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NASA NTRS1985

Diffusion in Immiscible Melts

The objective of this program is to measure the diffusion coefficients for molten Pb in Zn in the immiscible liquid-phase region. Diffusion couples of pure Pb and Zn were prepared using a shear cell. These have been placed in graphite crucibles and encapsulated in stainless steel cartridges and are awaiting the next Materials Experiment Assembly (MEA) flight opportunity. In flight, one couple will be soaked for 40 minutes at 440 deg C (just above the monotectic temperature) and the second couple will be soaked for 40 minutes 820 deg C (just above the consolute temperature). After the soak both samples will be rapidly quenched by flowing He to minimize redistribution of the immiscible phases. Post flight compositional analysis will be accomplished using X-ray fluorescence in the scanning electron microscopy.

Pond, R. B.↗

NASA NTRS1985

Some observations on the geology of the Apollo 15 landing site

High resolution (panoramic) and high geometric fidelity (metric) photos were taken from orbit of the lunar landing sites. Gamma ray and X-ray fluorescence spectroscopic measurement were taken to determine regional chemical composition of the Moon. Distinctive features of the Apennine Bench Formation are described. The structurally controlled topography of the Apennine Bench Formation is suggested of a lava channel or collapsed lava tube.

Swann, G. A.↗

NASA NTRS2005

CheMin: A Definitive Mineralogy Instrument in the Analytical Laboratory of the Mars Science Laboratory (MSL '09)

An important goal of the Mars Science Laboratory (MSL 09) mission is the determination of definitive mineralogy and chemical composition. CheMin is a miniature X-ray diffraction/X-ray fluorescence (XRD/XRF) instrument that has been chosen for the analytical laboratory of MSL. CheMin utilizes a miniature microfocus source cobalt X-ray tube, a transmission sample cell and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D X-ray diffraction patterns and X-ray fluorescence spectra from powdered or crushed samples. A diagrammatic view of the instrument is shown.

Blake, D. F.↗

NASA NTRS2005

CheMin: A Definitive Mineralogy Instrument in the Analytical Laboratory of the Mars Science Laboratory

An important goal of the Mars Science Laboratory (MSL '09) mission is the determination of definitive mineralogy and chemical composition. CheMin is a miniature X-ray diffraction/X-ray fluorescence (XRD/XRF) instrument that has been chosen for the analytical laboratory of MSL. CheMin utilizes a miniature microfocus source cobalt X-ray tube, a transmission sample cell and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D X-ray diffraction patterns and X-ray fluorescence spectra from powdered or crushed samples. A diagrammatic view of the instrument is shown. Additional information is included in the original extended abstract.

Blake, David F.↗

NASA NTRS2003

Development and Testing of Laser-induced Breakdown Spectroscopy for the Mars Rover Program: Elemental Analyses at Stand-Off Distances

One of the most fundamental pieces of information about any planetary body is the elemental composition of its surface materials. The Viking Martian landers employed XRF (x-ray fluorescence) and the MER rovers are carrying APXS (alpha-proton x-ray spectrometer) instruments upgraded from that used on the Pathfinder rover to supply elemental composition information for soils and rocks to which direct contact is possible. These in- situ analyses require that the lander or rover be in contact with the sample. In addition to in-situ instrumentation, the present generation of rovers carry instruments that operate at stand-off distances. The Mini-TES is an example of a stand-off instrument on the MER rovers. Other examples for future missions include infrared point spectrometers and microscopic-imagers that can operate at a distance. The main advantage of such types of analyses is obvious: the sensing element does not need to be in contact or even adjacent to the target sample. This opens up new sensing capabilities. For example, targets that cannot be reached by a rover due to impassable terrain or targets positioned on a cliff face can now be accessed using stand-off analysis. In addition, the duty cycle of stand-off analysis can be much greater than that provided by in-situ measurements because the stand-off analysis probe can be aimed rapidly at different features of interest eliminating the need for the rover to actually move to the target. Over the past five years we have been developing a stand-off method of elemental analysis based on atomic emission spectroscopy called laser-induced breakdown spectroscopy (LIBS). A laser-produced spark vaporizes and excites the target material, the elements of which emit at characteristic wavelengths. Using this method, material can be analyzed from within a radius of several tens of meters from the instrument platform. A relatively large area can therefore be sampled from a simple lander without requiring a rover or sampling arms. The placement of such an instrument on a rover would allow the sampling of locations distant from the landing site. Here we give a description of the LIBS method and its advantages. We discuss recent work on determining its characteristics for Mars exploration, including accuracy, detection limits, and suitability for determining the presence of water ice and hydrated minerals. We also give a description of prototype instruments we have tested in field settings.

