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At least 811 records · Page 45
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Impact of Boron-Containing Lubricant Additive on Three-Way Catalyst Reactivity and Physicochemical Properties

Boron-containing compounds are one of the lubricant additive options due to their suitable properties for additives and have been used as commercial lubricant additives. In the present study, the impact of a boron-containing lubricant oil additive, AR9100 (BR), on Pd/Rh-based three-way catalyst (TWC) performance is investigated, and the results are compared with the baseline no-additive (NA) case and the industry standard zinc dialkyl-dithiophosphate (ZDDP) results. Accelerated engine aging is performed using a genset to expose the catalysts to lubricant additives at high temperatures. All aged TWC samples are investigated for reactivity in a bench-flow reactor and characterized using a variety of analytical techniques. Compared with the no-additive case, the temperatures of 90% conversion (T 90 ) of NO, CO, C 3 H 6 , and C 3 H 8 for the ZDDP-aged TWC sample increased by 34, 30, 37, and 48 °C. However, the T 90 of all gas species for the BR-aged TWC sample are similar to the NA-aged TWC sample. Additionally, a significant decrease in water–gas shift reactivity and oxygen storage capacity is observed in the ZDDP-aged sample, but not in the BR-aged sample. Inductively coupled plasma-optical emission spectrometry (ICP-OES) analysis and electron probe microanalysis (EPMA) maps of accelerated engine aging samples show the presence of phosphorus and boron in ZDDP- and BR-aged TWC samples, respectively. However, no boron-related peaks are observed in the X-ray diffraction (XRD) pattern of the BR-aged TWC sample, which may exist in the form of an amorphous phase.

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

Improvement of Drop‐Hammer Impact Testing for Safety Assessment of High Explosives Using 10‐mg Samples

Here, in this study, we established an improved method for drop-hammer impact testing of small quantities of high explosives (10 mg). We performed about seven hundred impact tests under various experimental conditions (e.g., sandpaper vs bare anvil, different sample masses, drop-weights, and striker diameters) to determine an optimal set of conditions and reaction detection methods (e.g., gas analysis, video, and sound recordings) that give the most statistically reliable results with 10 mg samples. We used both Frequentist and Bayesian statistical approaches to compare estimates of the drop height (DH50) that initiates a reaction 50% of the time, and to quantify the associated uncertainty. Gas analysis proved to be the most reliable reaction detection method, showing unambiguous rises in HE decomposition products (e.g., CO 2 ) even when the other indicators (e.g., sound, video) were inconclusive. The impact tests performed with a bare anvil showed much better reproducibility than those conducted with sandpaper, reducing the largest uncertainty observed in the data sets by a factor of 1.7. The DH 50 values obtained from three different sample masses (10, 20, and 35 mg) fell within the uncertainties of the measurements. We demonstrated the improved procedure (i.e., 10-mg samples, gas analysis, bare anvil, and Bayesian approach) on a variety of PETN samples having different surface areas and thermal histories.

PETN↗
NASA NTRS1998

Dissolved gases in perennially ice-covered lakes of the McMurdo Dry Valleys, Antarctica

Measurements of dissolved N2, O2, Ar, CO2, and CH4 were made in perennially ice-covered Lake Hoare. Results confirm previous reports that O2 concentrations in the upper water column exceed atmospheric equilibrium and that N2 and Ar are supersaturated throughout the water column. The mean supersaturation of N2 was found to be 2.0 (+/- 0.37) and Ar was 3.8 (+/- 1.1). The ratios of N2/Ar (20.3 +/- 13.8), and O2/Ar (22.5 +/- 4.0) at the ice-water interface are consistent with those previously measured, suggesting that bubble formation is the main process for removing gas from the lake. However, the saturations of N2 and Ar greatly exceed those previously predicted for degassing by bubble formation only at the ice-water interface. The data support the hypothesis that removal of gas by bubbles occurs in the water column to a depth of 11 m in Lake Hoare. CO2 concentration increases from near zero at the ice-water interface to 80-100 times saturation at and below the chemocline at c. 28 m. There is considerable variability in the gas concentrations throughout the water column; samples separated in depth by one metre may vary by more than 50% in gas content. It is likely that this phenomenon results from the lack of turbulent mixing in the water column. Methane (c. 2 micrograms l-1) was detected below the chemocline and immediately above the sediment/water interface at a depth of 30 m. Samples from lakes Vanda, Joyce, and Miers, also show supersaturations of O2, N2, and Ar at levels similar to levels found in Lake Hoare.

