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DOE OSTI2022

Estimating the energy requirement for hydrogen production in proton exchange membrane electrolysis cells using rapid operando hydrogen crossover analysis

Hydrogen (H 2 ) crossover in proton exchange membrane water electrolyzers refers to the process by which hydrogen produced at the cathode traverses the membrane and mixes with the oxygen produced at the anode. This phenomenon reduces efficiency and may pose flammability hazards. In this work we present a method for quantifying the H 2 content of the anode exhaust gas using a gas chromatograph that is capable of sampling data every 2 min. Subsequent theory is presented to calculate the crossover flux, overall H 2 efficiency, and H 2 energy requirements. Results the effects of membrane thickness using Nafion TM N117 (178 um) and Nafion TM NR212 (51 um) membranes. Furthermore, it was found that thinner membranes lead to improved VI performance but exhibit higher crossover rates. Despite their increased crossover, leading to decreased hydrogen efficiency, the calculated required energy for NR212 membrane-electrode assemblies (MEAs) was significantly lower than that of N117 MEAs.

08 HYDROGEN↗

NASA NTRS1974

Computer programs for pressurization (RAMP) and pressurized expulsion from a cryogenic liquid propellant tank

An analysis to predict the pressurant gas requirements for the discharge of cryogenic liquid propellants from storage tanks is presented, along with an algorithm and two computer programs. One program deals with the pressurization (ramp) phase of bringing the propellant tank up to its operating pressure. The method of analysis involves a numerical solution of the temperature and velocity functions for the tank ullage at a discrete set of points in time and space. The input requirements of the program are the initial ullage conditions, the initial temperature and pressure of the pressurant gas, and the time for the expulsion or the ramp. Computations are performed which determine the heat transfer between the ullage gas and the tank wall. Heat transfer to the liquid interface and to the hardware components may be included in the analysis. The program output includes predictions of mass of pressurant required, total energy transfer, and wall and ullage temperatures. The analysis, the algorithm, a complete description of input and output, and the FORTRAN 4 program listings are presented. Sample cases are included to illustrate use of the programs.

Masters, P. A.↗

NASA NTRS1975

Gas chromatograph injection system

An injection system for a gas chromatograph is described which uses a small injector chamber (available in various configurations). The sample is placed in the chamber while the chamber is not under pressure and is not heated, and there is no chance of leakage caused by either pressure or heat. It is injected into the apparatus by changing the position of a valve and heating the chamber, and is volatilized and swept by a carrier gas into the analysis apparatus.

Pollock, G. E.↗

NASA NTRS1985

Aluminum oxide barriers in MCrAlY superalloy systems

An investigation was made of sputtered aluminum oxide diffusion barriers to protect gas turbine engine blade and vane alloys from their coatings. MAR M200 + Hf coated with sputtered NiCoCrAlY and MAR M509 coated with sputtered FeCrAlY were obtained both with and without 1 and 2 micron sputtered Al2O3 barrier layers. Electron dispersive X-ray analysis was used to determine the concentration profiles of as-received and heat treated samples.

Kreider, Kenneth G.↗

NASA NTRS2012

Gas Composition Sensing Using Carbon Nanotube Arrays

This innovation is a lightweight, small sensor for inert gases that consumes a relatively small amount of power and provides measurements that are as accurate as conventional approaches. The sensing approach is based on generating an electrical discharge and measuring the specific gas breakdown voltage associated with each gas present in a sample. An array of carbon nanotubes (CNTs) in a substrate is connected to a variable-pulse voltage source. The CNT tips are spaced appropriately from the second electrode maintained at a constant voltage. A sequence of voltage pulses is applied and a pulse discharge breakdown threshold voltage is estimated for one or more gas components, from an analysis of the current-voltage characteristics. Each estimated pulse discharge breakdown threshold voltage is compared with known threshold voltages for candidate gas components to estimate whether at least one candidate gas component is present in the gas. The procedure can be repeated at higher pulse voltages to estimate a pulse discharge breakdown threshold voltage for a second component present in the gas. The CNTs in the gas sensor have a sharp (low radius of curvature) tip; they are preferably multi-wall carbon nanotubes (MWCNTs) or carbon nanofibers (CNFs), to generate high-strength electrical fields adjacent to the tips for breakdown of the gas components with lower voltage application and generation of high current. The sensor system can provide a high-sensitivity, low-power-consumption tool that is very specific for identification of one or more gas components. The sensor can be multiplexed to measure current from multiple CNT arrays for simultaneous detection of several gas components.

