Search NASA⌕ Search

SEARCH · Search NASA

Results for “quantitative mass spectroscopy”

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 19 records

The sublimation kinetics of GeSe single crystals

The sublimation kinetics of (001) oriented GeSe single crystal platelets was studied by high-temperature mass spectroscopy, quantitative vacuum microbalance techniques, and hot stage optical microscopy. For a mean experimental temperature of 563 K, the activation enthalpy and entropy are found to equal 32.3 kcal/mole and 19.1 eu, respectively. The vaporization coefficient is less than unity for the range of test temperatures, and decreases with increasing temperature. The combined experimental data are correlated by means of a multistep surface adsorption mechanism.

Irene, E. A.↗

Modern Material Analysis Instruments Add a New Dimension to Materials Characterization and Failure Analysis

Modern analytical tools can yield invaluable results during materials characterization and failure analysis. Scanning electron microscopes (SEMs) provide significant analytical capabilities, including angstrom-level resolution. These systems can be equipped with a silicon drift detector (SDD) for very fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations, chambers that admit large samples, variable pressure for wet samples, and quantitative analysis software to examine phases. Advanced solid-state electronics have also improved surface and bulk analysis instruments: Secondary ion mass spectroscopy (SIMS) can quantitatively determine and map light elements such as hydrogen, lithium, and boron - with their isotopes. Its high sensitivity detects impurities at parts per billion (ppb) levels. X-ray photo-electron spectroscopy (XPS) can determine oxidation states of elements, as well as identifying polymers and measuring film thicknesses on coated composites. This technique is also known as electron spectroscopy for chemical analysis (ESCA). Scanning Auger electron spectroscopy (SAM) combines surface sensitivity, spatial lateral resolution (10 nm), and depth profiling capabilities to describe elemental compositions of near and below surface regions down to the chemical state of an atom.

Panda, Binayak↗

Laboratory Instruments Available to Support Space Station Researchers at Marshall Space Flight Center

A number of research instruments are available at NASA's Marshall Space Flight Center (MSFC) to support ISS researchers and their investigations. These modern analytical tools yield valuable and sometimes new informative resulting from sample characterization. Instruments include modern scanning electron microscopes equipped with field emission guns providing analytical capabilities that include angstron-level image resolution of dry, wet and biological samples. These microscopes are also equipped with silicon drift X-ray detectors (SDD) for fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations in crystalline alloys. Sample chambers admit large samples, provide variable pressures for wet samples, and quantitative analysis software to determine phase relations. Advances in solid-state electronics have also facilitated improvements for surface chemical analysis that are successfully employed to analyze metallic materials and alloys, ceramics, slags, and organic polymers. Another analytical capability at MSFC is a mganetic sector Secondary Ion Mass Spectroscopy (SIMS) that quantitatively determines and maps light elements such as hydrogen, lithium, and boron along with their isotopes, identifies and quantifies very low level impurities even at parts per billion (ppb) levels. Still other methods available at MSFC include X-ray photo-electron spectroscopy (XPS) that can determine oxidation states of elements as well as identify polymers and measure film thicknesses on coated materials, Scanning Auger electron spectroscopy (SAM) which combines surface sensitivity, spatial lateral resolution (approximately 20 nm), and depth profiling capabilities to describe elemental compositions in near surface regions and even the chemical state of analyzed atoms. Conventional Transmission Electron Microscope (TEM) for observing internal microstructures at very high magnifications and the Electron Probe Micro-analyzer (EPMA) for very precise microanalysis are available as needed by the researcher. Space Station researchers are invited to work with MSFC in analyzing their samples using these techniques.