NASA Discipline Exobiology↗
NASA NTRS1973

Inert gas stratigraphy of Apollo 15 drill core sections 15001 and 15003

Rare gase contents were studied in Apollo 15 drill core sections corresponding to 207 to 238 and 125 to 161-cm depths, with respect to layering of the core, turnover on a centimeter scale, and cosmic proton bombardment history. Trapped gas abundance was established in all samples, the mean grain size being a major factor influencing the absolute rare gas contents. Analysis of the results suggests that the regolith materials were exposed to galactic and solar cosmic rays long before their deposition.

Huebner, W.↗
NASA NTRS2014

Characterizing the Phyllosilicate Component of the Sheepbed Mudstone in Gale Crater, Mars Using Laboratory XRD and EGA

The Curiosity rover investigated the mineralogy of the Sheepbed mudstone member of the Yellowknife Bay formation in Gale crater. Data from the Chemistry and Mineralogy (CheMin) X-ray diffractometer (XRD) helped identify phyllosilicates in the two drilled samples, John Klein and Cumberland. These patterns showed peaks at low angles, consistent with (001) peaks in 2:1 swelling phyllosilicates [1]. Evolved gas analyses (EGA) by the Sample Analysis at Mars (SAM) instrument of these samples confirmed the presence of phyllosilicates through the release of H2O at high temperatures, consistent with dehydroxylation of octahedral OH in phyllosilicates [2]. CheMin data for the phyllosilicates at John Klein and Cumberland show that they are structurally similar in that their (02l) peaks are near 22.5 deg 2theta, suggesting both samples contain trioctahedral 2:1 phyllosilicates [1]. However, the positions of the (001) peaks differ: the phyllosilicate at John Klein has its (001) peak at 10 Angstroms, whereas the phyllosilicate at Cumberland has an (001) peak at 14 Angstroms. Such differences in (001) dspacings can be ascribed to the type of cation in the interlayer site [3]. For example, large monovalent cations (e.g., K(+)) have low hydration energies and readily lose their H2O of hydration, whereas small divalent cations (e.g., Mg(2+)) have high energies of hydration and retain H2O in the phyllosilicate interlayers [3,4]. The goal of this study is to determine whether differences in the interlayer cation composition can explain the CheMin data from John Klein and Cumberland and to use this knowledge to better understand phyllosilicate formation mechanisms.

Rampe, E. B.↗
NASA NTRS1975

Cosmic ray exposure ages of features and events at the Apollo landing sites

Cosmic-ray exposure ages of lunar samples have been used to date surface features related to impact cratering and downslope movement of material. Only when multiple samples related to a feature have the same rare-gas exposure age or when a single sample has the same Kr-81 -Kr and track-exposure age can a feature be considered as reliably dated. Based on these criteria, there are only five well-dated lunar features: Cone Crater (Apollo 14), 26 m.y,; North Ray Crater (Apollo 16), 50 m.y.; South Ray Crater (Apollo 16), 2 m.y.; the emplacement of the Station 6 boulders (Apollo 17), 22 m.y.; and the emplacement of the Station 7 boulder (Apollo 17), 28 m.y. Other features are tentatively dated or have limits set on their ages: Bench Crater (Apollo 12), upper limit of 99 m.y.; Baby Ray Crater (Apollo 16), upper limit of 2 m.y.; Shorty Crater (Apollo 17), approximately 30 m.y.; Camelot Crater (Apollo 17) upper limit of 140 m.y.; the emplacement of the Station 2 boulder 1 (Apollo 17), 45 to 55 m.y.; and the slide which generated the light mantle (Apollo 17), lower limit of 50 m.y.

