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NASA NTRS2011

Field Characterization of the Mineralogy and Organic Chemistry of Carbonates from the 2010 Arctic Mars Analog Svalbard Expedition by Evolved Gas Analysis

The 2010 Arctic Mars Analog Svalbard Expedition (AMASE) investigated two geologic settings using methodologies and techniques being developed or considered for future Mars missions, such as the Mars Science Laboratory (MSL), ExoMars, and Mars Sample Return. The Sample Analysis at Mars (SAM) [1] instrument suite, which will be on MSL, consists of a quadrupole mass spectrometer (QMS), a gas chromatograph (GC), and a tunable laser mass spectrometer (TLS); all will be applied to analyze gases created by pyrolysis of samples. During AMASE, a Hiden Evolved Gas Analysis-Mass Spectrometer (EGA-MS) system represented the EGA-MS capability of SAM. Another MSL instrument, CheMin, will use x-ray diffraction (XRD) and x-ray fluorescence (XRF) to perform quantitative mineralogical characterization of samples [e.g., 2]. Field-portable versions of CheMin were used during AMASE. AMASE 2010 focused on two sites that represented biotic and abiotic analogs. The abiotic site was the basaltic Sigurdfjell vent complex, which contains Mars-analog carbonate cements including carbonate globules which are excellent analogs for the globules in the ALH84001 martian meteorite [e.g., 3, 4]. The biotic site was the Knorringfjell fossil methane seep, which featured carbonates precipitated in a methane-supported chemosynthetic community [5]. This contribution focuses on EGA-MS analyses of samples from each site, with mineralogy comparisons to CheMin team results. The results give insight into organic content and organic-mineral associations, as well as some constraints on the minerals present.

McAdam, A. C.↗

NASA NTRS2005

Identifying Objects via Encased X-Ray-Fluorescent Materials - the Bar Code Inside

Systems for identifying objects by means of x-ray fluorescence (XRF) of encased labeling elements have been developed. The XRF spectra of objects so labeled would be analogous to the external bar code labels now used to track objects in everyday commerce. In conjunction with computer-based tracking systems, databases, and labeling conventions, the XRF labels could be used in essentially the same manner as that of bar codes to track inventories and to record and process commercial transactions. In addition, as summarized briefly below, embedded XRF labels could be used to verify the authenticity of products, thereby helping to deter counterfeiting and fraud. A system, as described above, is called an encased core product identification and authentication system (ECPIAS). The ECPIAS concept is a modified version of that of a related recently initiated commercial development of handheld XRF spectral scanners that would identify alloys or detect labeling elements deposited on the surfaces of objects. In contrast, an ECPIAS would utilize labeling elements encased within the objects of interest. The basic ECPIAS concept is best illustrated by means of an example of one of several potential applications: labeling of cultured pearls by labeling the seed particles implanted in oysters to grow the pearls. Each pearl farmer would be assigned a unique mixture of labeling elements that could be distinguished from the corresponding mixtures of other farmers. The mixture would be either incorporated into or applied to the surfaces of the seed prior to implantation in the oyster. If necessary, the labeled seed would be further coated to make it nontoxic to the oyster. After implantation, the growth of layers of mother of pearl on the seed would encase the XRF labels, making these labels integral, permanent parts of the pearls that could not be removed without destroying the pearls themselves. The XRF labels would be read by use of XRF scanners, the spectral data outputs of which would be converted to alphanumeric data in a digital equivalent data system (DEDS), which is the subject of the previous article. These alphanumeric data would be used to track the pearls through all stages of commerce, from the farmer to the retail customer.

