Search NASA⌕ Search

SEARCH · Search NASA

Results for “energy-dispersive X-ray spectrometer”

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
All sourcesNASA NTRSDOE OSTI
NASA NTRS1985

Hypervelocity impacts on Skylab 4/Apollo windows

The three largest Skylab 4 Command Module windows that were exposed for 84 days to space were optically scanned for impact features as small as 30 microns in diameter. This scanning effort which was carried out at an opptical magnification of 35x, detected features approximately three times smaller than were found in the original 5x scanning effort over the entire window surface. Some 289 features were recorded from the 35x scan for later detailed analyses. Sixty of the largest and most promising features were cored from the windows for SEM and energy-dispersive X-ray spectrometer (EDS) analysis. Twenty-six of the cores contained craters with glassy pits, and of these, fourteen were found to contain strikingly obvious liners coating the interior of the glassy pit. The six largest features cored from the windows do not have a central glassy pit which leaves their previously reported hypervelocity origin in some doubt. The remaining twenty-eight features that were cored from the windows show no clear evidence for a hypervelocity origin and evidence available at this time is insufficient to identify an origin in Earth orbit or as ground damage. The EDS analysis of six of the seven liners that were examined show detectable aluminum in the liner or lip of the glassy pit. The source of aluminum is most probably an Earth orbiting population of aluminum oxide spherules, exhaust from solid rocket motors.

Clanton, U. S.↗
NASA NTRS1985

Survey of probable micrometer-sized Earth-orbital debris fragments in the NASA-JSC cosmic dust sample collection

A program to collect extraterrestrial dust samples from the stratosphere using impactors mounted on NASA U-2 and WB-57F aircraft is discussed. Sample collection, preparation, and analysis techniques are described and the particle types found are reviewed. Preliminary examination of the particles indicates that they represent not only extraterrestrial material, but some fraction of terrestrial contamination from both natural and manmade sources. This examination involves a combination of optical microscopy, scanning electron microscopy (SEM) and qualitative bulk elemental analysis using an energy-dispersive X-ray spectrometer (EDS) to characterize each particle. The cosmic dust collection contains samples of at least three classes of material that may present some hazard to extended spacecraft operations in near-Earth orbit: (1) micrometeorites/cosmic dust, (2) aluminum oxide spheres, and (3) alloy spherules and fragments.

Clanton, U. S.↗
NASA NTRS2005

High-Resolution Electron Energy-Loss Spectroscopy (HREELS) Using a Monochromated TEM/STEM

A 200 keV FEI TF20 XT monochromated (scanning) transmission electron microscope funded by NASA's SRLIDAP program is undergoing installation at Lawrence Livermore National Laboratory. Instrument specifications in STEM mode are Cs =1.0 mm, Cc =1.2 mm, image resolution =0.18 nm, and in TEM mode Cs =1.3 mm, Cc =1.3 mm, information limit =0.14 nm. Key features of the instrument are a voltage-stabilized high tension (HT) supply, a monochromator, a high-resolution electron energy-loss spectrometer/energy filter, a high-resolution annular darkfield detector, and a solid-state x-ray energy-dispersive spectrometer. The high-tension tank contains additional sections for 60Hz and high frequency filtering, resulting in an operating voltage of 200 kV plus or minus 0.005V, a greater than 10-fold improvement over earlier systems. The monochromator is a single Wien filter design. The energy filter is a Gatan model 866 Tridiem-ERS high resolution GIF spec d for less than or equal to 0.15 eV energy resolution with 29 pA of current in a 2 nm diameter probe. 0.13 eV has already been achieved during early installation. The x-ray detector (EDAX/Genesis 4000) has a take-off angle of 20 degrees, an active area of 30 square millimeters, and a solid angle of 0.3 steradians. The higher solid angle is possible because the objective pole-piece allows the detector to be positioned as close as 9.47 mm from the specimen. The voltage-stabilized HT supply, monochromator and GIF enable high-resolution electron energy-loss spectroscopy (HREELS) with energy resolution comparable to synchrotron XANES, but with approximately 100X better spatial resolution. The region between 0 and 100 eV is called the low-loss or valence electron energy-loss spectroscopy (VEELS) region where features due to collective plasma oscillations and single electron transitions of valence electrons are observed. Most of the low-loss VEELS features we are detecting are being observed for the first time in IDPs. A major focus of our research is to understand the origin and significance of these features and how they might be exploited to gain insight about IDPs and other meteoritic materials.