D A Cremers↗

NASA NTRS2002

Crime scene investigations using portable, non-destructive space exploration technology

The National Institute of Justice (NIJ) and the National Aeronautics and Space Administration's (NASAs) Goddard Space Flight Center (GSFC) have teamed up to explore the use of NASA developed technologies to help criminal justice agencies and professionals solve crimes. The objective of the program is to produce instruments and communication networks that have application within both NASA's space program and NIJ programs with state and local forensic laboratories. A working group of NASA scientists and law enforcement professionals has been established to develop and implement a feasibility demonstration program. Specifically, the group has focused its efforts on identifying gunpowder and primer residue, blood, and semen at crime scenes. Non-destructive elemental composition identification methods are carried out using portable X-ray fluorescence (XRF) systems. These systems are similar to those being developed for planetary exploration programs. A breadboard model of a portable XRF system has been constructed for these tests using room temperature silicon and cadmium-zinc telluride (CZT) detectors. Preliminary tests have been completed with gunshot residue (GSR), blood-spatter and semen samples. Many of the element composition lines have been identified. Studies to determine the minimum detectable limits needed for the analyses of GSR, blood and semen in the crime scene environment have been initiated and preliminary results obtained. Furthermore, a database made up of the inorganic composition of GSR is being developed. Using data obtained from the open literature of the elemental composition of barium (Ba) and antimony (Sb) in handswipes of GSR, we believe that there may be a unique GSR signature based on the Sb to Ba ratio.

Firearms↗

NASA NTRS1993

Remote sensing x ray fluorescence spectrometry for future lunar exploration missions

Measurement of discrete line X-ray emission from space can be used to obtain both qualitative and quantitative elemental surface composition information. Remote orbital X-ray elemental analysis is the measurement of characteristic X-rays following the interaction of solar X-rays with the surface of a given solid body. Thus, X-ray emission from a surface is strongly dependent on the incident solar spectrum as well as on the chemical composition of the surface. In this paper, the relationship between the solar flux and the major lunar element fluorescence and scattered X-ray flux is characterized. A model was developed to calculate lunar surface X-ray fluorescence emission spectra under a variety of solar conditions and, in particular, conditions that might be expected for a Lunar Scout mission proposed for 1995 or 1996. This time period should be during solar minimum.

Clark, Pamela E.↗

DOE OSTI2022

Aerosol iron speciation and seasonal variation of iron oxidation state over the western Antarctic Peninsula

The iron (Fe) speciation and oxidation state have been considered critical factors affecting Fe solubility in the atmosphere and bioavailability in the surface ocean. In this study, elemental composition and Fe speciation in aerosol samples collected at the Palmer Station in the West Antarctic Peninsula were determined using synchrotron-based X-ray fluorescence (XRF) and X-ray Absorption Near-Edge Structure (XANES) spectroscopy. The elemental composition of coarse-mode (>1 mu m) Fe-containing particles suggests that the region's crustal emission is the primary source of aerosol Fe. The Fe minerals in these aerosol particles were predominantly hematite and biotite, but minor fractions of pyrite and ilmenite were observed as well. The Fe oxidation state showed an evident seasonal variation. Further, the Fe(II) content accounted for 71% of the total Fe in the austral summer, while this fraction dropped to 60% in the austral winter. Multivariate linear models involving meteorological parameters suggested that the wind speed, relative humidity, and solar irradiance were the factors that significantly controlled the percentage of Fe(II) in the austral summer. On the contrary, no relationship was found between these factors and the Fe(II) percentage in the austral winter, suggesting that atmospheric photoreduction and regional dust emission were limited. Moreover, the snow depth was significantly (p < 0.05) correlated with the aerosol Fe concentration, confirming the limiting effect of snow/ice cover on the regional dust emission. Given that the Antarctic Peninsula has experienced rapid warming during recent decades, the ice-free areas in the Antarctic Peninsula may act as potential dust sources.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1982

