Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “Gas sampling”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 703 records · Page 39

Deployment of a Fast-GCMS System to Measure C2 to C5 Carbonyls, Methanol and Ethanol Aboard Aircraft

Through funding of this proposal, a fast response gas chromatograph/mass spectrometer (FGCMS) instrument to measure less than or equal to C4 carbonyl compounds and methanol was developed for the NASA GTE TRACE-P (Global Tropospheric Experiment, Transport And Chemical Evolution Over The Pacific) mission. The system consists of four major components: sample inlet, preconcentration system, gas chromatograph (GC), and detector. The preconcentration system is a custom-built cryogen-conservative system. The GC is a compact, custom-built unit that can be temperature programmed and rapidly cooled. Detection is accomplished with an Agilent Technologies 5973 mass spectrometer. The FGCMS instrument provides positive identification because the compounds are chromatographically separated and mass selected. During TRACE-P, a sample was analyzed every 5 minutes. The FGCMS limit of detection was between 5 and 75 pptv, depending on the compound. The entire instrument package is contained in a standard NASA instrument rack (106 cm x 61 cm x 135 cm), consumes less than 1200 watts and is fully automated with LabViEW 6i. Methods were developed or producing highly accurate gas phase standards for the target compounds and for testing the system in the presence of potential interferents. This report presents data on these tests and on the general overall performance of the system in the laboratory and aboard the DC-8 aircraft during the mission. Vertical profiles for acetaldehyde, methanol, acetone, propanal, methyl ethyl ketone, and butanal from FGCMS data collected over the entire mission are also presented.

Apel, Eric C.↗

COMPASS-FME Synoptic Site Tree Greenhouse Gas Concentrations

These data are tree stem greenhouse gas concentrations collected from tree gas wells at some of the COMPASS-FME (Coastal Observations, Mechanisms, and Predictions Across Systems and Scales; see https://compass.pnnl.gov/) 'synoptic' sites in the Chesapeake Bay region: Moneystump (MSM), Goodwin Islands (GWI), and GCReW (GCW). The sap flow monitoring trees at these sites in the Upland (UP) and Transition (TR) zones were cored and had gas wells installed at breast height. There were also some dead standing trees cored, gas well installed, and sampled at MSM and GWI. The GCW UP samples overlap with the TEMPEST experiment control plot, so the GCW UP data was pulled from the TEMPEST page and included here. These data provide crucial information about possible pathways for the greenhouse gas (carbon dioxide and methane, CO2 and CH4 respectively) production and emission (or in the case of CH4, perhaps taken up from) the atmosphere.All data are plain text CSV (comma separated value) files and require no special software to read.Updated 2025-10-09 to fix two missing dates (lines 77 and 78 in the data file).

54 ENVIRONMENTAL SCIENCES↗

Measuring Multicomponent Adsorption of Tracer Gases on Natural Zeolites

A natural clinoptilolite sample near the Nevada National Security Site was obtained to study adsorption and retardation on gas transport. Of interest is understanding the competition for adsorption sites that may reduce tracer gas adsorption relative to single-component measurements, which may be affected by the multi-scale pore structure of clinoptilolite. Clinoptilolite has three distinct domains of pore size distributions ranging from nanometers to micrometers: micropores with 0.4–0.7 nm diameters, measured on powders by CO2 adsorption at 273 K, representing the zeolite cages; mesopores with 4–200 nm diameters, observed using liquid nitrogen adsorption at 77 K; and macropores with 300–1000 nm diameters, measured by mercury injection on rock chips (~ 100 mesh), likely representing the microfractures. These pore size distributions are consistent with X-ray computed tomography (CT) and focused ion beam scanning electron microscope (FIB-SEM) images, which are used to construct the three-dimensional (3D) pore network to be used in future gas transport modeling. To quantify tracer gas adsorption in this multi-scale pore structure and multicomponent gas species environment, natural zeolite samples initially in equilibrium in air were exposed to a mixture of tracer gases. As the tracer gases diffuse and adsorb in the sample, the remaining tracer gases outside the sample fractionate. Using a quadrupole mass spectrometer to quantify this fractionation, the degree of adsorption of tracer gases in the multicomponent gas environment and multi-scale pore structure is assessed. The major finding is that Kr reaches equilibrium much faster than Xe in the presence of ambient air, which leads to more Kr uptake than Xe over limited exposure periods. When the clinoptilolite chips were exposed to humid air, the adsorption capability decreases significantly for both Xe and Kr with relative humidity (RH) as low as 3%. Both Xe and Kr reaches equilibrium faster at higher RH. The different, unexpected, adsorption behavior for Xe and Kr is due to their kinetic diameters similar to the micropores in clinoptilolite which makes it harder for Xe to access compared to Kr.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Subtask 2.6 – Optimization of Aerosol Mitigation Technology for Postcombustion CO 2 Capture