Schramm, Harry F.↗

NASA NTRS2006

The Role of Materials Degradation and Analysis in the Space Shuttle Columbia Accident Investigation

The efforts following the loss of the Space Shuttle Columbia included debris recovery, reconstruction, and analysis. The debris was subjected to myriad quantitative and semiquantitative chemical analysis techniques, ranging from examination via the scanning electron microscope (SEM) with energy dispersive spectrometer (EDS) to X-Ray diffraction (XRD) and electron probe micro-analysis (EPMA). The results from the work with the debris helped the investigators determine the location where a breach likely occurred in the leading edge of the left wing during lift off of the Orbiter from the Kennedy Space Center. Likewise, the information evidenced by the debris was also crucial in ascertaining the path of impinging plasma flow once it had breached the wing. After the Columbia Accident Investigation Board (CAIB) issued its findings, the major portion of the investigation was concluded. However, additional work remained to be done on many pieces of debris from portions of the Orbiter which were not directly related to the initial impact during ascent. This subsequent work was not only performed in the laboratory, but was also performed with portable equipment, including examination via portable X-Ray fluorescence (XRF) and Fourier transform infrared spectroscopy (FTIR). Likewise, acetate and silicon-rubber replicas of various fracture surfaces were obtained for later macroscopic and fractographic examination. This paper will detail the efforts and findings from the initial investigation, as well as present results obtained by the later examination and analysis of debris from the Orbiter including its windows, bulkhead structures, and other components which had not been examined during the primary investigation.

McDanels, Steven J.↗

NASA NTRS2012

Evolved Gas Analysis of Mars Analog Samples from the Arctic Mars Analog Svalbard Expedition: Implications for Analyses by the Mars Science Laboratory

The 2011 Arctic Mars Analog Svalbard Expedition (AMASE) investigated several geologic settings on Svalbard, using methodologies and techniques being developed or considered for future Mars missions, such as the Mars Science Laboratory (MSL). The Sample Analysis at Mars (SAM) instrument suite on MSL consists of a quadrupole mass spectrometer (QMS), a gas chromatograph (GC), and a tunable laser spectrometer (TLS), which analyze gases created by pyrolysis of samples. During AMASE, a Hiden Evolved Gas Analysis-Mass Spectrometer (EGA-MS) system represented the EGA-QMS capability of SAM. Another MSL instrument, CheMin, will use x-ray diffraction (XRD) and x-ray fluorescence (XRF) to perform quantitative mineralogical characterization of samples. Field-portable versions of CheMin were used during AMASE. AMASE 2011 sites spanned a range of environments relevant to understanding martian surface materials, processes and habitability. They included the basaltic Sverrefjell volcano, which hosts carbonate globules, cements and coatings, carbonate and sulfate units at Colletth0gda, Devonian sandstone redbeds in Bockfjorden, altered basaltic lava delta deposits at Mt. Scott Keltie, and altered dolerites and volcanics at Botniahalvoya. Here we focus on SAM-like EGA-MS of a subset of the samples, with mineralogy comparisons to CheMin team results. The results allow insight into sample organic content as well as some constraints on sample mineralogy.

McAdam, A.↗

NASA NTRS2010

Surface-Enhanced X-Ray Fluorescence

Surface-enhanced x-ray fluorescence (SEn-XRF) spectroscopy is a form of surface- enhanced spectroscopy that was conceived as a means of obtaining greater sensitivity in x-ray fluorescence (XRF) spectroscopy. As such, SEn-XRF spectroscopy joins the ranks of such other, longer-wavelength surface-enhanced spectroscopies as those based on surface-enhanced Raman scattering (SERS), surface-enhanced resonance Raman scattering (SERRS), and surfaceenhanced infrared Raman absorption (SEIRA), which have been described in previous NASA Tech Briefs articles. XRF spectroscopy has been used in analytical chemistry for determining the elemental compositions of small samples. XRF spectroscopy is rapid and quantitative and has been applied to a variety of metal and mineralogical samples. The main drawback of XRF spectroscopy as practiced heretofore is that sensitivity has not been as high as required for some applications. In SEn-XRF as in the other surface-enhanced spectroscopies, one exploits several interacting near-field phenomena, occurring on nanotextured surfaces, that give rise to local concentrations of incident far-field illumination. In this case, the far-field illumination comes from an x-ray source. Depending on the chemical composition and the geometry of a given nanotextured surface, these phenomena could include the lightning-rod effect (concentration of electric fields at the sharpest points on needlelike surface features), surface plasmon resonances, and grazing incidence geometric effects. In the far field, the observable effect of these phenomena is an increase in the intensity of the spectrum of interest - in this case, the x-ray fluorescence spectrum of chemical elements of interest that may be present within a surface layer at distances no more than a few nanometers from the surface.