Panda, Binayak↗

X-ray photoelectron and mass spectroscopic study of electron irradiation and thermal stability of polytetrafluoroethylene

Polytetrafluoroethylene (PTFE) was subjected to 3 keV electron bombardment and then heated in vacuum to 300 C. The behavior of the material as a function of radiation dose and temperature was studied by X-ray photoelectron spectroscopy (XPS) of the surface and mass spectroscopy of the species evolved. A quantitative comparison of the radiation dose rate with that in other reported studies showed that, for a given total dose, the damage observed by XPS is greater for higher dose rates. Lightly damaged material heated to 300 C evolved saturated fluorocarbon species, whereas unsaturated fluorocarbon species evolved from heavily damaged material. After heating the heavily damaged material, those features in the XPS that were associated with damage diminished, giving the appearance that the radiation damage annealed. The apparent annealing of the radiation damage was found to be due to the covering of the network by saturated fragments that easily diffused through the decomposed material to the surface region upon heating.

Wheeler, Donald R.↗

Experimental Measurements of the High-Temperature Oxidation of Carbon Fibers

We carried out laboratory experiments to study the decomposition of carbon fibers at high temperature and studied the material used in charring carbon phenolic ablators for planetary probe heatshields. Porous plug samples were exposed to controlled rates of molecular oxygen, carbon dioxide, and carbon monoxide at furnace-heated flow-tube reactor temperatures between 700 and 1500 K and pressures between 2000 and 6200 Pa. We used calibrated mass spectroscopy to make time-resolved quantitative measurements of decomposition products of the gases downstream of the test sample. Absolute and differential pressure measurements were used to determine the high-temperature permeability of the material and to monitor changes during material decomposition, and we characterized the microstructure of the porous sample using scanning electron microscopy. We found substantial carbon fiber oxidation for O2 flows, resulting in increasing CO/CO2 production ratios with increasing temperature. The CO2 was shown to react with carbon fibers following a Boudouard reaction at temperatures above 1200 K.

Francesco Panerai↗

Mass loss from cool stars, facts, fads, and fallacies

The accumulation of observational material (ultraviolet spectroscopic measures, quantitative optical spectroscopy, and X-ray photometry) and its use in discerning the presence and character of mass loss across the cool half of the H-R diagram and establishing constraints on theoretical models are discussed. Analogies with closed and open solar magnetic structures are found. Two determinants of atmospheric wind structure, temperature and gravity, may suffice in a most superficial way to define the wind and atmospheric structure in a star, however it is apparent that there is still a missing parameter which may stem from magnetic activity and its particular configuration. Theories that appear successful in reproducing observed line profiles, wind temperatures, and terminal velocities incorporate Alfven wave heating and momentum deposition. Successive observations of an active binary (lambda and G8III-IV) and a supergiant star, alpha Aqr (G2 Ib) revealed that magnetic activity and perhaps mass loss occur on restricted regions of a stellar surface and that long-term structures are present in the wind. These phenomena are present in the solar atmosphere and wind and may be considered a general characteristic of stellar winds.

Dupree, A. K.↗

Method for the Collection, Gravimetric and Chemical Analysis of Nonvolatile Residue (NVR) on Surfaces

Nonvolatile residue (NVR), sometimes referred to as molecular contamination is the term used for the total composition of the inorganic and high boiling point organic components in particulates and molecular films deposited on critical surfaces surrounding space structures, with the particulate and NVR contamination originating primarily from pre-launch operations. The "nonvolatile" suggestion from the terminology NVR implies that the collected residue will not experience much loss under ambient conditions. NVR has been shown to have a dramatic impact on the ability to perform optical measurements from platforms based in space. Such contaminants can be detected early by the controlled application of various detection techniques and contamination analyses. Contamination analyses are the techniques used to determine if materials, components, and subsystems can be expected to meet the performance requirements of a system. Of particular concern is the quantity of NVR contaminants that might be deposited on critical payload surfaces from these sources. Subsequent chemical analysis of the contaminant samples by infrared spectroscopy and gas chromatography mass spectrometry identifies the components, gives semi-quantitative estimates of contaminant thickness, indicates possible sources of the NVR, and provides guidance for effective cleanup procedures. In this report, a method for the collection and determination of the mass of NVR was generated by the authors at NASA Langley Research Center. This report describes the method developed and implemented for collecting NVR contaminants, and procedures for gravimetric and chemical analysis of the residue obtained. The result of this NVR analysis collaboration will help pave the way for Langley's ability to certify flight hardware outgassing requirements in support of flight projects such as Stratospheric Aerosol and Gas Experiment III (SAGE III), Clouds and the Earth's Radiant Energy System (CERES), Materials International Space Station Experiment - X (MISSE-X), and Doppler Aerosol Wind Lidar (DAWN).