Growing concerns over the impact of CO 2 emissions from combustion sources on global climate change have prompted numerous research and development projects aimed at developing cost-effective technologies for CO 2 capture. One family of technologies being demonstrated at pilot and full scale globally is postcombustion CO 2 capture (PCCC) systems that employ amine-based solvents. The captured CO 2 can be compressed and permanently stored underground or used for enhanced oil recovery (EOR). The proximity of North Dakota’s lignite-fired fleet of power plants to potential CO 2 storage options creates a unique atmosphere for PCCC within the state. However, the aerosols present in lignite flue gas present a challenge for large-scale PCCC at North Dakota power plants. Aerosols can negatively impact the long-term performance of amine-based solvents for CO 2 capture. Amine-based solvents are volatile, and aerosols provide nucleation sites where amine vapors can condense. Because aerosols cannot be easily captured at the column outlet using conventional technologies, the amine-laden aerosols escape the system and lead to accelerated solvent losses. Moreover, aerosol components can chemically react with amines to form degradation products that can permanently deactivate the amine, cause fouling, and lead to hazardous emissions. Many of the elements that have been shown to catalyze solvent degradation are present in lignite coals and can exacerbate solvent replacement economics. Understanding this issue is critical to the implementation of solvent-based CO 2 capture systems as applied to lignite-fired generation systems. The Energy & Environmental Research Center (EERC) designed and carried out this project to optimize aerosol mitigation technology for PCCC at a lignite-fired power plant. To meet the goal of this project, the following objectives were identified: Determine the effectiveness of a wet electrostatic precipitator (WESP) on collection of aerosols at a low-rank coal-fired power station. Determine the impact of aerosols on the efficiency and degradation products of amine-based carbon capture systems fired with low-rank fuels. Work was conducted at Minnkota Power Cooperative’s (MPC’s) Milton R. Young (MRY) Station Unit 2 using a slipstream of flue gas from the outlet of the plant’s flue gas desulfurization (FGD) unit. To gather initial data for sizing and specifying a WESP for this system, a temporary pilot-scale WESP was rented and installed on-site. Several different conditions were tested to examine the impact of flow rate, voltage, and current on WESP performance. The WESP was effective at removing large particulate (>200 nm) but caused an increase in fine particulate (<75 nm). Fine particulate material at the inlet and outlet of the WESP was collected, analyzed, and showed that crystalline sulfates carried over from the plant’s FGD unit were being converted to fine aerosols and SO 2 was being converted to SO 3 through the WESP. Additionally, the high moisture content of the flue gas stream at this sample location also contributed to an overall increase in aerosol mass under some of the test conditions. Using the results from the rented WESP, the project team installed a smaller-scale WESP upstream of the EERC’s slipstream CO 2 capture system. Flue gas was routed through a pilot-scale FGD unit to remove SO 2 to very low levels (~1 ppm) and then through a direct contact cooler (DCC) to further cool the gas and to remove moisture. The gas exiting the DCC was then routed through the new WESP before passing to the CO 2 absorber columns. Fluor’s amine-based solvent was used to scrub CO 2 from the slipstream through a set of two absorber columns. The rich solvent was regenerated in a stripper column by heating to drive off captured CO 2 . The system operated using a catch-and-release method where the CO 2 was separated to provide data on the process, but the captured CO 2 was released back into the host site stack. Aerosols and sulfur species were measured at multiple locations throughout the pilot-scale system. The inlet FGD and DCC removed much of the particulate matter and gaseous sulfur upstream of the WESP. With this configuration, the WESP achieved >95% particulate capture. The new WESP did not show any of the increases in SO 3 or other aerosol species that had been consistently observed with the larger-scale WESP installed immediately downstream of the plant’s full-scale FGD unit. Particulate samples captured and analyzed from the WESP inlet did not show any presence of crystalline sulfate materials, indicating that the pilot-scale FGD and DCC were efficient at reducing carryover from the plant’s full-scale FGD unit. A set of parametric tests were conducted on the new WESP to assess the impacts of flow rate, voltage, number of online WESP fields, and gas-phase sulfur content on aerosol and sulfur transformations. The results showed that the WESP performed similarly well at all sets of conditions. Sulfur and particulate matter exiting the WESP were further reduced through the absorber column as the amine-based solvent captured some of the residual contaminants. Solvent analysis showed that these species were slowly concentrating in the solvent over the duration of the test. When the WESP was taken offline and the sulfur slip through the FGD allowed to rise, the sulfate content in the solvent rose sharply, showing that the extra FGD and WESP were effective at reducing sulfate and cation uptake. This would be expected to extend amine-based solvent life by slowing the formation of heat-stable salts and other degradation products. This subtask was cofunded through the EERC–U.S. Department of Energy Joint Program on Research and Development for Fossil Energy-Related Resources Cooperative Agreement No. DE-FE0024233. Nonfederal funding was provided by the North Dakota Industrial Commission and MPC.