Li, Jing↗

NASA NTRSDate not supplied

Challenges of Building, Launching, and Operating The Curiosity SAM Instrument on Mars

The Sample Analysis at Mars (SAM) Suite Investigation onboard the Mars Science Laboratory (MSL) Curiosity rover is currently roving up Mt Sharp in Gale Crater on Mars. It is investigating the present and past habitability of Mars by exploring molecular and elemental chemistry relevant to life. SAM is a suite of three instruments, a Quadrupole Mass Spectrometer (QMS), a Gas Chromatograph (GC), and a Tunable Laser Spectrometer (TLS). As Curiosity climbs Mt. Sharp, SAM’s instrument suite search for and measure the abundances of carbon, oxygen, hydrogen, and nitrogen - elements that are associated with life as we know it. SAM quantitatively addresses the habitability of Mars, an essential step in the search for past or present life on Mars. This talk provides a behind-the-scenes look at the vignettes of the engineering challenges of building, integrating, testing, launching, and the SAM’s team’s initial experiences of operating SAM on Mars.

Florence Tan↗

DOE OSTI2021

Practical considerations for amino acid isotope analysis

Over the last few decades, isotopic analysis of amino acids at the compound- and position-specific levels has been rapidly advancing across diverse fields. As these techniques progress, evaluation of isotopic fractionation associated with sample workup is essential. This critical review of analytical methods through the lens of isotope geochemistry provides a benchmark for researchers across disciplines seeking to make compound- and position-specific amino acid isotope measurements. We focus on preparation, acid hydrolysis, clean-up, derivatization, separation, and C, H, N, and S isotope measurement. Despite substantial customizability across these steps, the following general recommendations should maximize recovery while minimizing isotopic fractionation. Samples should be freeze-dried and stored anoxically at ≤ –20 °C prior to conventional acid hydrolysis (6N HCl, 110 °C, 20–24 h, anoxic), which suffices for many residues. Both gas and liquid chromatographic (GC and LC, respectively) techniques are well-established and separate about 15 amino acids; LC bypasses the need for derivatization, while GC provides higher sensitivity. Furthermore, when derivatization is needed, n-acetyl and alkoxycarbonyl esters provide the most reproducible C isotope ratios. For compound-specific analyses, online GC–IRMS and LC–IRMS systems offer the easiest workflow, but EA–IRMS enables potential multi-element isotope analysis. Emerging techniques like high-resolution mass spectrometry are also promising for multi-element analysis and recover position-specific isotopic information. Looking forward to the next decade of innovation, isotope geochemists and ecologists can improve amino acid isotope analysis by focusing on streamlining multi-element analysis and standardizing calibration practices across laboratories.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Determining the Effect of Catechins on SOD1 Conformation and Aggregation by Ion Mobility Mass Spectrometry Combined with Optical Spectroscopy

The aggregation of Cu,Zn-superoxide dismutase (SOD1) plays an important role in the etiology of amyotrophic lateral sclerosis (ALS). For the disruption of ALS progression, discovering new drugs or compounds that can prevent SOD1 aggregation is important. In this study, ESI-MS was used to investigate the interaction of catechins and SOD1. The noncovalent complex of catechins that interact with SOD1 was found and retained in the gas phase under native ESI-MS condition. The conformation changes of SOD1 after binding with catechins were also explored via traveling wave ion mobility (IM) spectrometry. Epigallocatechin gallate (EGCG) can stabilize SOD1 conformation against unfolding in three catechins. To further evaluate the efficacy of EGCG, we monitored the fluorescence changes of dimer E{sub 2},E{sub 2},-SOD1(apo-SOD1, E:empty) with and without ligands under denaturation conditions, and found that EGCG can inhibit apo-SOD1 aggregation. In addition, the circular dichroism spectra of the samples showed that EGCG can decrease the β-sheet content of SOD1, which can produce aggregates. These results indicated that orthogonal separation dimension in the gas-phase IM coupled with ESI-MS (ESI-IM-MS) can potentially provide insight into the interaction between SOD1 and small molecules. The advantage is that it dramatically decreases the analysis time. Meantime, optical spectroscopy techniques can be used to confirm ESI-IM-MS results. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2023