Anderson, Mark↗

NASA NTRS1999

In Situ Identification of Mineral Resources with an X-Ray-Optical "Hands-Lens" Instrument

The recognition of material resources on a planetary surface requires exploration strategies not dissimilar to those employed by early field geologists who searched for ore deposits primarily from surface clues. In order to determine the location of mineral ores or other materials, it will be necessary to characterize host terranes at regional or subregional scales. This requires geographically broad surveys in which statistically significant numbers of samples are rapidly scanned from a roving platform. To enable broad-scale, yet power-conservative planetary-surface exploration, we are developing an instrument that combines x-ray diffractometry (XRD), x-ray fluorescence spectrometry (XRF), and optical capabilities; the instrument can be deployed at the end of a rover's robotic arm, without the need for sample capture or preparation. The instrument provides XRD data for identification of mineral species and lithological types; diffractometry of minerals is conducted by ascertaining the characteristic lattice parameters or "d-spacings" of mineral compounds. D-spacings of 1.4 to 25 angstroms can be determined to include the large molecular structures of hydrated minerals such as clays. The XRF data will identify elements ranging from carbon (Atomic Number = 6) to elements as heavy as barium (Atomic Number = 56). While a sample is being x-rayed, the instrument simultaneously acquires an optical image of the sample surface at magnifications from lx to at least 50x (200x being feasible, depending on the sample surface). We believe that imaging the sample is extremely important as corroborative sample-identification data (the need for this capability having been illustrated by the experience of the Pathfinder rover). Very few geologists would rely on instrument data for sample identification without having seen the sample. Visual inspection provides critical recognition data such as texture, crystallinity, granularity, porosity, vesicularity, color, lustre, opacity, and so forth. These data can immediately distinguish sedimentary from igneous rocks, for example, and can thus eliminate geochemical or mineral ambiguities arising, say between arkose and granite. It would be important to know if the clay being analyzed was part of a uniform varve deposit laid down in a quiescent lake, or the matrix of a megabreccia diamictite deposited as a catastrophic impact ejecta blanket. The unique design of the instrument, which combines Debye-Scherrer geometry with elements of standard goniometry, negates the need for sample preparation of any kind, and thus negates the need for power-hungry and mechanically-complex sampling systems that would have to chip, crush, sieve, and mount the sample for x-ray analysis. Instead, the instrument is simply rested on the sample surface of interest (like a hand lens); the device can interrogate rough rock surfaces, coarse granular material, or fine rock flour. A breadboard version of the instrument has been deployed from the robotic arm of the Marsokhod rover in field trials at NASA Ames, where large vesicular boulders were x-rayed to demonstrate the functionality of the instrument design, and the ability of such a device to comply with constraints imposed by a roving platform. Currently under development is a flight prototype concept of this instrument that will weigh 0.3 kg, using about 4500 J of energy per sample analysis. It requires about 5 min. for XRD analysis, and about 30 min. for XRF interrogation. Its small mass and rugged design make it ideal for deployment on small rovers of the type currently envisaged for the exploration of Mars (e.g., Sojourner-scale platforms). The design utilizes a monolithic P-N junction photodiode pixel array for XRD, a Si PIN photodiode/avalanche photodiode system for XRF, and an endoscopic imaging camera system unobtrusively embedded between the detectors and the x-ray source (the endoscope with its board-mounted camera can be adapted for IR light in addition to visible wavelenths. A rugged, miniature (7 cu cm) x-ray source for the instrument has already been breadboarded.

Marshall, J.↗

NASA NTRS1994

Innovative instrumentation for mineralogical and elemental analyses of solid extraterrestrial surfaces: The Backscatter Moessbauer Spectrometer/X Ray Fluorescence analyzer (BaMS/XRF)

We have developed a four-detector research-grade backscatter Moessbauer spectrometer (BaMS) instrument with low resolution x-ray fluorescence analysis (XRF) capability. A flight-qualified instrument based on this design would be suitable for use on missions to the surfaces of solid solar-system objects (Moon, Mars, asteroids, etc.). Target specifications for the flight instrument are as follows: mass less than 500 g; volumes less than 300 cu cm; and power less than 2 W. The BaMS/XRF instrument would provide data on the oxidation state of iron and its distribution among iron-bearing mineralogies and elemental composition information. This data is a primary concern for the characterization of extraterrestrial surface materials.