Arvidson, R.↗
NASA NTRS2009

Evolved Gas Measurements Planned for the Lower Layers of the Gale Crater Mound with the Sample Analysis at Mars Instrument Suite

The lower mound strata of Gale Crater provide a diverse set of chemical environments for exploration by the varied tools of the Curiosity Rover of the Mars Science Laboratory (MSL) Mission. Orbital imaging and spectroscopy clearly reveal distinct layers of hydrated minerals, sulfates, and clays with abundant evidence of a variety of fluvial processes. The three instruments of the MSL Sample Analysis at aMars (SAM) investigation, the Quadrupole Mass Spectrometer (QMS), the Tunable Laser Spectrometer (TLS), and the Gas Chromatograph (GC) are designed to analyze either atmospheric gases or volatiles thermally evolved or chemically extracted from powdered rock or soil. The presence or absence of organic compounds in these layers is of great interest since such an in situ search for this type of record has not been successfully implemented since the mid-60s Viking GCMS experiments. However, regardless of the outcome of the analysis for organics, the abundance and isotopic composition of thermally evolved inorganic compounds should also provide a rich data set to complement the mineralogical and elemental information provided by other MSL instruments. In addition, these evolved gas analysis (EGA) experiments will help test sedimentary models proposed by Malin and Edgett (2000) and then further developed by Milliken et al (2010) for Gale Crater. In the SAM EGA experiments the evolution temperatures of H2O, CO2, SO2, O2, or other simple compounds as the samples are heated in a helium stream to 1000 C provides information on mineral types and their associations. The isotopic composition of O, H, C, and S can be precisely determined in several evolved compounds and compared with the present day atmosphere. Such SAM results might be able to test mineralogical evidence of changing sedimentary and alteration processes over an extended period of time. For example, Bibring et al (2006) have suggested such a major shift from early nonacidic to later acidic alteration. We will illustrate through a variety of evolved gas experiments implemented under SAM-like gas flow and temperature ramp conditions on terrestrial analog minerals on high fidelity Sam breadboards the type of chemical information we expect SAM to provide.

Mahaffy, Paul↗
NASA NTRS1973

Development of mass spectrometric techniques applicable to the search for organic matter in the lunar crust

Data processing techniques were developed to measure with high precision and sensitivity the line spectra produced by a high resolution mass spectrometer. The most important aspect of this phase was the interfacing of a modified precision microphotometer-comparator with a computer and the improvement of existing software to serve the special needs of the investigation of lunar samples. In addition, a gas-chromatograph mass spectrometer system was interfaced with the same computer to allow continuous recording of mass spectra on a gas chromatographic effluent and efficient evaluation of the resulting data. These techniques were then used to detect and identify organic compounds present in the samples returned by the Apollo 11 and 12 missions.

Biemann, K.↗
NASA NTRS2013

Possible Detection of Perchlorates by Evolved Gas Analysis of Rocknest Soils: Global Implication

The Sample Analysis at Mars (SAM) instrument suite on board the Mars Science Laboratory (MSL) recently ran four samples from an aeolian bedform named Rocknest. Rocknest was selected as the source of the first samples analyzed because it is representative of both windblown material in Gale crater as well as the globally-distributed dust. The four samples analyzed by SAM were portioned from the fifth scoop at this location. The material delivered to SAM passed through a 150 m sieve and should have been well mixed during the sample acquisition/ preparation/handoff process. Rocknest samples were heated to ~835 C at a 35 C/minute ramp rate with a He carrier gas flow rate of ~1.5 standard cubic centimeters per minute and at an oven pressure of ~30 mbar. Evolved gases were detected by a quadrupole mass spectrometer (QMS).

Archer, P. D., Jr.↗
DOE OSTI2020

Multimodal Mass Spectrometry Imaging (MSI) of Archean and Jurassic Geologic Samples