An Interactive Spectral Analysis Tool for Chemical Identification and Quantification of Gas-Phase Species in Complex Spectra

A spectral analysis tool has been developed to interactively identify and quantify individual gas-phase species from complex infrared absorbance spectra obtained from laboratory or field data. The SpecQuant program has an intuitive graphical interface that accommodates both reference and experimental data with varying resolution and instrumental lineshape, as well as algorithms to readily align the wavenumber axis of a sample spectrum with the raster of a reference spectrum. Using a classical least squares model in conjunction with reference spectra such as those from the Pacific Northwest National Laboratory (PNNL) gas-phase infrared database or simulated spectra derived from the HITRAN line-by-line database, the mixing ratio of each identified species is determined along with its associated estimation error. After correcting the wavelength and intensity of the field data, SpecQuant displays the calculated mixing ratio versus the experimental data for each analyte along with the residual spectrum with any or all analyte fits subtracted for visual inspection of the fit and residuals. The software performance for multianalyte quantification was demonstrated using moderate resolution (0.5 cm –1 ) infrared spectra that were collected during the time-resolved infrared photolysis of methyl iodide.

Thompson, Christopher J.↗

DOE OSTI2017

GASP. I. Gas Stripping Phenomena in Galaxies with MUSE

GAs Stripping Phenomena in galaxies with MUSE (GASP) is a new integral-field spectroscopic survey with MUSE at the VLT aimed at studying gas removal processes in galaxies. We present an overview of the survey and show a first example of a galaxy undergoing strong gas stripping. GASP is obtaining deep MUSE data for 114 galaxies at z = 0.04–0.07 with stellar masses in the range 10{sup 9.2}--10{sup 11.5} M{sub ⊙} in different environments (galaxy clusters and groups over more than four orders of magnitude in halo mass). GASP targets galaxies with optical signatures of unilateral debris or tails reminiscent of gas-stripping processes (“jellyfish galaxies”), as well as a control sample of disk galaxies with no morphological anomalies. GASP is the only existing integral field unit (IFU) survey covering both the main galaxy body and the outskirts and surroundings, where the IFU data can reveal the presence and origin of the outer gas. To demonstrate GASP’s ability to probe the physics of gas and stars, we show the complete analysis of a textbook case of a jellyfish galaxy, JO206. This is a massive galaxy (9×10{sup 10} M{sub ⊙}) in a low-mass cluster (σ∼500 km s{sup −1}) at a small projected clustercentric radius and a high relative velocity, with ≥90 kpc long tentacles of ionized gas stripped away by ram pressure. We present the spatially resolved kinematics and physical properties of the gas and stars and depict the evolutionary history of this galaxy.

79 ASTRONOMY AND ASTROPHYSICS↗

NASA NTRS1988

Reactions of silicon-based ceramics in mixed oxidation chlorination environments

The reaction of silicon-based ceramics with 2 percent Cl2/Ar and 1 percent Cl2/1 percent to 20 percent O2/Ar at 950 C was studied with thermogravimetric analysis and high-pressure mass spectrometry. Pure Si, SiO2, several types of SiC, and Si3N4 were examined. The primary corrosion products were SiCl4(g) and SiO2(s) with smaller amounts of volatile silicon oxychlorides. The reactions appear to occur by chlorine penetration of the SiO2 layer, and gas-phase diffusion of the silicon chlorides away from the sample appears to be rate limiting. Pure SiO2 shows very little reaction with Cl2, SiC with excess Si is more reactive than the other materials with Cl2, whereas SiC with excess carbon is more reactive than the other materials with Cl2/O2. Si3N4 shows very little reaction with Cl2. These differences are explained on the basis of thermodynamic and microstructural factors.

Marra, John E.↗

NASA NTRS2011

Understanding Geospace on a Grand Scale: The Global Ionoshphere/Thermosphere Constellation