Chemical composition of Martian fines

Of the 21 samples acquired for the Viking X-ray fluorescence spectrometer, 17 were analyzed to high precision. Compared to typical terrestrial continental soils and lunar mare fines, the Martian fines are lower in Al, higher in Fe, and much higher in S and Cl concentrations. Protected fines at the two lander sites are almost indistinguishable, but concentration of the element S is somewhat higher at Utopia. Duricrust fragments, successfully acquired only at the Chryse site, invariably contained about 50% higher S than fines. No elements correlate positively with S, except Cl and possibly Mg. A sympathetic variation is found among the triad Si, Al, Ca; positive correlation occurs between Ti and Fe. Sample variabilities are as great within a few meters as between lander locations (4500 km apart), implying the existence of a universal Martian regolith component of constant average composition. The nature of the source materials for the regolith fines must be mafic to ultramafic.

Clark, B. C.↗

DOE OSTI2026

3D printed water-stable Cd-doped Cs 4 MnBi 2 Cl 12 /polylactic acid perovskite/polymer composites for high-flux X-ray scintillation

Stable and efficient X-ray scintillators are crucial for medical diagnostics, industrial, and defense applications. However, conventional scintillator technologies face a trade-off between stability, optimal performance, and sustainability. Herein, we introduce 3D-printed Cs 4 MnBi 2 Cl 12 (Pero1) and Cs 4 Cd 0.68 Mn 0.32 Bi 2 Cl 12 (Pero2) perovskite microcrystals embedded within a polylactic acid (PLA) polymer composite as X-ray scintillators, combining efficiency, stability, and sustainability. The orange luminescent perovskite powder phosphors exhibited poor water stability, which was successfully addressed through incorporation into PLA via filament extrusion and fused deposition modeling (FDM) 3D printing. The resulting composite films demonstrated remarkable water stability while maintaining uniform orange emission throughout the polymer matrix, as confirmed by 3D topography scanning and X-ray fluorescence mapping. Structural characterization revealed minimal chemical interaction between the perovskite and PLA matrix, with the composites retaining their crystalline properties. The PLA-Pero2 composite exhibited superior optical properties, with a photoluminescence quantum yield of 47%, nearly 17 times higher than that of PLA-Pero1 (2.8%), attributed to the effective suppression of non-radiative decay pathways through Cd 2+ doping. Under hard X-ray irradiation at synchrotron beamlines, both composites exhibited excellent radioluminescence, with emission peaks at 605 nm, a linear response across a wide X-ray flux range, and remarkable radiation stability, showing less than 3% intensity degradation after 600 seconds of continuous high-dose exposure. The PLA-Pero2 composite achieved a spatial resolution of 5 line pairs per millimeter and a contrast ratio of 0.255. These performance metrics, combined with the polymer's biodegradability and scalability through additive manufacturing, position PLA-based composites as a more sustainable alternative to conventional petroleum-based polymer scintillators for next-generation medical imaging, radiation monitoring, and industrial radiography applications.

3D Printing↗

DOE OSTI2020

Multimodal Imaging of Autofluorescent Sites Reveals Varied Chemical Speciation in SSZ-13 Crystals

Here, a multimodal imaging study of chabazite is used to show the distribution of and discriminate between different emissive deposits arising as a result of the detemplation process. 3D confocal imaging, fluorescence lifetime imaging, spectral imaging, and Raman mapping are used to show three different types of emissive behaviours each characterised by different spatial distributions, trends in lifetime, spectral signals, and Raman signatures. A notable difference is seen in the morphology of agglomerated surface deposits and larger subsurface deposits, which experience lifetime augmentation due to spatial confinement. The distribution of organic residue throughout the crystal volume is comparable to XRF mapping that shows Si enrichment on the outer edges and higher Al content through the centre, demonstrating that a fluorescence-based technique can also be used to indirectly comment on the compositional chemistry of the inorganic framework.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2026