Sai, Z. R.↗
NASA NTRS2013

Microchemical and Structural Evidence for Space Weathering in Soils from Asteroid Itokawa

The chemistry, microstructure and optical properties of grains on the surfaces of airless bodies are continu-ously modified due to their interactions predominantly with solar energetic ions and micrometeorite impacts. Collectively known as space weathering, this phenomenon results in a discrepancy between remotely sensed spectra from asteroids and those ac-quired directly from meteorites. The return of pristine samples from the asteroid Itokawa provides insight into surface processes on airless bodies and will help in correlating remote sensing data with laboratory analysis of meteorites. Samples and Methods: We examined Itokawa samples RA-QD02-0042-01 and RA-QD-02-0042-02, ultramicrotomed sec-tions of a singular grain prepared by the Hayabusa sample cura-tion team. We analyzed these slices using a 200 keV JEOL 2010F transmission electron microscope (TEM) at Arizona State Uni-versity and a 200 keV JEOL 2500SE TEM at NASA JSC. Both field emission TEMs are equipped with energy-dispersive X-ray spectrometers (EDS) and scanning TEM (STEM) detectors. Results and Discussion: TEM observations reveal that the sectioned grain predominantly consists of a single crystal of low-Ca orthopyroxene, with subsidiary smaller regions of olivine, Fe-Ni sulfide, and Fe-Ni metal. EDS-spectrum imaging and high-resolution TEM (HRTEM) show local, nanocrystalline regions of the outermost 2 to 5 nm of the pyroxene are composed of an Fe-Mg-S-rich and Si- and O-depleted layer that is underlain by a 2- to 5-nm thick amorphous zone enriched in Si. These layers occur in multiple microtome slices and have uniform thicknesses. We also observe localized 'islands' of material on the surface of the pyroxene which HRTEM imaging indicates are amorphous and EDS measurements show are compositionally heterogeneous. A 10- to 60-nm thick partially amorphous zone occurs below the compositionally distinct rim. While this this zone is associated with the compositionally heterogeneous outer layer, it also occurs as a local stand-alone feature on the exterior rim of the grain. Ar-eas of the pyroxene grain rim also exhibit a vesicular texture. The TEM data indicate a complex history of space weather-ing for samples RA-QD02-0042-01 and -02. The outermost layer of nanocrystalline material with varied composition is consistent with previously suggested [3-4] chemical and structural pro-cessing by solar wind ions, with a possible additional role for im-pact vapor deposition [3-4]. The amorphous and compositionally distinct islands on the surface of this grain, similar to lunar glasses, suggest formation through vapor deposition via micrometeor-ite impact events. In comparison, the amorphization and vesicula-tion textures are likely a product of radiation damage from the solar wind. The depth and degree of amorphization, in conjunction with model calculations, will help provide an upper limit on exposure time for these particles.

Thompson, M. S.↗
NASA NTRS2014

Space Weathering of Olivine in Lunar Soils: A Comparison to Itokawa Regolith Samples