We present the concept of a constellation of polar orbiting satellites equally spaced in longitude (local time) to systematically sample both the neutral and ionzed gas components of the Earth in circular orbits near 350 km, including their density, temperature, and velocities. The instrumentation would include techniques to measure the height of the ionospheric "F-peak" and its variations along the orbit. The number of satellites (l2? 24? 48?) and their configuration would be determined from modeling analysis and expected geophysical phenomena, including their drivers and characteristic time scales. Together with imaging data from separate satellites, the array of satellites with in situ probes would be expected to provide a new picture of (1) high latitude electrodynamics and atmospheric processes and associated coupling with magnetospheric mass and momentum input, (2) the response of the global ionosphere and thermosphere to magnetic storms, and (3) global neutral wind circulation patterns, neutral density structure, tides, planetary waves, and gravity waves. The comprehensive measurements gathered by the IT-Constellation envisioned here would provide a major leap forward in each of these areas, addressing global physical processes and providing fundamental, new knowledge of Geospace. In particular, by its very nature, the constellation addresses "system science", revealing how the ionosphere-thermosphere connects globally to the magnetosphere above and the troposphere below. We present this concept as the next logical step in observing the "whole" space environment using in situ probes in conjunction with imagers. We invite modelers to not only comment on this concept but also to become actively engaged in helping to define it.

Pfaff, Robert↗

NASA NTRS2009

Dynamic Measurement of Temperature, Velocity, and Density in Hot Jets Using Rayleigh Scattering

A molecular Rayleigh scattering technique is utilized to measure gas temperature, velocity, and density in unseeded gas flows at sampling rates up to 10 kHz, providing fluctuation information up to 5 kHz based on the Nyquist theorem. A high-power continuous-wave laser beam is focused at a point in an air flow field and Rayleigh scattered light is collected and fiber-optically transmitted to a Fabry-Perot interferometer for spectral analysis. Photomultiplier tubes operated in the photon counting mode allow high-frequency sampling of the total signal level and the circular interference pattern to provide dynamic density, temperature, and velocity measurements. Mean and root mean square velocity, temperature, and density, as well as power spectral density calculations, are presented for measurements in a hydrogen-combustor heated jet facility with a 50.8-mm diameter nozzle at NASA John H. Glenn Research Center at Lewis Field. The Rayleigh measurements are compared with particle image velocimetry data and computational fluid dynamics predictions. This technique is aimed at aeronautics research related to identifying noise sources in free jets, as well as applications in supersonic and hypersonic flows where measurement of flow properties, including mass flux, is required in the presence of shocks and ionization occurrence.

Mielke, Amy F.↗

DOE OSTI2020

Geochemical Changes in Response to CO 2 Injection in a CO 2 -EOR Complex in Northern Michigan

The overall purpose of the geochemical monitoring program under Midwestern Regional Carbon Sequestration Partnership (MRCSP) is to use stable and radiogenic isotope geochemistry in concert with analysis of general geochemical parameters of fluids and gases and analysis of core samples to determine geochemical processes occurring in the reef structure because of CO 2 injection..

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2025

Intrinsic Kinetics of Polyethylene Terephthalate Pyrolysis via Micropyrolysis and Multivariate Chromatographic Analysis

This study provides an in-depth investigation of the primary decomposition of polyethylene terephthalate (PET) via pyrolysis, employing an experimental-analytic workflow that integrates design of experiments (DoE), micropyrolysis coupled with comprehensive two-dimensional gas chromatography (GC×GC), and multivariate data analysis to verify intrinsic kinetic conditions and elucidate evolving product distributions for mapping key reaction pathways. Peaks that could not be identified using commercial spectral libraries were assigned using Mass Frontier simulations, enabling the identification of divinyl terephthalate, ethyl vinyl terephthalate, and 2-(benzoyloxy)ethyl vinyl terephthalate. A polar×polar (non-orthogonal) column set tailored for the detection of carboxylic acids enhanced the quantification of benzoic acid, 4-vinylbenzoic acid, 4-ethylbenzoic acid, and methylbenzoic acid by up to 6-fold relative to an orthogonal column combination (non-polar×mid-polar). Moreover, pyrolysis variables were systematically evaluated using a Box- Behnken design (BBD), encompassing pyrolysis temperature (500−600 °C), sample weight (50−150 μg), and carrier gas flow rate (100−300 mL min −1 ). Among these, pyrolysis temperature was the only statistically significant factor influencing product yields, ranging from 58.78 to 84.26 wt %. In contrast, neither the sample weight nor the carrier gas flow rate had a significant effect on product yields within the evaluated experimental space. At 600 °C, the major pyrolysis products were benzoic acid (up to 20.20 ± 1.46 wt %) and CO 2 (up to 21.28 ± 1.46 wt %), which can be produced through decarboxylation reactions. These findings underscore the critical importance of selecting appropriate analytical columns for the accurate quantification of heteroatomcontaining products such as carboxylic acids, which may otherwise be underestimated or undetected due to their reactivity with the stationary phase of non-polar and mid-polar columns, as well as other GC components. They also highlight the importance of selecting pyrolysis conditions for investigating the primary decomposition of PET under an isothermal kinetically limited regime.