01 COAL, LIGNITE, AND PEAT↗

Trapped solar and cosmogenic noble gas abundances in Apollo 15 and 16 deep drill samples

Abundances and isotopic compositions of all the stable noble gases (He, Ne, Ar, Kr, Xe) were measured at different depths of the Apollo 15 and Apollo 16 deep drill cores, and in several surface fines and breccias. All samples analyzed from both drill cores were found to contain large concentrations of solar wind implanted gases. This means that even the deepest layers of both cores have experienced a lunar surface history. The Apollo 15 core data are consistent with a combined accretion plus static time of a few hundred million years, and also indicate variable pre-accretion irradiation of core material. Depth profiles of cosmogenic gases in the Apollo 16 core show considerably larger concentrations of cosmic gases below 65 cm depth than above. This pattern may be interpreted either as an accretionary process, or by a more recent deposition of regolith to the upper 70 cm of the core.

Bogard, D. D.↗

Laser, vacuum and gas reaction chamber for operando measurements at NSLS-II's 28-ID-2

We present a laser reaction chamber that we have developed for in situ/operando X-ray diffraction measurements at the NSLS-II 28-ID-2 X-ray powder diffraction beamline. This chamber allows for rapid and dynamic sample heating under specialized gas environments, spanning ambient conditions down to vacuum pressures. We demonstrate the capabilities of this setup through two applications: laser-driven heating in polycrystalline iron oxide and in single-crystal WTe 2 . Our measurements reveal the ability to resolve chemical reaction kinetics over minutes with 1 s time resolution. This setup advances opportunities for in situ/operando X-ray diffraction studies of both bulk and single-crystal materials.

36 MATERIALS SCIENCE↗

SAGAbg. I. A Near-unity Mass-loading Factor in Low-mass Galaxies via Their Low-redshift Evolution in Stellar Mass, Oxygen Abundance, and Star Formation Rate

Measuring the relation between star formation and galactic winds is observationally difficult. In this work we make an indirect measurement of the mass-loading factor (the ratio between the mass outflow rate and star formation rate) in low-mass galaxies using a differential approach to modeling the low-redshift evolution of the star-forming main sequence and mass–metallicity relation. We use Satellites Around Galactic Analogs (SAGA) background galaxies, i.e., spectra observed by the SAGA Survey that are not associated with the main SAGA host galaxies, to construct a sample of 11,925 spectroscopically confirmed low-mass galaxies from 0.01 ≲ z ≤ 0.21 and measure auroral line metallicities for 120 galaxies. The crux of the method is to use the lowest-redshift galaxies as the boundary condition of our model, and to infer a mass-loading factor for the sample by comparing the expected evolution of the low-redshift reference sample in stellar mass, gas-phase metallicity, and star formation rate against the observed properties of the sample at higher redshift. We infer a mass-loading factor of η m = $0.92^{+1.76}_{-0.74}$, which is in line with direct measurements of the mass-loading factor from the literature despite the drastically different sets of assumptions needed for each approach. While our estimate of the mass-loading factor is in good agreement with recent galaxy simulations that focus on resolving the dynamics of the interstellar medium, it is smaller by over an order of magnitude than the mass-loading factor produced by many contemporary cosmological simulations.