Gordon, Keith↗

Results of special mechanical analyses of Luna 16 material

The studies carried out on the Luna 16 regolith have confirmed the data that were already published internationally. By means of activation analysis under irradiation in the reactor, activation analysis with a 14 MeV U-generator, and mass spectroscopy on samples of 10 or 20 mg, six main and 63 trace elements were quantitatively determined and compared with known data.

Stiller, H.↗

Compensation mechanism in liquid encapsulated Czochralski GaAs Importance of melt stoichiometry

It is shown that the key to reproducible growth of undoped semi-insulating GaAs by the liquid encapsulated Czochralski (LEC) technique is the control over the melt stoichiometry. Twelve crystals were grown from stoichiometric and nonstoichiometric melts. The material was characterized by secondary ion mass spectrometry, localized vibrational mode far infrared spectroscopy, Hall-effect measurements, optical absorption, and photoluminescence. A quantitative model for the compensation mechanism in the semi-insulating material was developed based on these measurements. The free carrier concentration is controlled by the balance between EL2 deep donors and carbon acceptors; furthermore, the incorporation of EL2 is controlled by the melt stoichiometry, increasing as the As atom fraction in the melt increases. As a result, semi-insulating material can be grown only from melts above a critical As composition. The practical significance of these results is discussed in terms of achieving high yield and reproducibility in the crystal growth process.

Holmes, D. E.↗

Observation of winds in cool stars

Sufficient observational material - ultraviolet spectroscopic measures, quantitative optical spectroscopy, and X-ray photometry exists to enable discernment of the presence and character of mass loss in cool stars and to establish meaningful constraints on theoretical models. Two determinants of atmospheric wind structure - temperature and gravity - may suffice in a most superficial way to define the wind and atmospheric structure in a star; however more extensive observations demonstrate the importance of magnetic surface activity and its particular geometrical configuration. Successive observations of an active binary system and a supergiant star reveal that magnetic activity and perhaps mass loss occur on restricted regions of a stellar surface and that long lived structures are present in a wind.

Dupree, A. K.↗

Spatially resolved quantitative spectroscopy of comets

The pristine nucleus of a comet, in particular, its chemical composition is studied. More immediate goals are to quantitatively compare the mass-loss-rates of various periodic comets, and to map out the distribution of coma region ions and neutral radicals with the hope of indirectly determining their parent molecules.

Spinrad, H.↗

Non-intrusive flow measurements on a reentry vehicle

This study evaluates the utility of various non-intrusive techniques for the measurement of the flow field on the windward side of the Space Shuttle or a similar re-entry vehicle. Included are linear (Rayleigh, Raman, Mie, Laser Doppler Velocimetry, Resonant Doppler Velocimetry) and nonlinear (Coherent Anti-Stokes Raman, Laser Induced Fluorescence) light scattering, electron beam fluorescence, thermal emission and mass spectroscopy. Flow field properties are taken from a nonequilibrium flow model by Shinn, Moss and Simmonds at NASA Langley. Conclusions are, when possible, based on quantitative scaling of known laboratory results to the conditions projected. Detailed discussion with researchers in the field contributed further to these conclusions and provided valuable insights regarding the experimental feasibility of each of the techniques.