Regolith particles from airless bodies preserve a record of the space weathering processes that occurred during their surface exposure history. These processes have major implications for interpreting remote-sensing data from airless bodies. Solar wind irradiation effects occur in the rims of exposed grains, and impact processes result in the accumulation of vapordeposited elements and other surface-adhering materials. The grains returned from the surface of Itokawa by the Hayabusa mission allow the space weathering "style" of a chondritic, asteroidal "soil" to be compared to the lunar case. Here, we present new studies of space-weathered olivine grains from lunar soils, and compare these results to olivine grains from Itokawa. Samples and Methods: We analyzed microtome thin sections of olivine grains from the 20-45 micron fractions of three lunar soils: 71061, 71501 and 10084 (immature, submature and mature, respectively). Imaging and analytical data were obtained using a JEOL 2500SE 200kV field-emission scanning-transmission electron microscope equipped with a thin-window energy-dispersive x-ray spectrometer. Similar analyses were obtained from three Hayabusa olivine grains. Results and Discussion: We observed lunar grains showing a range of solar flare track densities (from <10(exp 9) to approx.10(exp 12)/sq cm). The lunar olivines all show disordered, highly strained, nanocrystalline rims up to 150-nm thick. The disordered rim thickness is positively correlated with solar flare track density. All of the disordered rims are overlain by a Si-rich amorphous layer, ranging up to 50-nm thick, enriched in elements that are not derived from the host olivine (e.g., Ca, Al, and Ti). The outmost layer represents impact-generated vapor deposits typically observed on other lunar soil grains. The Hayabusa olivine grains show track densities <10(exp 10)/sq cm and display disordered rims 50- to 100-nm thick. The track densities are intermediate to those observed in olivines in immature and submature lunar soils and indicate surface exposures of approx. 10(exp 5) years. The outermost few nanometers of the disordered rims on Hayabusa olivines are more Si-rich and Mg- and Fe-depleted relative to the cores of the grains and likely represent a minor accumulation of impact-generated vapors or sputter deposits. Nanophase Fe metal particles are less abundant in the Hayabusa rims compared to the rims on lunar grains. Conclusions: The Hayabusa and lunar olivine grain rims have widths and microstructures consistent with formation from atomic displacement damage from solar wind ions. The space weathering features in the Hayabusa grains are similar to those observed in olivines from immature to submature lunar soils. A major difference, however, is that the Hayabusa grains appear to lack the hypervelocity impact products (melt spherules, thick vapor deposits, and abundant nanophase Fe metal particles) that are common in lunar soil grains with a similar exposure history.

Keller, L. P.↗
NASA NTRSDate not supplied

Applicability of Micro X-Ray Fluorescence Spectroscopy to Astromaterials Curation and Research