Shelfer, T. D.↗

NASA NTRS1997

In Situ identification of mineral resources with an X-ray-optical "Hand-Lens" instrument

Marshall, J.↗

NASA NTRS2008

In Situ Analysis of Martian Phyllosilicates Using the Chemin Minerological Instrument on Mars Science Laboratory

The CheMin minerological instrument on Mars Science Laboratory (MSL'09) [1] will return quantitive Xray diffraction data (XRD) and quantative X-ray fluorescence data (XRF;14<Z<92) from scooped soil samples and drilled rock powders collected from the Mars surface. Samples of 45-65 mm 3 from material sieved to less than 150 micrometers will be delivered through a funnel to one of 27 reusable sample cells (five additional cells on the sample wheel contain diffraction of fluorescence standards). Sample cells are 8-mm diamater discs with 7-micrometer thick Mylar or Kapton windows spaced 170 micrometers apart. Within this volume, the sample is shaken by piezoelectric vibration at sonic frequencies, causing the powder to flow past a narrow, collimated -ray beam in random orientation can be obtained even from minnerals exhibiting strong preferred orientation such as phylosilicates.

Blake, David F.↗

NASA NTRS2010

Test and Delivery of the Chemin Mineralogical Instrument for Mars Science Laboratory

The CheMin mineralogical instrument on MSL will return quantitative powder X-ray diffraction data (XRD) and qualitative X-ray fluorescence data (XRF; 14<Z<92) from scooped soil samples and drilled rock powders collected on the Mars surface. The geometry of the source, sample, and detector is shown. A transmission geometry was chosen so that diffracted intensities in the low-20 region (5-15 deg), important for phyllosilicate identification, could be detected.

Blake, D. F.↗

NASA NTRS1999

Strategies and Technologies for In Situ Mineralogical Investigations on Mars

Surface landers on Mars (Viking and Pathfinder) have not revealed satisfying answers to the mineralogy and lithology of the planet's surface. In part, this results from their prime directives: Viking focused on exobiology, Pathfinder focused on technology demonstration. The analytical instruments on board the landers made admirable attempts to extract the mineralogy and geology of Mars, as did countless modeling efforts after the missions. Here we suggest a framework for elucidating martian, or any other planetary geology, through an approach that defines (a) type of information required, (b) explorational strategy harmonious with acquisition of these data, (c) interpretation approach to the data, (d) compatible mission architecture, (e) instrumentation for interrogating rocks and soil. (a) Data required: The composition of a planet is ordered at scales ranging from molecules to minerals to rocks, and from geological units to provinces to planetary-scale systems. The largest ordering that in situ compositional instruments can attempt to interrogate is rock type "aggregate" information. This is what the geologist attempts to identify first. From this, mineralogy can be either directly seen or inferred. From mineralogy can be determined elemental abundances and perhaps the state of the compounds as being crystalline or amorphous. Knowledge of rock type and mineralogy is critical for elucidating geologic process. Mars landers acquired extremely valuable elemental data, but attempted to move from elements to aggregates, but this can only be done by making many assumptions and sometimes giant leaps of faith. Data we believe essential are elements, minerals, degree of ordering of compounds, and the aggregate or rock type that these materials compose. (b) Explorational strategy: A lander should function as a surrogate geologist. Of the total landscape, a geologist sees much, but gives detailed attention to an infinitesimally small amount of what is seen. To acquire samples worth detailed scrutiny, as many samples as possible need examining at a cursory or reconnaissance level. A representative, statistically-meaningful sample number cannot be overemphasized. This maxim still applies to geological exploration of our own planet of which we have abundant knowledge. Analysis of many samples mandates low-power consumption per sample. (c) Data interpretation: No single instrument can analyze the full spectrum of the x-axis. An instrument is optimized for detecting certain material characteristics and must therefore affix itself to some point on the x-axis. Any conclusions drawn about data to the left or right of the instrument's position on this axis must necessarily be derived by inference. Hence, it seems logical to include on a mission, instruments that are not closely spaced in their x-axis-position, and if only two analytical methods are used, as shown, they should start at opposite ends of the axis and work towards the center. As examples, we depict a high-resolution camera to evaluate rock type ("aggregate" state) and mineralogy, and an x-ray diffractometer-fluorescence spectrometer (XRD-XRF) to determine elements, minerals, and the degree of order of materials. (d) Mission architecture: No instrument or suite of instruments can be relied upon to always give truly unequivocal analyses. The suite of instruments should therefore permit conclusions of one instrument to be checked against those of another through closed analytical loops. These "loops" can be structured by a combination of orbital imagery, descent imagery, broad-band site viewing/analysis, and data that cover both x and y axes. For example, the detection of a basaltic-looking rock with a microscope should be checked against the elements detected, the appearance of the rock as a lava flow from descent imagery, and so forth. (e) Instrumentation: To satisfy the above criteria, it is necessary to: (i) See the rock or soil with high resolution + magnification, (ii) Examine many samples, (iii) Consume little power per analysis, (iv) Determine elemental species, (v) Determine mineralogy directly (not inferentially) and the degree of ordering of compounds, (vi) Start analyzing from both ends of the x-axis. Every geologist wants to see the hand sample first, and apply a hand lens to its surface. This has not been the starting point for missions to Mars. Thus, our technology satisfies all these criteria . This XRD-XRF-Optical instrument currently being developed, analyses rock or soil surfaces without the need for sample acquisition or preparation; this satisfies the power criterion, and enables many analyses. The device acquires direct mineralogy and determines elemental species. The embedded endoscopic camera satisfies the critical criterion of close inspection of samples; the fiber optic cable can also be used for IR, LTV, or laser sample analysis. Additional information is contained in the original (Figures).