Miles, R. B.↗

Evaluation of non-intrusive flow measurement techniques for a re-entry flight experiment

This study evaluates various non-intrusive techniques for the measurement of the flow field on the windward side of the Space Shuttle orbiter or a similar reentry vehicle. Included are linear (Rayleigh, Raman, Mie, Laser Doppler Velocimetry, Resonant Doppler Velocimetry) and nonlinear (Coherent Anti-Stokes Raman, Laser-Induced Fluorescence) light scattering, electron-beam fluorescence, thermal emission, and mass spectroscopy. Flow-field properties were taken from a nonequilibrium flow model by Shinn, Moss, and Simmonds at the NASA Langley Research Center. Conclusions are, when possible, based on quantitative scaling of known laboratory results to the conditions projected. Detailed discussion with researchers in the field contributed further to these conclusions and provided valuable insights regarding the experimental feasibility of each of the techniques.

Miles, R. B.↗

Interpretation of discrepancies in mass spectroscopy data obtained from different experimental configurations

Many helium mass spectrometer leak detectors at KSC employ sampling systems that feature hand held sniffer probes. Authors of general leakage-testing literature recommend sniffer probes for leak location but not for quantitative leakage measurement. Their use in the latter application at KSC involves assumptions that may be subtle. The purpose of the research effort reported herein was to establish the significance of indicated leak rates displayed by sniffer-probe equipped leak detectors and to determine whether the use of alternative hardware or testing procedures may reduce the uncertainty of leakage measurements made with them. The report classifies probe-type sampling systems for helium leak detectors according to their internal plumbing (direct or branched), presents a basic analysis of the fluid dynamics in the sampling system in the branched-conduit case, describes the usual test method for measuring the internal supply-to-sample flowrate ratio (a.k.a permeation ratio), and describes a concept for a sponge-tipped probe whose external supply-to-sample flowrate ratio promises to be lower than that of a simple-ended probe. One conclusion is that the main source of uncertainty in the use of probe-type sampling systems for leakage measurement is uncertainty in the external supply-to-sample flowrate ratio. In contrast, the present method for measuring the internal supply-to-sample flowrate ratio is quantitative and satisfactory. The implication is that probes of lower external supply-to-sample flowrate ratio must be developed before this uncertainty may be reduced significantly.

Russell, John M.↗

Quantitative UV spectroscopy of early O stars on the Magellanic Clouds: The determination of the stellar metallicities

Ultraviolet spectra of four O stars in the Magellanic Clouds obtained with the faint object spectrograph of the Hubble Space Telescope are analyzed with respect to their metallicity. The metal abundances are derived from the stellar parameters and the mass loss rate with a two step procedure: hydrodynamic radiation-driven wind models with metallicity as a free parameter are constructed to fit the observed wind momentum rate and thus yield a dynamical metallicity, and synthetic spectra are computed for different metal abundances and compared to the observed spectra in order to obtain a spectroscopic metallicity.

Haser, Stefan M.↗

First results from the Goddard High-Resolution Spectrograph - Spectroscopic determination of stellar parameters of Melnick 42, an O3f star in the Large Magellanic Cloud

GHRS and optical (ESO 3.6 m) observations of the O3f star Melnick 42 in the 30 Doradus complex are reported. A first analysis reveals that with a luminosity of 2.3 million L(solar) and a present mass of 100 M(solar), Melnick 42 is one of the most luminous and massive stars known. An estimate of abundances indicates that iron and oxygen are very likely reduced by a factor of four relative to the sun, whereas carbon is more strongly depleted and nitrogen is approximately solar. The terminal velocity of the stellar wind is 3000 km/s. The mass-loss rate is 4 x 10 to the -6th M(solar)/yr, with a large uncertainty. The excellent quality GHRS spectrum taken in a crowded region of the LMC demonstrates the superiority of the HST for quantitative ultraviolet spectroscopy of hot stars in other galaxies.