79 ASTRONOMY AND ASTROPHYSICS↗

In-Field Alpha Spectrometry to Assess Uranium Enrichment In Uranium Hexafluoride

A new In-Field Alpha Spectrometry (IFAS) system is being developed to allow quick turnaround measurements of uranium enrichment in uranium hexafluoride (UF6) samples. Samples are collected using specially-designed Single-Use Destructive Assay (SUDA) wafers which have an absorptive film of zeolite deposited onto a quartz or metal substrate. The SUDA samples, along with a special holder, are designed to be attached directly to a sampling tap at a gas centrifuge enrichment plant or a uranium conversion facility, allowing gaseous UF6 to come into direct contact with the zeolite. The zeolite absorbs this material and converts it into stable, safe UO2F2 within a few minutes. Once the sample has been collected it is transferred to the IFAS system where a solid-state, silicon alpha spectrometer is used to quantitatively measure the alpha emissions from 234U, 235U, and 238U in the sample. The IFAS system is a small, light-weight device that can be quickly turned on and put into use. The SUDA samples and IFAS hardware are designed so that thin-film spectra are produced, allowing a complete measurement with a final 235U:Utotal determination having a precision <±2% to be made in less than eight hours. This short time frame will allow an inspector to get results on-site within one working shift; further innovations may reduce this to even shorter times.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

In-Field Alpha Spectrometry to Assess Uranium Enrichment In Uranium Hexafluoride

A new In-Field Alpha Spectrometry (IFAS) system is being developed to allow quick turnaround measurements of uranium enrichment in uranium hexafluoride samples. Samples are collected using specially-designed Single-Use Destructive Assay (SUDA) wafers which have an absorptive thin film of zeolite deposited onto a quartz substrate. The SUDA samples, along with a special holder, are designed to be attached directly to a sampling tap at a gas centrifuge enrichment plant or a uranium conversion facility, allowing gaseous UF6 to come into direct contact with the zeolite. The zeolite absorbs this material and converts it into stable, safe UO2F2 within a few minutes. Once the sample has been collected it is transferred to the IFAS system where a solid-state, silicon alpha spectrometer is used to quantitatively measure the alpha emissions from 234U, 235U, and 238U form the sample. The SUDA samples are designed so that thin-film spectra are produced, and the SUDA samples and IFAS system are designed so that a complete measurement, with a final 235U:Utotal determination of <±2%, can be made in less than eight hours. This short time frame will allow an inspector to get results on-site within one working shift.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗

Laboratory corroboration of the Pioneer Venus gas chromatograph analyses

Laboratory simulation and tests of the inlet sampling system and columns of the Pioneer Venus gas chromatograph show that the sensitivity to argon is not diminished after the column regeneration step, that argon isotopes are not separated, that oxygen and sulfur dioxide are not produced in the inlet sampling system from sulfur trioxide, and that sulfur trioxide is not formed from sulfur dioxide and oxygen. Comparisons of the volatile inventory of Venus and earth imply similar efficiencies of early outgassing but a lower efficiency for later outgassing in the case of Venus. The high oxidation state of the Venus atmosphere in the region of cloud formation may prohibit the generation of elemental sulfur particles.