Marshall, J. R.↗

NASA NTRS1978

Utilization of independent solar flux measurements to eliminate nongeochemical variation in X-ray fluorescence data

It is shown that the direct method of solar activity correction for lunar XRF data produces XRF data with better statistics than uncorrected data. Direct measurements of the solar flux made by Solrad 10 are converted to emissions of the sun from two assumed temperature regions. These emissions are ratioed to produce emission measure ratios, sensitive indicators of shifts in solar activity. The Tucker-Koren model (1971) of the solar flux is used in the calculation of EMRs and in the calculation of theoretical lunar Si, Al, and Mg fluorescence of maria and highland soils. Al/Si(Mg/Si) ratios calculated at a 'normal' EMR of 0.030 are divided by Al/Si(Mg/Si) ratios at particular EMRs. The relationship between EMR and the quotients of this division, called 'correction factors', is well explained by empirically derived power law functions.

Clark, P. E.↗

NASA NTRS1978

A new color correlation method applied to XRF Al/Si ratios and other lunar remote sensing data

Orbital X-ray fluorescence Al/Si intensity ratios, corrected for variations in solar activity, are correlated with normal albedo, elevation measurements from laser altimetry data, and gamma ray data in the 2.75-8.60 MeV range. Each of these data sets is placed into a digital array consisting of 1/4 deg latitude by 1/4 deg longitude pixels. Information relative to the correlation of Al/Si ratios with each of the other data sets is presented in the following forms: (1) histograms are given for each data set to show the frequency distribution within the areas of common coverage; (2) density plots are produced from the plot of a two-dimensional array consisting of the Al/Si ratio vs the other parameter value for each pixel; and (3) color correlation maps are produced by placing the two-dimensional array into a 3 x 3 matrix consisting of nine equal subarrays containing an equal number of data points.

Clark, P. E.↗

NASA NTRS1988

X-ray fluorescence analysis of alloy and stainless steels using a mercuric iodide detector

A mercuric iodide detector was used for the XRF analysis of a number of NBS standard steels, applying a specially developed correction method for interelemental effects. It is shown that, using this method and a good peak-deconvolution technique, the HgI2 detector is capable of achieving resolutions and count rates needed in the XRF anlysis of multielement samples. The freedom from cryogenic cooling and from power supplies necessary for an electrically cooled device makes this detector a very good candidate for a portable instrument.