Introduction: The Astromaterials Acquisition and Curation Office at NASA’s Johnson Space Center (JSC) curates NASA’s astromaterial sample collections which includes: Apollo samples, Luna samples, Ant-arctic meteorites, cosmic dust particles, microparticle impacts into space-flown materials, Genesis solar wind atoms, Stardust comet Wild-2 particles, Stardust inter-stellar particles, Hayabusa asteroid Itokawa particles, Hayabusa 2 asteroid Ryugu particles, and future OSIRIS-Rex asteroid Bennu particles (landing in Sep-tember, 2023) [1–3]. To enhance JSC’s advanced cu-ration capabilities, we have recently installed a high-performance micro-X-ray fluorescence (µXRF) spec-trometer to assist in sample characterization through rapid, non-destructive, in-situ elemental analyses that do not require the sample preparation protocols (i.e., polishing and carbon-coating) commonly needed for electron beam analyses. With this new instrument, we are capable of detecting all elements down to carbon in a variable-pressure or He-purged chamber for anal-ysis of a wide range of sample types. Here we describe the instrumental set-up, capabilities, and applicability of µXRF analysis to astromaterials curation and re-search. Instrumentation and Methodology: The X-ray fluorescence and computed tomography lab (X-FaCT) lab at JSC is now equipped with a Bruker M4 Tornado Plus µXRF (Fig. 1). This system is an energy-dispersive x-ray spectrometer equipped with two 60 mm2 silicon drift detectors (SDD) that are able to be used simulta-neously for output count rates ~500,000 cps. New light element windows allow detecting and analyzing the entire elemental range from carbon to americium. Two x-ray tubes (micro-focus Rh with polycapillary lenses and W with collimators of 0.5, 1.0, 2.0, and 4.5 mm) with max excitation parameters of 50 kV, 30 W and 50 kV, 40 W, respectively, allow for more flexibility of the analysis of high energy lines. The motorized X-Y-Z stage has a mapping range of 190 x 160 mm and can support samples up to 7 kg (~15.5 lbs) and a height of 120 mm [4]. Analytical modes include elemental analysis (down to ~20 µm spot size) via point, line, or area of bulk materials (rock surfaces, thin sections, thick sections, etc.) as well as coating analysis (determination of thickness and composition) of samples. This system has a variable vacuum chamber (1 mbar to 1 atm) that is also equipped with a He-purge system which accommodates vacuum sensitive samples while still allowing detection of light elements at atmospheric pressure. Utility and Applicability of µXRF in Astro-materials research and exploration science (ARES): Elemental analysis using µXRF is commonly em-ployed for both terrestrial and planetary geological science disciplines [5]. It is especially useful for analy-sis of astromaterials given the limited sample prepara-tion required, which is not feasible for certain materi-als. Here we show select applications of µXRF anal-yses of astromaterials that can, have, and will be done at JSC’s X-FaCT lab. Point analysis: In-situ spot analyses (~20 µm spot size) on a cut slab of Martian meteorite NWA 10922 allowed for the discovery, qualitative elemental analy-sis and determination of different feldspar minerals [6]. These point analyses served as an effective prelim-inary step for subsequent quantitative analyses. Ana-lytical standards can be employed for more accurate quantification of µXRF spot analyses. Area analysis: This analytical mode measures all detectable elements (from C to Am) at each pixel (>5 µm pixel size) in a user-defined area. The results are shown as elemental maps which can be extracted as 16-bit TIFF’s for further data processing. In Fig. 2. we show elemental distribution maps of the high-Ti basalt 73001,531 that have been processed using ImageJ software. From these maps you can accurately and quickly (this map took ~50 mins.) identify mineral components, such as pyroxene, plagioclase, oxides, and phosphates, compositional zoning, and mineral textures. Detection of high-Z phases: µXRF techniques are es-pecially effective at analyzing trace minerals with high-atomic-number (high-Z) elements because the high-energy characteristic X-rays used (relative to SEM EDS) allow for mapping of K lines in elements up to La (typically SEM maps use L X-ray lines for elements >Zn, and these can often have interferences). Thus, µXRF is especially suited for identifying minerals like zircon, baddeleyite, REE-rich phosphates, Fe-rich met-als, oxides, sulfides, and phosphides [4]. In Fig. 3 we show elemental distribution maps for 73001,530 where we are able to correlate the original video image with, Zr, Si, Y and Hf elemental maps together identi-fying the location of a zircon. In this location you would expect lower Si compared to surrounding mate-rial, as well as higher Zr, Y, and Hf content compared to surrounding material, all of which is confirmed by our XRF ele-mental distribution maps (Figure 2.) Conclusions: The new M4 Tornado Plus µXRF within the Astromaterials Acquisition and Curation office at NASA JSC allows for rapid and non-destructive elemental analysis of astromaterials with limited or no sample preparation. µXRF analyses pro-vide crucial compositional knowledge for the prelimi-nary examination and curation of astromaterials. This instrument enhances the advanced curation capabili-ties in the X-FaCT laboratory at JSC by allowing pro-ductive, cohesive, and non-destructive multi-modal x-ray analyses on astromaterial samples, which is neces-sary for the comprehensive curation and study of our current and future astromaterial collections. Addition-ally, µXRF can provide complimentary information to researchers for studies on astromaterials. References: [1] Allen, C. et al., (2011). Chemie De Erde Geochemistry, 71, 1-20. [2] McCubbin, F. M. et al., (2016) 47th LPSC, abstract #2668 [3] Zeigler, R. A. et al., (2017) 48th LPSC, abstract #2772 [4] Bruker User Manual [5] Young et al., (2016) Appl. Geochemistry, 72, 77-87 [6] Mor-ris, R. V. et al., (2023) 54th LPSC.

E W O'Neal↗
NASA NTRS1973

Inorganic chemical investigation by X-ray fluorescence analysis - The Viking Mars Lander

The inorganic chemical investigation experiment added in August 1972 to the Viking Lander scientific package uses an energy-dispersive X-ray fluorescence spectrometer in which four sealed, gas-filled proportional counters detect X-rays emitted from samples of the Martian surface materials irradiated by X-rays from radioisotope sources (Fe-55 and Cd-109). The instrument is inside the Lander body, and samples are to be delivered to it by the Viking Lander Surface Sampler. Instrument design is described along with details of the data processing and analysis procedures. The results of the investigation will characterize the surface materials of Mars as to elemental composition with accuracies ranging from a few tens of parts per million (at the trace-element level) to a few per cent (for major elements) depending on the element in question.