A new water-based scintillator for efficient Cherenkov and scintillation separation

Neutrinos offer a unique window into the world around us, allowing us to probe otherwise unreachable regions like the interior of stars and the depths of the earth, as well as potentially offering a mechanism for monitoring nuclear activity. Both pure-water and organic liquid scintillators have been used as the detection medium of large-scale neutrino detectors. Organic liquid scintillators offer higher sensitivity at lower energies, which is desirable for many applications, but detection of the Cherenkov radiation required for directional sensitivity is very difficult. A possible solution is to use water-based liquid scintillators (WbLSs), where some fraction of the water is replaced with a micellar solution of the liquid scintillator. This can enhance the detection sensitivity beyond that of pure water, without significantly affecting the ability to leverage the topological Cherenkov signature. Very specific scintillation properties are required to achieve this goal: the scintillation decay time should be significantly slower than that of the Cherenkov emission, so timing-based discrimination of Cherenkov light from scintillation can be applied. At the same time, the light yield should be high enough to enhance the overall sensitivity of the detector, but without losing too much of the Cherenkov light. In this study, we report a new water-based liquid scintillation cocktail based on a 9-methylcarbazole fluorescent dye and a linear alkylbenzene solvent. Here, the proposed composition offers 13.8 ns scintillation decay time and 368 nm emission that matches the desired properties.

Wolszczak, Weronika W. [Lawrence Berkeley National↗

NASA NTRS1993

Trace element content of chondritic cosmic dust: Volatile enrichments, thermal alterations, and the possibility of contamination

Trace element abundances in 51 chondritic Interplanetary Dust Particles (IDP's) were measured by Synchrotron X-Ray Fluorescence (SXRF). The data allow us to determine an average composition of chondritic IDP's and to examine the questions of volatile loss during the heating pulse experienced on atmospheric entry and possible element addition due to contamination during atmospheric entry, stratospheric residence, and curation.

Flynn, G. J.↗

NASA NTRS2002

A Miniature Mineralogical Instrument for In-Situ Characterization of Ices and Hydrous Minerals at the Lunar Poles

Lunar missions over the past few years have provided new evidence that water may be present at the lunar poles in the form of cold-trapped ice deposits, thereby rekindling interest in sampling the polar regions. Robotic landers fitted with mineralogical instrumentation for in-situ analyses could provide unequivocal answers on the presence of crystalline water ice and/or hydrous minerals at the lunar poles. Data from Lunar Prospector suggest that any surface exploration of the lunar poles should include the capability to drill to depths of more than 40 cm. Limited data on the lunar geotherm indicate temperatures of approximately 245-255 K at regolith depths of 40 cm, within a range where water may exist in the liquid state as brine. A relevant terrestrial analog occurs in Antarctica, where the zeolite mineral chabazite has been found at the boundary between ice-free and ice-cemented regolith horizons, and precipitation from a regolith brine is indicated. Soluble halogens and sulfur in the lunar regolith could provide comparable brine chemistry in an analogous setting. Regolith samples collected by a drilling device could be readily analyzed by CheMin, a mineralogical instrument that combines X-ray diffraction (XRD) and X-ray fluorescence (XRF) techniques to simultaneously characterize the chemical and mineralogical compositions of granular or powdered samples. CheMin can unambiguously determine not only the presence of hydrous alteration phases such as clays or zeolites, but it can also identify the structural variants or types of clay or zeolite present (e.g., well-ordered versus poorly ordered smectite; chabazite versus phillipsite). In addition, CheMin can readily measure the abundances of key elements that may occur in lunar minerals (Na, Mg, Al, Si, K, Ca, Fe) as well as the likely constituents of lunar brines (F, Cl, S). Finally, if coring and analysis are done during the lunar night or in permanent shadow, CheMin can provide information on the chemistry and structure of any crystalline ices that might occur in the regolith samples.