Current geochemical analytical techniques such as gas chromatography-mass spectrometry (GC-MS and $G\acute{C}GC-MS$) can effectively determine the composition and structure of the organic biosignatures within a sample but cannot resolve the spatial distribution of organic biosignatures within rocks or sediments. The spatial distribution can be used to determine the character of the organic biosignatures [1], which can be indigenous (deposited with host rocks), non-indigenous (incorporated after deposition via fluid migration), or contaminant. Determining the character of organic biosignatures is critical for ancient samples [2] and will be critical if organics are observed in samples returned from Mars [3].Fs-LDPI-MS has the ability to map organic compounds across the surface of samples at 2 - 10 μm lateral resolution. Furthermore, fs-LDPI-MS can be used to carry out multiple analyses in the same location for micron-scale analysis of previously buried material [4]. We used fs-LDPI-MS to examine a ~164 million year old organic-rich mudstone from SW England (14.2 wt. % total organic carbon) [5] and determined the spatial distribution of likely indigenous components buried below potentially contaminated surface layers.We then used ToF-SIMS to re-analyze the mudstone to directly compare ToF-SIMS to fs-LDPI-MS datasets, and to analyze a series of ~2.7 billion year old geologic samples from Timmins, ON, CA [6]. Ref. [6] previously analyzed the Archean samples and observed a series of archaeal biomarkers, as well as hopanes and steranes. Using ToF-SIMS analysis, we were able to detect hopanes and steranes in the mudstone samples, but not in the Archean samples indicating that the hopanes and steranes are most likely contaminants in the Archean samples. We also did not observe the archaeal biomarkers; however, this may be from the lack of molecular ion preservation during ToF-SIMS.

Pasterski, Michael↗
NASA NTRS1977

Anomalous krypton in the Allende meteorite

The reported investigation provides important new data for the heavy noble gases, especially Kr, in the Allende meteorite. The data are used to criticize the original model of Lewis et al. (1975) based on the noble gas data of these researchers. The conclusions reached in the investigation support alternative models which have been mainly based on Xe data by Lewis et al. (1975, 1977). Because of the relatively high noble gas abundances in the separates studied, disturbance from nuclear effects occurring in situ such as spallation and neutron capture is insignificant, offering an opportunity to study primordial Ar, Kr, and Xe. The isotopic and abundance data obtained from the samples largely confirm the noble gas results of Lewis et al. (1975, 1977) where isotopic correlations agree with the correlations of the considered samples. It is found that both Kr and Xe data are consistent with a two component mixture of 'ordinary' as well as 'anomalous' planetary gases.

Frick, U.↗
NASA NTRS1972

Microphysical, microchemical and adhesive properties of lunar material. 3: Gas interaction with lunar material

Knowledge of the reactivity of lunar material surfaces is important for understanding the effects of the lunar or space environment upon this material, particularly its nature, behavior and exposure history in comparison to terrestrial materials. Adsorptive properties are one of the important techniques for such studies. Gas adsorption measurements were made on an Apollo 12 ultrahigh vacuum-stored sample and Apollo 14 and 15 N2-stored samples. Surface area measurements were made on the latter two. Adsorbate gases used were N2, A, O2 and H2O. Krypton was used for the surface area determinations. Runs were made at room and liquid nitrogen temperature in volumetric and gravimetric systems. It was found that the adsorptive/desorptive behavior was in general significantly different from that of terrestrial materials of similar type and form. Specifically (1) the UHV-stored sample exhibited very high initial adsorption indicative of high surface reactivity, and (2) the N2-stored samples at room and liquid nitrogen temperatures showed that more gas was desorbed than introduced during adsorption, indicative of gas release from the samples. The high reactivity is a scribed cosmic ray track and solar wind damage.

Grossman, J. J.↗
NASA NTRS1985

Submillimeter wave absorption of n-type InSb at low temperatures

The absorption coefficient of two high-purity n-InSb samples is measured in the 10-40 per cm range using Fourier transform spectroscopy. The absorption coefficient spectrum is presented for both samples at 4.2 K. It is also shown for the lower resistance sample cooled to 2.2 K and heated by dc bias to elevated electron gas temperatures of 7.5 and 17.9 K. ac Drude theory gives rather poor agreement with experiment at 2.2 and 4.2 K but does much better when the sample electron gas is heated. In contrast, a simple quantum mechanical theory of absorption based on inverse Bremsstrahlung yields promising agreement at the lower temperatures although its applicability is questionable. The non-Drudian absorption is shown to have a favorable effect on the performance of InSb hot-electron bolometers.

