10-40 micrometer spatial resolution, is given.

Zare, Richard N.↗
NASA NTRS2005

Spool Valve for Switching Air Flows Between Two Beds

U.S. Patent 6,142,151 describes a dual-bed ventilation system for a space suit, with emphasis on a multiport spool valve that switches air flows between two chemical beds that adsorb carbon dioxide and water vapor. The valve is used to alternately make the air flow through one bed while exposing the other bed to the outer-space environment to regenerate that bed through vacuum desorption of CO2 and H2O. Oxygen flowing from a supply tank is routed through a pair of periodically switched solenoid valves to drive the spool valve in a reciprocating motion. The spool valve equalizes the pressures of air in the beds and the volumes of air flowing into and out of the beds during the alternations between the adsorption and desorption phases, in such a manner that the volume of air that must be vented to outer space is half of what it would be in the absence of pressure equalization. Oxygen that has been used to actuate the spool valve in its reciprocating motion is released into the ventilation loop to replenish air lost to vacuum during the previous desorption phase of the operating cycle.

Dean, W. Clark↗
NASA NTRS2014

Cold Water Vapor in the Barnard 5 Molecular Cloud

After more than 30 yr of investigations, the nature of gas-grain interactions at low temperatures remains an unresolved issue in astrochemistry. Water ice is the dominant ice found in cold molecular clouds; however, there is only one region where cold ((is) approximately 10 K) water vapor has been detected-L1544. This study aims to shed light on ice desorption mechanisms under cold cloud conditions by expanding the sample. The clumpy distribution of methanol in dark clouds testifies to transient desorption processes at work-likely to also disrupt water ice mantles. Therefore, the Herschel HIFI instrument was used to search for cold water in a small sample of prominent methanol emission peaks. We report detections of the ground-state transition of o-H2O (J = 110-101) at 556.9360 GHz toward two positions in the cold molecular cloud, Barnard 5. The relative abundances of methanol and water gas support a desorption mechanism which disrupts the outer ice mantle layers, rather than causing complete mantle removal.

ISM: molecules↗
DOE OSTI2020

Method and system for treatment of a gas stream that contains carbon dioxide

A method for separating carbon dioxide (CO2) from a gas stream is disclosed, in which the gas stream is reacted with a lean aminosilicone solvent in an absorber, resulting in a rich aminosilicone solvent that is then treated in a desorber to release the CO2 and regenerate lean aminosilicone solvent in a desorption reaction. The regenerated solvent is directed into a steam-producing, indirect heat exchanger that is configured to supply steam to the desorber at a temperature high enough to augment the desorption reaction. Also, selected amounts of make-up water are added to the rich aminosilicone solvent at one or more process locations between the absorber and the desorber, to lower the viscosity of the solvent and to lower the temperature required for the desorption reaction.

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

Atomic Layer Deposition for Materials-Based H2 Storage: Opportunities and Limitations

The transportation demands in our growing hydrogen (H2) economy requires robust storage systems. The current commercially implemented technology in fuel cell cars relies on the well-established technology of hydrogen gas compressed to 350-700 bar, depending on the application. The compressed gas tanks in use today are bulky and cost intensive. To address this challenge, material-based storage is one of the long-term alternatives considered and constitutes the focus of this talk. Material-based storage is broadly defined as hydrogen bound to solid materials, with its binding strength varying from physisorption to porous materials, such as zeolites and metal organic frameworks, to chemisorption in (complex) metal hydrides. The ultimate targets set by the U.S. Department of Energy for this technology include a system gravimetric capacity of 6.5 wt% and volumetric capacity of 40 g/L at 100 bar, operating temperatures ranging between -40 C and +40 C and adsorption/desorption timescales of < 5 min. Storage in the form of physisorbed or chemisorbed hydrogen has guided the materials research, which metal- organic framework and (complex) metal hydrides being the most promising materials classes. A variety of these materials have met one or more of the targets, but it has remained elusive for a single material system to meet all these stringent requirements. Nano-encapsulation and low-concentration chemical additives have previously been employed separately to overcome such challenges. Functionalization via atomic layer deposition (ALD), however, offers unique characteristics that make it suitable for both, nano-encapsulation and "doping" with low-concentration additives. This deposition technique has sub-monolayer thickness control, is highly conformal in high-surface area materials and is self-limiting, i.e., once the gas-phase precursor reacts with the available surface sites, the surface reactions stop. In this presentation, we will showcase examples where ALD, more generally vapor-phase functionalization, on (complex) metal hydrides and organic frameworks has improved the material properties for H2 storage. In our first study, Al2O3 was deposited on magnesium borohydride, Mg(BH4)2, at room temperature using trimethylaluminum (TMA) and water. From our findings, encouraging initial results were obtained: the H2 desorption temperature was lowered by 60-120 degrees C, the desorbed gravimetric H2 capacity at temperatures < 250 degrees C was doubled, and the desorption kinetics increased by a factor of ~6 compared to uncoated Mg(BH4)2. However, hydrolysis reactions caused by residual surface -OH groups from the ALD water-pulse degraded the sample substantially. Through this study, the use of TMA was observed to be highly reactive with the Mg(BH4)2 surface species, leading to the strategy of exposing the sample only to TMA. The relative mole fraction of the vapor-phase additive can be precisely controlled with the number of TMA pulses and pulse duration. By tuning these parameters, we show in our second study that 10 pulses of TMA at ambient conditions were able to decrease the H2 desorption temperature by ~100 degrees C while retaining <95 % of its H2 capacity. We applied this approach with other additives such as BBr3, TiCl4 and tetrahydrofuran, and demonstrate that this unique approach opens the door to a new class of molecular additives and catalysts which cannot easily be introduced with conventional mechano-chemical or solvent-based techniques for (complex) metal-hydrides. In the case of metal organic frameworks, ALD is a promising technique to functionalize the pores with metal atoms or functional groups able to tune the gas selectivity and binding energy, for which ~15 kJ/mol has been established as the optimal value for H2 storage in sorbent materials. Vapor-phase techniques such as ALD have numerous benefits over other functionalization tools for H2 storage materials opening innumerable opportunities to the field. To exploit these opportunities, the current limitations on room temperature and water-less ALD processes needs to be overcome which will greatly expand the possibilities of encapsulation and incorporation of additives for organic frameworks and (complex) metal hydrides.