Oyama, V. I.↗

Swelling and Fission Gas Release of U-10Mo and U-17Mo Following Neutron Irradiation at 250 – 500°C

The performance of metallic fuel alloys, U-10Mo and U-17Mo, was examined using the MiniFuel test system in the High Flux Isotope Reactor. Approximately 0.8 mm thick disks were irradiated at target temperatures of 250°C, 350°C, 450°C, and 500°C up to three different fission densities, culminating at a maximum fission density of 6.8 × 10 20 cm −3 . Fission rates decayed from 3 – 6 × 10 13 cm −3 s −1 to 2 – 4 × 10 13 cm −3 s −1 over the course of the longest, eight cycle, irradiation as the 235 U was consumed and the 239 Pu concentration accumulated. Actual irradiation temperature on the last day of irradiation was measured via dilatometry using the SiC passive thermometry recovered from the MiniFuel subcapsules and compared favorably with the thermal calculations using as-built geometry and test conditions. Furthermore, average simulated temperatures were within 50°C of the target temperatures, except for the 500°C irradiation, for which the temperature variation was 62°C, 32°C, and 90°C in the in two, four, and eight cycle irradiations, respectively. Fission gas release (FGR) measurements showed no release above recoil for any U-17Mo fuels or for the U-10Mo fuel irradiated at 250°C. Finally, significant (40%–80%) FGR was found for the medium- to highest-burnup U-10Mo samples irradiated at target temperatures 350°C–500°C. Significant FGR correlated with sample thickness swelling, which was as high as 13%–35% for high-release samples and below 7% for all other (low–gas release) samples.

FGR↗

Ecology and thermal inactivation of microbes in and on interplanetary space vehicle components

An experimental sterilization facility was developed to simulate conditions that will be encountered during terminal sterilization of space vehicles. The system consists of a temperature controlled oven with a nitrogen gas stream containing a known concentration of water. Moisture analyzers are utilized to monitor the gas flowing over spore samples contained in the oven. In its original configuration, no provision was made for the control of water vapor during the sterilization cycle. Because moisture profoundly influences the thermal inactivation of bacterial spores, an upper limit for the moisture content in the gas used to sterilize the space vehicle was established (25% RH at 0 C STP). Accordingly, a controller was developed and installed to provide these conditions in the experimental sterilization facility.

Wimsatt, J. C.↗

Ambient Mass Spectrometry Rapid Analysis Methods for Trace Inorganics

The ability to rapidly detect and characterize the chemistry of trace quantities of inorganic species has multiple potential applications, including nuclear safeguards, nuclear forensics, and environmental monitoring. Some mass spectrometric methods currently exist, but they are costly and time-intensive, often destroying chemical information in the process of ionization. Ambient mass spectrometry is a relatively new analytical method in which samples are introduced to the mass spectrometer from atmospheric pressure, rather than from high vacuum. Ambient MS can operate with gentler ionization methods such as electrospray ionization (ESI) and paper-spray ionization (PSI), reducing fragmentation and preserving the chemical information of the analyte. This may be useful for determining the intended purpose of material in a sample. Strontium, part of nuclear fallout, is analyzed here to test these new analytical methods for viability. Electrospray ionization mass spectrometry functions by spraying the sample as a solution through a needle charged to a few kV. A nebulizing gas flows out along with the sample to create the spray before droplets enter a drying chamber with heated drying gas to remove the solvent molecules. From there bare analyte ions enter the mass spectrometer. This method has the advantage of relatively fast sample preparation and stable ionization. More stable ionization produces higher-quality data. Paper-spray ionization mass spectrometry operates by applying sample to a paper triangle. The paper triangle is then electrified in a metal clamp to a few kV before spray solvent is applied. The spray solvent transports analyte in the sample to the tip, where it is ionized and enters the mass spectrometer. One advantage of this method is reduced sample preparation - an analyst can even swipe a surface and cut a triangle directly from the swipe. The data analysis serves to rapidly process tens of samples all at once. The mass spectrometer outputs a file containing a few hundred spectra for each sample. The pipeline processes each one to identify peaks of interest. A full palette of data analysis metrics are generated, including plots of the raw data and plots of calculated values such as isotopic ratios. The pipeline filters the raw data to remove noise and background peaks, as well as peaks representing detector saturation. A heat map is generated to show the overall spectrum in mass-time- intensity space. Post-processing, we obtained the desired calibration curves, demonstrating that both ESI-MS and PSI-MS are viable methods for quantifying trace amounts of inorganics while retaining their chemical speciation information. ESI-MS demonstrated a linear response region of 100 ppb to 20 ppm, with a limit-of-detection of around 100 ppb. At top left is an example spectrum with the {sup 88}SrNO{sub 3} peak identified to show the retention of chemical speciation. PSI-MS showed a linear response region of around 1 ppb to 1 ppm, with a limit-of-detection of near 1 ppb. PSI-MS produced more erratic results than ESI-MS, likely due to the variability in ionization resulting from manual positioning of the paper triangle near the MS inlet. Future efforts will focus on improving the repeatability of PSI-MS as well as analyzing other species of interest such as cerium and uranium. Improvements will also be made to create more reliable data extraction and intelligent data filtering.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Peroxide-modified titanium dioxide: a chemical analog of putative Martian soil oxidants