Brown, E. R.↗
NASA NTRS2003

The Search for Water and Other Volatile-bearing Phases on Mars: Mauna Kea Volcano as an Analog

Over the past 5 years, we have conducted field studies on the summit cones of Mauna Kea Volcano in Hawaii. Basaltic materials on several of these summit cones have been significantly altered by hydrothermal activity, whereas other summit cones have not undergone extensive aqueous alteration. These summit cones provide an important environment to study analogs of Martian surface alteration materials and analog surface processes (i.e., hydrothermal alteration, palagonitization. In on-going research, we have characterized the thermal and evolved gas behaviors of volatile-bearing reference minerals at reduced pressures in support of TEGA. We have expanded those studies to characterize the thermal and evolved gas behaviors of Mauna Kea samples as an analog for Mars surface materials. These samples were chosen for two reasons. First, many have chemical and spectral properties similar to what we see from remote sensing data from the Martian surface. Second, these samples have a range of mineralogical and chemical properties, ranging from simple to very complex; hence it will be challenging to characterize their thermal and evolved gas behaviors and to provide a context for their geological evolution. However, these types of studies are absolutely critical to understanding relevant geologic processes on Mars during robotic missions to the surface.

Ming, D. W.↗
NASA NTRS2003

Infrared Spectroscopy as a Chemical Fingerprinting Tool

Infrared (IR) spectroscopy is a powerful analytical tool in the chemical fingerprinting of materials. Any sample material that will interact with infrared light produces a spectrum and, although normally associated with organic materials, inorganic compounds may also be infrared active. The technique is rapid, reproducible and usually non-invasive to the sample. That it is non-invasive allows for additional characterization of the original material using other analytical techniques including thermal analysis and RAMAN spectroscopic techniques. With the appropriate accessories, the technique can be used to examine samples in liquid, solid or gas phase. Both aqueous and non-aqueous free-flowing solutions can be analyzed, as can viscous liquids such as heavy oils and greases. Solid samples of varying sizes and shapes may also be examined and with the addition of microscopic IR (microspectroscopy) capabilities, minute materials such as single fibers and threads may be analyzed. With the addition of appropriate software, microspectroscopy can be used for automated discrete point or compositional surface area mapping, with the latter providing a means to record changes in the chemical composition of a material surface over a defined area. Due to the ability to characterize gaseous samples, IR spectroscopy can also be coupled with thermal processes such as thermogravimetric (TG) analyses to provide both thermal and chemical data in a single run. In this configuration, solids (or liquids) heated in a TG analyzer undergo decomposition, with the evolving gases directed into the IR spectrometer. Thus, information is provided on the thermal properties of a material and the order in which its chemical constituents are broken down during incremental heating. Specific examples of these varied applications will be cited, with data interpretation and method limitations further discussed.

Huff, Timothy L.↗
NASA NTRS1975

A sample holding technique for study of crystal growth in silicate melts

A thin platinum wire loop is an effective way to hold silicate melts during experimentation in a gas-mixing furnace. This method results in a minimum of physical and chemical interaction between the sample and container but maximum interaction between sample and gas mixture. However, volatilization of sodium occurs while the silicate is molten. By minimizing the chance of heterogeneous nucleation, the method is ideal for experimental investigation of the origin of rock textures.

Donaldson, C. H.↗
DOE OSTI2020

A mass spectrometry-based high-throughput screening method for engineering fatty acid synthases with improved production of medium-chain fatty acids

Microbial cell factories have been extensively engineered to produce free fatty acids (FFAs), key components of crucial nutrients, soaps, industrial chemicals, and fuels. Yet, our ability to control the specificity of microbially synthesized FFAs is still limited for medium-chain fatty acids (MCFAs), which is mainly due to lack of high-throughput approaches for FFA analysis. Here we report a mass spectrometry (MS)-based method for rapid profiling of MCFAs in Saccharomyces cerevisiae by using membrane lipids as a proxy. Specially, matrix-assisted laser desorption/ionization time-of-flight (MALDI-ToF) MS was used to detect shorter acyl chain phosphatidylcholines from membrane lipids and the m/z peak ratio at 730 and 758 was used as an index for improved MCFA production. This yeast colony-based method can be performed at a rate of ~2 second per sample, which is much faster than the gold standard gas chromatography (GC)-MS (typically > 30 min per sample). To demonstrate the power of this method, we performed site-saturation mutagenesis of the yeast fatty acid synthase and identified 9 mutants that resulted in improved MCFA production relative to the wild-type strain. This colony-based MALDI-ToF MS screening method offers an alternative way for engineering microbial fatty acid compositions in a high-throughput manner.

59 BASIC BIOLOGICAL SCIENCES↗