Kelliher, Warren C.↗

NASA NTRS2005

Methods for identification and verification using vacuum XRF system

Apparatus and methods in which one or more elemental taggants that are intrinsically located in an object are detected by x-ray fluorescence analysis under vacuum conditions to identify or verify the object's elemental content for elements with lower atomic numbers. By using x-ray fluorescence analysis, the apparatus and methods of the invention are simple and easy to use, as well as provide detection by a non line-of-sight method to establish the origin of objects, as well as their point of manufacture, authenticity, verification, security, and the presence of impurities. The invention is extremely advantageous because it provides the capability to measure lower atomic number elements in the field with a portable instrument.

Schramm, Fred↗

NASA NTRS1986

Molecular and Elemental Dust Analyzer (MEDA) for the comet rendezvous asteroid flyby mission

Comets are some to the most primitive bodies in the solar system and therefore should contain elemental, chemical, and isotopic records of the early history of the solar system. An opportunity to perform in situ analyses of a comet nucleus exists with the Comet Rendezvous Asteroid Flyby (CRAF) mission. An integrated gas chromatograph/X-ray fluorescence instrument (MEDA), being proposed for inclusion onboard the CRAF spacecraft, will measure the molecular and elemental constituents of collected dust grains and ices. The gas chromatograph, employing helium ionization detectors and three columns designed to separate light gases, polar gases, and hydrocarbons will measure the volatile compounds of the biogenic elements thermally released from collected dust grains. The sensitivity of the GC for compounds of interest is at the picogram level. X-ray fluorescence utilized cryogenically cooled Si(Li) solid state detectors of nominal 150 eV resolution at 5.9 keV. Based on laboratory work with carbonaceous meteorites, both the GC and XRF can perform meaningful analyses with a few micrograms of collected comet dust.

Ohara, B. J.↗

NASA NTRS1987

Elemental composition of the Martian surface

The Viking landers carried X-ray fluorescence spectrometers (XRFS) to the surface of Mars for direct in-situ measurements of the elemental composition of samples that could be acquired by the surface sampler scoops. A total of 21 samples at two landing sites were acquired and analyzed. In this review, the constraints imposed on the design and operation of the XRFS; the accuracy and precision limitations of XRF; and the interpretation of the results are discussed. The latter includes relevance of the investigation to Martian geological processes, SNC meteorites, the formation and history of Mars, and future mission objectives/capabilities.

Clark, Benton C.↗

NASA NTRS2000

CHEMIN: A Mineralogical Dust Analyzer for the Odyssey Mission to Comet Kopff

The Odyssey spacecraft will be launched in June 2006 and will rendezvous with periodic Comet Kopff in September 2009. Odyssey will initially perform slow flybys of the active Kopff nucleus at distances between 500 and 100 km, and will then be placed in orbit around the nucleus at altitudes between 200 and 50 km. Odyssey's scientific payload of seven instruments includes CHEMIN, a mineralogical dust analyzer, which will make the first direct measurements of the crystal structure and elemental composition of cometary dust. CHEMIN will simultaneously perform X-ray Diffraction and X-ray Fluorescence (XRD/XRF) of individual 1-100 micron dust particles collected passively as the spacecraft is immersed in the comet's coma. The instrument has the geometry of a microfocus X-ray camera, with a postage stamp-sized energy-discriminating CCD in place of the film, and a miniature Cu target X-ray tube as the X-ray source. The CHEMIN flight instrument will weigh less than 2 kg., will have a total volume of about 1 liter, and will operate on 3 watts of power. Individual analyses will require 1-2 hours. XRD maxima from 5 to 65 degrees two-theta will be collected, encompassing definitive peaks for all known minerals. XRF data will be simultaneously collected for elements C through U. The instrument has sufficient resolution to allow Rietveld refinement of the diffraction data. Rock types as complex as basalt have been quantitatively analyzed using a CHEMIN laboratory prototype. Selected examples of diffraction experiments performed on more than 30 minerals and rock types by the CHEMIN laboratory prototype will be discussed.

Blake, David↗