atomic layer deposition↗
DOE OSTI2022

Electrochemical pumping: An alternative solution for hydrogen embrittlement

Hydrogen embrittlement is a form of chemo-mechanical damage that is special in that it can be partially reversible. Here, in this paper, we propose a method for recovering structural alloys from hydrogen embrittlement at room temperature by electrochemically biased desorption of hydrogen. We demonstrate that the method can enable the reversion of hydrogen-induced degradation of mechanical properties, by comparing the mechanical behavior of commercial stainless steel specimens at different hydrogen charging and desorption states. These case studies also reveal the influence of electrochemical potential, H content and the characteristics of H trapping sites, on the effectiveness of this recovery approach. The limitations arising from the presence of unhealable forms of hydrogen damage, and the generic applicability of this electrochemically-assisted recovery method are also discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Ettringite hysteresis under sorption from molecular simulations

Highlights: • Hybrid Grand Canonical Monte Carlo (GCMC) and Molecular Dynamics (MD) simulations are performed. • Anisotropic large strain coefficient of crystal shrinkage of ettringite is provided. • Entropy increases when ettringite converts into metaettringite. • Sorption-induced stress may lead to columns collapse upon drying. • H-bonds involving OH groups in columns play a role in hysteresis. The response of ettringite under sorption is critical for the utilization of this mineral as an energy storage material and to understand the concrete durability problems associated with ettringite formation. We report molecular simulations directly sampling the osmotic ensemble to understand the sorption processes and structural changes in ettringite-metaettringite transition. Desorption branch and sorption-induced volume changes from simulations agree with the experiments. The structural changes at low relative humidity are analyzed, revealing for the first time details of metaettringite structure. The reversibility under sorption observed experimentally is captured by simulation in the ettringite domain. The reversibility in the conversion of metaettringite into ettringite is not captured by the direct simulations in the osmotic ensemble due to the large volume changes associated with ettringite desorption. Finally, we discuss the role of hydrogen bonds on the hysteresis in ettringite.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Experimental Assessment of Mammalian Lipidome Complexity Using Multimodal 21 T FTICR Mass Spectrometry Imaging

Herein, we assess the complementarity and complexity of data that can be detected within mammalian lipidome mass spectrometry imaging (MSI) via matrix-assisted laser desorption ionization (MALDI) and nanospray desorption electrospray ionization (nano-DESI). We do so by employing 21 T Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS) with absorption mode FT processing in both cases, allowing unmatched mass resolving power per unit time (≥613k at m/z 760, 1.536 s transients). While our results demonstrated that molecular coverage and dynamic range capabilities were greater in MALDI analysis, nano-DESI provided superior mass error, and all annotations for both modes had sub-ppm error. Taken together, these experiments highlight the coverage of 1676 lipids and serve as a functional guide for expected lipidome complexity within nano-DESI-MSI and MALDI-MSI. To further assess the lipidome complexity, mass splits (i.e., the difference in mass between neighboring peaks) within single pixels were collated across all pixels from each respective MSI experiment. The spatial localization of these mass splits was powerful in informing whether the observed mass splits were biological or artificial (e.g., matrix related). Mass splits down to 2.4 mDa were observed (i.e., sodium adduct ambiguity) in each experiment, and both modalities highlighted comparable degrees of lipidome complexity. Further, we highlight the persistence of certain mass splits (e.g., 8.9 mDa; double bond ambiguity) independent of ionization biases. Here, we also evaluate the need for ultrahigh mass resolving power for mass splits ≤4.6 mDa (potassium adduct ambiguity) at m/z > 1000, which may only be resolved by advanced FTICR-MS instrumentation.

21T-FTICR-MS↗