Toulmin, P., III↗
NASA NTRS1999

Space Weathering in the Fine Size Fractions of Lunar Soils: Soil Maturity Effects

The effects of space weathering on the optical properties of lunar materials have been well documented. These effects include a reddened continuum slope, lowered albedo, and attenuated absorption features in reflectance spectra of lunar soils as compared to finely comminuted rocks from the same Apollo sites. However, the regolith processes that cause these effects are not well known, nor is the petrographic setting of the products of these processes fully understood. A Lunar Soil Characterization Consortium has been formed with the purpose of systematically integrating chemical and mineralogical data with the optical properties of lunar soils. Understanding space-weathering effects is critical in order to fully integrate the lunar sample collection with remotely-sensed data from recent robotic missions (e.g., Lunar Prospector, Clementine, and Galileo) We have shown that depositional processes (condensation of impact-derived vapors, sputter deposits, accreted impact material, e.g., splash glass, spherules, etc.) are a major factor in the modification of the optical surfaces of lunar regolith materials. In mature soils, it is the size and distribution of the nanophase metal in the soil grains that has the major effect on optical properties. In this report, we compare and contrast the space-weathering effects in an immature and a mature soil with similar elemental compositions. For this study, we analyzed <10 micron sieve fractions of two Apollo 17 soils, 79221 (mature, Is/FeO = 81) and 71061 (immature, Is/FeO = 14). Details of the sieving procedures and allocation scheme are given else where. The results of other detailed chemical, mineralogical, and spectroscopic analyses of these soil samples are reported elsewhere. A representative sample of each soil was embedded in low-viscosity epoxy, and thin sections (about 70nm thick) were obtained through ultra microtomy. The thin sections used for these analyses typically contained cross sections of up to 500 individual grains. The thin sections were studied using a JEOL 2010 transmission electron microscope (TEM) equipped with a thin window energy-dispersive X-ray (EDX) spectrometer. An individual thin section was selected from each soil, and for each grain in the section we determined (1) the elemental composition by EDX; (2) whether the grain was crystalline or glassy using electron diffraction and darkfield imaging; (3) the presence or absence of rims and accreted material; and (4) the distribution of nanophase Fe where present. Most of the categories are self-evident; however, we divide the agglutinate derived material into agglutinitic glass (glass with approximately the same composition as the bulk soil that contains nanophase Fe with or without vesicles) and agglutinate fragments, which are composed of crystalline grains and agglutinitic glass. Lithic fragments are defined as polymineralic grains with no glass. Pyroxene grains have been divided into high- and low-Ca groups. As expected, there are a number of differences in the petrography of the <10-microns fractions of 79221 and 71061 given the great difference in their respective maturities, but we focus here on two major distinctions: agglutinate content and the number of grains with micropatina. Slightly over 50% of the particles in 79221 consist of agglutinitic glass and agglutinate fragments, while the remainder are predominantly crystalline mineral grains. The agglutinic glass particles contain abundant nanophase Fe and vesicles. Angular particles are rare, with most showing smooth, rounded exteriors, Of the mineral grains analyzed thus far, over 90% of the grains have amorphous rims that contain nanophase Fe (these rims are believed to have formed by vapor deposition and irradiation effects). The nanophase Fe in these rims probably accounts for a significant fraction of the increase in Is/FeO measured in these size fractions. In addition to the rims, the majority of particles also show abundant accreted material in the form of glass splashes and spherules that also contain nanophase Fe. In stark contrast, the surfaces of the mineral grains in the 71061 sample are relatively prisitine, as only about 14% of the mineral grains in the sample exhibited amorphous rims. Furthermore, the mineral particles are more angular and show greater surface roughness than in the mature sample. Accreted material on particle surfaces is rare. Agglutinitic material is a major component of the 71061 sample; however, nanophase Fe and vesicles are not as well developed as in the 79221 sample. It is now recognized that nanophase Fe is probably the main agent in modifying the optical properties of lunar soil grains. The most important result of this study is the observation that in the fine size fractions of mature soils, nearly every grain has nanophase Fe within 100 run of the particle surface. (Additional Information contained in original)