Heap, S. R.↗

Trace Elemental Abundances in Calcium-Aluminum-Rich Inclusions in CV Chondrites

Introduction: Calcium-aluminum-rich inclusions (CAIs), are the first formed solids that define the age of the Solar System [1,2]. CAIs are thought to have condensed from nebular gas [3,4] within the first <1 Ma of Solar System formation [5,6]. CAIs have experienced numerous early Solar System processes including condensation, evaporation, melting, recrystallization, and aqueous alteration [e.g., 7]. The chemical, mineralogical, and textural diversity among CAIs results from a range of chemical and physical processes recorded during nebular and parent body epoch. This study aims to explore the mineralogical, textural, and chemical compositions of CAIs including the trace elemental abundances in CAI phases to determine the early Solar System processes recorded in them. Samples and Analytical Methods: We analyzed one CAI each from CV3 chondrites Northwest Africa (NWA) 5508 designated as ‘Saguaro’, and Northwest Africa (NWA) 12772 designated as ‘Hoopoe’. Back-scatter electron (BSE) images were collected using a Phenom XL scanning electron microscope (SEM) at the Lunar and Planetary Institute (LPI) and the JEOL JXA-8530F electron probe microanalyzer (EPMA) at Johnson Space Center (JSC)-NASA. Additionally, energy dispersive X-ray spectrometry (EDS) elemental maps of select areas for these samples were collected using a 15.0kV beam energy and a 40µA emission current. Using the EPMA, wavelength-dispersive X-ray spectroscopy (WDS) quantitative data were collected. In-situ trace element measurements for both CAIs were determined at JSC-NASA using a Photon Machines 193nm laser ablation system and a Thermo-Scientific Element-XR inductively coupled plasma mass spectrometer (ICP-MS). Analyses consisted of 30s ablations at 10Hz, spot sizes of 20-25µm, and a fluence of 6.0 J/cm2 for anorthite and melilite, and a 3.5 J/cm2 fluence for all other phases. NIST612 was used to correct for instrument drift, while BHVO-2g was used as a primary calibration standard. BCR-2g and in-house mineral standards were regularly measured as unknowns to ensure accuracy. Results: Saguaro is a coarse-grained CAI, ~11 x 6 mm in dimensions. Saguaro contains spinel, Al-rich pyroxene, anorthite, Mg-rich melilite, and minor perovskite in its interior and is therefore classified as a Type B CAI. Individual melilite grains shows normal compositional zoning with an Ak content ranging from ~24 to 54 with no apparent trend from the core to the edge of the CAI. The spinel appears euhedral and occurs both as clusters and as spinel palisades [8]. Two rim sequences surround most of the sample: the inner rim being a Wark-Lovering (WL) rim (~10-35 µm) containing pyroxene, spinel, and melilite (or anorthite), and the outer rim is a finer-grained, thicker (~100 µm), accretionary rim (Fig. 1). The mineral phases in Saguaro record an overall flat REE pattern with an average negative Eu anomaly in pyroxene, and an average positive Eu anomaly in anorthite and melilite respectively. Anorthite, melilite, and pyroxene have a minor depletion in Tm (Fig. 2). The Hoopoe CAI is a compact, coarse-grained ~6 × 4 mm in size. The major mineralogy includes hibonite, spinel, melilite, anorthite, and perovskite. Therefore, it is classified as a compact transitional type A and B. (?)zoning was observed in some hibonites. Individual melilite grains show both reverse and normal zoning, where the Ak content ranges from ~6- to 28. Melilite shows two distinct textures. One texture consisted of smooth melilite that appeared homogenous, while the second appeared to consist of many fine fractures. The spinel also often appears clustered. The WL-rim sequence surrounding Hoopoe is ~25 µm thick and composed of spinel, perovskite, hibonite, and melilite/anorthite. It is then partially surrounded by an outer accretionary rim (~75µm). Like before, refractory metal nuggets appeared concentrated near the WL rims. Other metal assemblages rich in Fe and Ni were also observed. All