Hydrogen peroxide chemisorbed on titanium dioxide (peroxide-modified titanium dioxide) is investigated as a chemical analog to the putative soil oxidants responsible for the chemical reactivity seen in the Viking biology experiments. When peroxide-modified titanium dioxide (anatase) was exposed to a solution similar to the Viking labeled release (LR) experiment organic medium, CO2 gas was released into the sample cell headspace. Storage of these samples at 10 degrees C for 48 hr prior to exposure to organics resulted in a positive response while storage for 7 days did not. In the Viking LR experiment, storage of the Martian surface samples for 2 sols (approximately 49 hr) resulted in a positive response while storage for 141 sols essentially eliminated the initial rapid release of CO2. Heating the peroxide-modified titanium dioxide to 50 degrees C prior to exposure to organics resulted in a negative response. This is similar to, but not identical to, the Viking samples where heating to approximately 46 degrees C diminished the response by 54-80% and heating to 51.5 apparently eliminated the response. When exposed to water vapor, the peroxide-modified titanium dioxide samples release O2 in a manner similar to the release seen in the Viking gas exchange experiment (GEx). Reactivity is retained upon heating at 50 degrees C for three hours, distinguishing this active agent from the one responsible for the release of CO2 from aqueous organics. The release of CO2 by the peroxide-modified titanium dioxide is attributed to the decomposition of organics by outer-sphere peroxide complexes associated with surface hydroxyl groups, while the release of O2 upon humidification is attributed to more stable inner-sphere peroxide complexes associated with Ti4+ cations. Heating the peroxide-modified titanium dioxide to 145 degrees C inhibited the release of O2, while in the Viking experiments heating to this temperature diminished but did not eliminated the response. Although the thermal stability of the titanium-peroxide complexes in this work is lower than the stability seen in the Viking experiments, it is expected that similar types of complexes will form in titanium containing minerals other than anatase and the stability of these complexes will vary with surface hydroxylation and mineralogy.

Review↗

X-Ray Amorphous Sulfur-Bearing Phases in Sedimentary Rocks of Gale Crater, Mars

The Curiosity rover in Gale crater is investigating a mineral transition observed from orbit—an older “clay unit” to a younger “sulfate unit”—hypothesized to reflect the aridification of Mars' climate. Below this transition, the rover detected crystalline Ca-sulfates with minor Fe-sulfates but also found that some fraction of a rock's bulk SO 3 is often in the poorly constrained X-ray amorphous component. Here, we characterize the abundances and compositions of the X-ray amorphous sulfur-bearing phases in 19 drilled samples using a mass balance approach, and in a subset of 5 samples using evolved SO 2 gas measured using the SAM instrument. We find that ∼20–90 wt% of a sample's bulk SO 3 is in the X-ray amorphous state and that X-ray amorphous sulfur-bearing phase compositions are consistent with mixtures of Mg-S, Fe-S, and possibly Ca-S phases, likely sulfates or sulfites. These phases reside in the bedrock, perhaps as cementing agents deposited with detrital sediments or during early diagenesis, and in diagenetic alteration halos deposited after lithification during late diagenesis. The likely presence of highly soluble Mg-sulfates in the rocks suggests negligible fluid flow through the bedrock post-Mg-sulfate deposition. The X-ray amorphous sulfur-bearing phases probably became amorphous through dehydration in the current Martian atmosphere or inside the CheMin instrument. X-ray amorphous sulfur-bearing materials likely contribute to orbital spectral detections of sulfates, and so our results help form multiple hypotheses to be tested in the sulfate unit and are important for understanding the evolution of the Martian surface environment at Gale crater.

R. J. Smith↗