Keller, L. P.↗
NASA NTRS2013

Transmission Electron Microscopy of Itokawa Regolith Grains

Introduction: In a remarkable engineering achievement, the JAXA space agency successfully recovered the Hayabusa space-craft in June 2010, following a non-optimal encounter and sur-face sampling mission to asteroid 25143 Itokawa. These are the first direct samples ever obtained and returned from the surface of an asteroid. The Hayabusa samples thus present a special op-portunity to directly investigate the evolution of asteroidal sur-faces, from the development of the regolith to the study of the effects of space weathering. Here we report on our preliminary TEM measurements on two Itokawa samples. Methods: We were allocated particles RA-QD02-0125 and RA-QD02-0211. Both particles were embedded in low viscosity epoxy and thin sections were prepared using ultramicrotomy. High resolution images and electron diffraction data were ob-tained using a JEOL 2500SE 200 kV field-emission scanning-transmission electron microscope. Quantitative maps and anal-yses were obtained using a Thermo thin-window energy-dispersive x-ray (EDX) spectrometer. Results: Both particles are olivine-rich (Fo70) with μm-sized inclusions of FeS and have microstructurally complex rims. Par-ticle RA-QD02-0125 is rounded and has numerous sub-μm grains attached to its surface including FeS, albite, olivine, and rare melt droplets. Solar flare tracks have not been observed, but the particle is surrounded by a continuous ~50 nm thick, stuctur-ally disordered rim that is compositionally similar to the core of the grain. One of the surface adhering grains is pyrrhotite show-ing a S-depleted rim (~8-10 nm thick) with nanophase Fe metal grains (<5 nm) decorating the outermost surface. The pyrrhotite displays a complex superstructure in its core that is absent in the S-depleted rim. Particle RA-QD02-0211 contains solar flare particle tracks (~2x109 cm-2) and shows a structurally disordered rim ~100 nm thick. The track density corresponds to a surface exposure of ~103-104 years based on the track production rate of [1]. The dis-ordered rim is nanocrystalline with minor amorphous material between crystalline domains. Quantitative element maps show the outermost ~10 nm of the disordered rim is Si-rich. Discussion and Conclusions: Both particles record the ef-fects of space weathering processes on Itokawa. Noguchi et al. [2] proposed that the disordered rims they observed on Itokawa particles largely result from solar wind radiation damage and we arrive at a similar conclusion for the two particles we analyzed. The microstructure of the S-depleted layer on the pyrrhotite grain in RA-QD02-0125 is similar to that observed in troilite irradiated with ~1018 4 kV He+ [3, 4]. Prolonged irradiation has also been shown to disorder pyrrhotite such that the superstructure reflec-tions are lost [5].

Keller, Lindsay P.↗
NASA NTRS1989

Possible use of pattern recognition for the analysis of Mars rover X-ray fluorescence spectra

On the Mars rover sample-return mission, the rover vehicle will collect and select samples from different locations on the Martian surface to be brought back to earth for laboratory studies. It is anticipated that an in situ energy-dispersive X-ray fluorescence (XRF) spectrometer will be on board the rover. On such a mission, sample selection is of higher priority than in situ quantitative chemical anlaysis. With this in mind, a pattern recognition technique is proposed as a simple, direct, and speedy alternative to detailed chemical analysis of the XRF spectra. The validity and efficacy of the pattern recognition technique are demonstrated by the analyses of laboratory XRF spectra obtained from a series of geological samples, in the form both of standardized pressed pellets and as unprepared rocks. It is found that pattern recognition techniques applied to the raw XRF spectra can provide for the same discrimination among samples as a knowledge of their actual chemical composition.

Yin, Lo I↗
NASA NTRS2002

Energy Dispersive Spectrometry and Quantitative Analysis Short Course. Introduction to X-ray Energy Dispersive Spectrometry and Quantitative Analysis

This course will cover practical applications of the energy-dispersive spectrometer (EDS) to x-ray microanalysis. Topics covered will include detector technology, advances in pulse processing, resolution and performance monitoring, detector modeling, peak deconvolution and fitting, qualitative and quantitative analysis, compositional mapping, and standards. An emphasis will be placed on use of the EDS for quantitative analysis, with discussion of typical problems encountered in the analysis of a wide range of materials and sample geometries.

Carpenter, Paul↗
NASA NTRS1996

X-ray digital imaging petrography of lunar mare soils: modal analyses of minerals and glasses

It is essential that accurate modal (i.e., volume) percentages of the various mineral and glass phases in lunar soils be used for addressing and resolving the effects of space weathering upon reflectance spectra, as well as for their calibration such data are also required for evaluating the resource potential of lunar minerals for use at a lunar base. However, these data are largely lacking. Particle-counting information for lunar soils, originally obtained to study formational processes, does not provide these necessary data, including the percentages of minerals locked in multi-phase lithic fragments and fused-soil particles, such as agglutinates. We have developed a technique for modal analyses, sensu stricto, of lunar soils, using digital imaging of X-ray maps obtained with an energy-dispersive spectrometer mounted on an electron microprobe. A suite of nine soils (90 to 150 micrometers size fraction) from the Apollo 11, 12, 15, and 17 mare sites was used for this study. This is the first collection of such modal data on soils from all Apollo mare sites. The abundances of free-mineral fragments in the mare soils are greater for immature and submature soils than for mature soils, largely because of the formation of agglutinitic glass as maturity progresses. In considerations of resource utilization at a lunar base, the best lunar soils to use for mineral beneficiation (i.e., most free-mineral fragments) have maturities near the immature/submature boundary (Is/FeO approximately or = 30), not the mature soils with their complications due to extensive agglutination. The particle data obtained from the nine mare soils confirm the generalizations for lunar soils predicted by L.A. Taylor and D.S. McKay (1992, Lunar Planet Sci. Conf. 23rd, pp. 1411-1412 [Abstract]).