aromatic compounds↗

DOE OSTI2019

Chemical Profiling of Volatile Organic Compounds in the Headspace of Algal Cultures as Early Biomarkers of Algal Pond Crashes

Algae ponds used in industrial biomass production are susceptible to pathogen or grazer infestation, resulting in pond crashes with high economic costs. Current methods to monitor and mitigate unhealthy ponds are hindered by a lack of early indicators that precede culture crash. We used solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS) to identify volatiles emitted from healthy and rotifer infested cultures of Microchloropsis salina. After 48 hours of algal growth, marine rotifers, Brachionus plicatilis, were added to the algae cultures and volatile organic compounds (VOC) were sampled from the headspace using SPME fibers. A GC-MS approach was used in an untargeted analysis of VOCs, followed by preliminary identification. The addition of B. plicatilis to healthy cultures of M. salina resulted in decreased algal cell numbers, relative to uninfected controls, and generated trans-β-ionone and β-cyclocitral, which were attributed to carotenoid degradation. The abundances of the carotenoid-derived VOCs increased with rotifer consumption of algae. Our results indicate that specific VOCs released by infected algae cultures may be early indicators for impending pond crashes, providing a useful tool to monitor algal biomass production and pond crash prevention.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Handling and Properties of Methanol as a Marine Fuel

Given the increasing concern around greenhouse gas emissions and the decline in the availability of fossil fuels, there is increasing global demand to develop alternate fuels for maritime transportation that are sustainable and which have lower greenhouse gas emissions. Methanol is one such alternative fuel that has garnered considerable attention given its potential to be produced by more sustainable processes and its more favorable greenhouse gas emission profile in comparison with current fossil fuels. Understanding the physical and chemical properties of methanol under a range of conditions is essential for its development as a marine fuel. In this study, we seek to define physical and chemical properties of different methanol samples to simulate real-world storage conditions as these data are lacking in the literature. Several methanol samples were evaluated: nearly pure methanol; International Organization for Standardization (ISO) marine methanol (MM) grades A, B, and C; and methanol plus higher alcohols. We first evaluated all methanol samples for impurities, acetic acid content, density, and distillation range. We then characterized the effects of water absorption and found that methanol can easily absorb unacceptable water content from humid air within hours, necessitating storage conditions that prevent this process. In eight-week aging experiments at 20 °C and 40 °C in ambient air, we did not observe significant oxidation for any of the methanol samples; however, we did observe increases in acid number. We assessed the impact of contamination of methanol with water, marine gas oil (MGO), and an MGO–biodiesel mixture on density, viscosity, distillation range, and lubricity. Finally, we show that MGO contamination of methanol results in a slight increase in sooting tendency. In aggregate, our results provide an in-depth analysis of physical and chemical properties of methanol as well as the impacts of storage conditions and impurities on the properties of fuel methanol.

09 BIOMASS FUELS↗

NASA NTRS1978

Static and dynamic cyclic oxidation of 12 nickel-, cobalt-, and iron-base high-temperature alloys

Twelve typical high-temperature nickel-, cobalt-, and iron-base alloys were tested by 1 hr cyclic exposures at 1038, 1093, and 1149 C and 0.05 hr exposures at 1093 C. The alloys were tested in both a dynamic burner rig at Mach 0.3 gas flow and in static air furnace for times up to 100 hr. The alloys were evaluated in terms of specific weight loss as a function of time, and X-ray diffraction analysis and metallographic examination of the posttest specimens. A method previously developed was used to estimate specific metal weight loss from the specific weight change of the sample. The alloys were then ranked on this basis. The burner-rig test was more severe than a comparable furnace test and resulted in an increased tendency for oxide spalling due to volatility of Cr in the protective scale and the more drastic cooling due to the air-blast quench of the samples. Increased cycle frequency also increased the tendency to spall for a given test exposure. The behavior of the alloys in both types of tests was related to their composition and their tendency to form scales. The alloys with the best overall behavior formed alpha-Al2O3 aluminate spinels.

Barrett, C. A.↗