Sarrazin, P.↗

NASA NTRS2011

Detection Limit of Smectite by Chemin IV Laboratory Instrument: Preliminary Implications for Chemin on the Mars Science Laboratory Mission

The CheMin instrument on the Mars Science Laboratory (MSL) is an miniature X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of detecting the mineralogical and elemental compositions of rocks, outcrops and soils on the surface of Mars. CheMin uses a microfocus-source Co X-ray tube, a transmission sample cell, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. CRISM and OMEGA have identified the presence of phyllosilicates at several locations on Mars including the four candidate MSL landing sites. The objective of this study was to conduct preliminary studies to determine the CheMin detection limit of smectite in a smectite/olivine mixed mineral system.

Archilles, Cherie↗

NASA NTRS2012

Effects of Kapton Sample Cell Windows on the Detection Limit of Smectite: Implications for CheMin on the Mars Science Laboratory Mission

The CheMin instrument on the Mars Science Laboratory (MSL) rover Curiosity is an X-ray diffraction (XRD) and X-ray fluorescence (XRF) instrument capable of providing the mineralogical and chemical compositions of rocks and soils on the surface of Mars. CheMin uses a microfocus X-ray tube with a Co target, transmission geometry, and an energy-discriminating X-ray sensitive CCD to produce simultaneous 2-D XRD patterns and energy-dispersive X-ray histograms from powdered samples. CheMin has two different window materials used for sample cells -- Mylar and Kapton. Instrument details are provided elsewhere. Fe/Mg-smectite (e.g., nontronite) has been identified in Gale Crater, the MSL future landing site, by CRISM spectra. While large quantities of phyllosilicate minerals will be easily detected by CheMin, it is important to establish detection limits of such phases to understand capabilities and limitations of the instrument. A previous study indicated that the (001) peak of smectite at 15 Ang was detectable in a mixture of 1 wt.% smectite with olivine when Mylar is the window material for the sample cell. Complications arise when Kapton is the window material because Kapton itself also has a diffraction peak near 15 Ang (6.8 deg 2 Theta). This study presents results of mineral mixtures of smectite and olivine to determine smectite detection limits for Kapton sample cells. Because the intensity and position of the smectite (001) peak depends on the hydration state, we also analyzed mixtures with "hydrated" and "dehydrated"h smectite to examine the effects of hydration state on detection limits.

Achilles, C. N.↗

NASA NTRS2013

X-Ray Diffraction Reference Intensity Ratios of Amorphous and Poorly Crystalline Phases: Implications for CheMin on the Mars Science Laboratory

Morris, R. V.↗

DOE OSTI2021

Chemical Composition of Outbursting Comet C/2015 ER61 (PanSTARRS)

Comet C/2015 ER61 (PanSTARRS) is a long-period Oort cloud comet whose favorable approach to the inner parts of the solar system in 2017 April–May enabled us to characterize its primary volatile composition using the iSHELL spectrograph mounted on the 3 m NASA Infrared Telescope Facility (IRTF) on Maunakea, Hawaii. We used three iSHELL settings (covering ~2.8–5.2 μm) to sample fluorescent emissions from H{sub 2}O, OH, CH{sub 3}OH, HCN, C{sub 2} H{sub 2}, NH{sub 3}, CO, CH{sub 4}, C{sub 2}H{sub 6}, H{sub 2}CO, and OCS on multiple dates ranging from UT 2017 April 15 (shortly after its April 4 outburst) to May 13, nearly 30 days before the detection of its double nucleus. Our observations also offered the opportunity to obtain sensitive 3σ upper limits for cyanoacetylene (HC{sub 3}N). We report rotational temperatures (T{sub rot}), production rates (Qs), abundance (mixing) ratios (relative to H{sub 2}O and C{sub 2}H{sub 6}), and spatial distributions in the coma. ER61 exhibits variability in production rates of many species on short (day-to-day) and long (pre- versus post-perihelion) timescales. The relative abundances of these volatile species remained consistent within uncertainties during our pre-perihelion observations but tended to decrease during our post-perihelion observations (with the exception of CH{sub 3}OH and HCN). The short-timescale variability in the production rates of these volatiles could be due to diurnal effects (over the course of the rotation of the nucleus) and/or the effect of its outburst. The decrease in the production rates and hence the mixing ratios in some volatiles in post-perihelion dates could be due to the presence of seasonal effects in ER61.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