NASA Discipline Exobiology↗
NASA NTRS2005

Quantitative Electron Probe Microanalysis: State of the Art

Quantitative electron-probe microanalysis (EPMA) has improved due to better instrument design and X-ray correction methods. Design improvement of the electron column and X-ray spectrometer has resulted in measurement precision that exceeds analytical accuracy. Wavelength-dispersive spectrometer (WDS) have layered-dispersive diffraction crystals with improved light-element sensitivity. Newer energy-dispersive spectrometers (EDS) have Si-drift detector elements, thin window designs, and digital processing electronics with X-ray throughput approaching that of WDS Systems. Using these systems, digital X-ray mapping coupled with spectrum imaging is a powerful compositional mapping tool. Improvements in analytical accuracy are due to better X-ray correction algorithms, mass absorption coefficient data sets,and analysis method for complex geometries. ZAF algorithms have ban superceded by Phi(pz) algorithms that better model the depth distribution of primary X-ray production. Complex thin film and particle geometries are treated using Phi(pz) algorithms, end results agree well with Monte Carlo simulations. For geological materials, X-ray absorption dominates the corretions end depends on the accuracy of mass absorption coefficient (MAC) data sets. However, few MACs have been experimentally measured, and the use of fitted coefficients continues due to general success of the analytical technique. A polynomial formulation of the Bence-Albec alpha-factor technique, calibrated using Phi(pz) algorithms, is used to critically evaluate accuracy issues and can be also be used for high 2% relative and is limited by measurement precision for ideal cases, but for many elements the analytical accuracy is unproven. The EPMA technique has improved to the point where it is frequently used instead of the petrogaphic microscope for reconnaissance work. Examples of stagnant research areas are: WDS detector design characterization of calibration standards, and the need for more complete treatment of the continuum X-ray fluorescence correction.

Carpernter, P. K.↗
NASA NTRS1989

The Wavelength-Dispersive Spectrometer and Its Proposed Use in the Analytical Electron Microscope

The Analytical Electron Microscope (AEM) equipped with a wavelength-dispersive spectrometer (WDS) should have the ability to resolve peaks which normally overlap in the spectra from an energy-dispersive spectrometer (EDS). With a WDS it should also be possible to measure lower concentrations of elements in thin foils due to the increased peak-to-background ratio compared with EDS. The WDS will measure X-ray from the light elements (4 less than Z less than 1O) more effectively. This paper addresses the possibility of interfacing a compact WDS with a focussing circle of approximately 4 cm to a modem AEM with a high-brightness (field emission) source of electrons.

Goldstein, Joseph I.↗
NASA NTRS2005

Atmospheric Electron-Induced X-Ray Spectrometer (AEXS) Development

This paper describes the progress in the development of the so-called Atmospheric Electron X-ray Spectrometer (AEXS) instrument in our laboratory at JPL. The AEXS is a novel miniature instrument concept based on the excitation of characteristic X-Ray Fluorescence (XRF) and luminescence spectra using a focused electron beam, for non-destructive evaluation of surfaces of samples in situ, in planetary ambient atmosphere. In situ operation is obtained through the use of a thin electron transmissive membrane to isolate the vacuum within the AEXS electron source from the outside ambient atmosphere. By using a focused electron beam, the impinging electrons on samples in the external atmosphere excite XRF spectra from the irradiated spots with high-to-medium spatial resolution. The XRF spectra are analyzed using an energy-dispersive detector to determine surface elemental composition. The use of high- intensity electron beam results in rapid spectrum acquisition (several minutes), and consequently low energy consumption (several tens of Joules) per acquired XRF spectrum in comparison to similar portable instruments.