major mineral phases in Hoopoe display relatively flat REE patterns, except for varying Eu and Tm between phases (Fig. 2). There is a prominent negative Eu anomaly in perovskite and an average positive Eu anomaly in spinel, anorthite, and hibonite respectively (Fig. 2, 3). The mixed phases along the rim of the CAI also display a negative Eu anomaly, and all phases the CAI were depleted in Pb. Discussion: The CV3 CAIs analyzed in this study were classified based on their mineralogy and textures into Type A versus Type B CAIs [10]. Hibonite appears to be pseudomorphically replacing the spinel, (i.e., is hibonite in composition, but appears in the shape of spinel). Spinel palisades. The presence of spinel palisades present in Saguaro are consistent with the melting and recrystallization experienced by this CAI. Trace elemental analyses. Saguaro and Hoopoe display similar trace element patterns to each other, with both appearing generally flat, with anomalies in Eu, and Tm. Melilite and anorthite display positive Eu anomalies in both CAIs, in addition to the hibonite in Hoopoe (Fig. 2). The phases that are depleted in Eu are pyroxene and perovskite in both Saguaro and Hoopoe, respectively (Fig. 3). Given that Eu is volatile in reducing environments [11], this could possibly indicate reducing conditions at the time anorthite and melilite crystallized, with the gas they formed from containing Eu. As these CAIs continued to form, this gas as a result would become depleted in Eu. This also could be supported by the propensity of anorthite and melilite to take up Eu from its surroundings and incorporate it into their structure [12]. In addition, analyzing the assemblage of the phases in the Saguaro, melilite and anorthite (Eu enriched) often surround the pyroxene (Eu depleted) as they are crystallized. This intergrowth of phases and the proximity of the phases would support that the Eu is being incorporated into some phases, preventing it from incorporating into other. Trace elemental analyses of the CAI rims will be evaluated in more detail, as they are complicated by the transient signal being composed of a mixture of mineral phases. Broadly, however, the patterns in the rims of both CAIs are comparable to each other, and for Hoopoe, to the mixed phase patterns in the core (Fig. 3). Other studies have found that CAI rims can be depleted in Ce and Yb [13], however we did not observe these anomalies in the two CAIs discussed here. Given their similarity, the trace elemental analyses of the mixed interior (i.e. core) and rim phases could be interpreted as forming from similar, if not the same, reservoirs. The REE abundance between the rim and core of Hoopoe are also similar, indicating they may have formed from a gas of the same or similar composition. Acknowledgments: We thank the ASU Center for Meteorite Studies for loaning the samples used in this work and Tabb Prissel for his assistance with the analysis. Mouti Al-Hashimi thanks Sam Crossley and Cyrena Goodrich for their help with the LPI SEM training. This work was supported by the LPI Summer Intern Program in Planetary Science and the LPI Cooperative Agreement. References: [1] Connelly J.N. (2012) Science, 338, 651-655. [2] MacPherson G. J. (2014) Treatise on Geochem., 2, 139-179. [3] Grossman L. (1972) GCA, 36, 597-619. [4] Ebel, D.S. (2006) Meteorites and the Early Solar System II (D. S. Lauretta & H. Y. McSween, Eds.) 253-277. [5] MacPherson G. J. (2012) Earth Planet. Sci. Lett., 331-332, 43-54. [6] MacPherson G.J. (2017) GCA, 201, 65-82. [7] Krot A.N. (1995) Meteoritics & Planet. Sci., 30, 748-775. [8] Wark and Lovering (1982) GCA, 46, 2595-2607. [9] Palme H. and Jones A. (2003) Treatise on Geochemistry (H. D. Holland and K. K. Turekian Eds.), 1, 41-61. [10] Grossman L. (1980) Ann. Rev. Earth Planet. Sci., 8, 559-608. [11] Floss C. et al. (1996) GCA, 60, 1975-1997. [12] Mason B. and Martin P. M. (1974) Earth Planet. Sci. Lett., 22, 141-144. [13] Wark B. and Boynton W. V. (2001) Meteoritics & Planet. Sci., 36, 1135-1166.

X Mouti↗