X-ray fluorescence (XRF)↗
NASA NTRS1999

A Mossbauer investigation of iron-rich terrestrial hydrothermal vent systems: lessons for Mars exploration

Hydrothermal spring systems may well have been present on early Mars and could have served as a habitat for primitive life. The integrated instrument suite of the Athena Rover has, as a component on the robotic arm, a Mossbauer spectrometer. In the context of future Mars exploration we present results of Mossbauer analysis of a suite of samples from an iron-rich thermal spring in the Chocolate Pots area of Yellowstone National Park (YNP) and from Obsidian Pool (YNP) and Manitou Springs, Colorado. We have found that Mossbauer spectroscopy can discriminate among the iron-bearing minerals in our samples. Those near the vent and on the surface are identified as ferrihydrite, an amorphous ferric mineraloid. Subsurface samples, collected from cores, which are likely to have undergone inorganic and/or biologically mediated alteration (diagenesis), exhibit spectral signatures that include nontronite (a smectite clay), hematite (alpha-Fe2O3), small-particle/nanophase goethite (alpha-FeOOH), and siderite (FeCO3). We find for iron minerals that Mossbauer spectroscopy is at least as efficient in identification as X-ray diffraction. This observation is important from an exploration standpoint. As a planetary surface instrument, Mossbauer spectroscopy can yield high-quality spectral data without sample preparation (backscatter mode). We have also used field emission scanning electron microscopy (FESEM), in conjunction with energy-dispersive X ray (EDX) fluorescence spectroscopy, to characterize the microbiological component of surface sinters and the relation between the microbiological and the mineralogical framework. Evidence is presented that the minerals found in these deposits can have multi-billion-year residence times and thus may have survived their possible production in a putative early Martian hot spring up to the present day. Examples include the nanophase property and the Mossbauer signature for siderite, which has been identified in a 2.09-billion-year old hematite-rich chert stromatolite. Our research demonstrates that in situ Mossbauer spectroscopy can help determine whether hydrothermal mineral deposits exist on Mars, which is significant for exobiology because of the issue of whether that world ever had conditions conductive to the origin of life. As a useful tool for selection of samples suitable for transport to Earth, Mossbauer spectroscopy will not only serve geological interests but will also have potential for exopaleontology.

NASA Discipline Exobiology↗
NASA NTRS2005

Atmospheric Electron-induced X-Ray Spectrometer (AEXS) Instrument Development

Instrument Development: The membrane properties were investigated in detail due to its critical role. A series of experiments determined that our designed membranes have high electron transmission, yet are capable of isolating high vacuum, are able to withstand differential pressure in excess of one atmosphere, survive vibrational shocks of a magnitude to be expected during a planetary mission. Our initial work has been with a 10 keV source and a 200 nm thick Silicon Nitride (SiN) encapsulation membrane micro-fabricated within a Si support frame (1.5 mm x 1.5 mm window openings. Fig 2 compares the spectra taken with the 10 keV source with spectra taken within SEM. Introduction: This paper describes the progress in the development of the AEXS instrument in our laboratory at JPL. The AEXS is a novel miniature instrument[1-3] based on the excitation of characteristic X-Ray Fluorescence (XRF) and luminescence spectra using a focused electron beam, for non-destructive evaluation of surfaces of samples in planetary ambient atmosphere. In situ operation is obtained through the use of a thin electron transmissive membrane to isolate the vacuum within the AEXS electron source from the outside ambient atmosphere. The impinging electrons excite XRF spectra from the irradiated spots on samples in external atmosphere with high-to-medium (sub-mm to cm-scale) spatial resolution at Mars atmospheric pressure. The XRF spectra are analyzed using an energy-dispersive detector to determine surface elemental composition, or in the case of electron-induced luminescence to identify unusual formations on surface that cathodo-luminescence (CL). The AEXS system (Fig 1) consists of a high-energy (>10keV) electron gun encapsulated by the isolation membrane, an EDX detection and analyzer system to determine the elemental abundance, an optional CL detection system, and a high voltage power supply. The approach to demonstrating a proof of concept of the AEXS has been through 1) demonstrating the viability of micro-fabricated membranes, 2) assembling AEXS setups with increasingly integrated functional components, and 3) simulating the AEXS observational capabilities. This paper will focus on description of the development of the instrument.

Wilcox, J. Z.↗