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At least 235 records · Page 13

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.↗

Evidence for Interlayer Collapse of Nontronite on Mars from Laboratory Visible and Near-IR Reflective Spectra

Dioctahedral smectites (e.g., nontronite and montmorillionite) are interpreted to occupy the optical surface of Mars at a number of locations on the basis of spectral features derived from interlayer H2O and MOH (M=Fe(3+)2, Fe(3+)Al, Al2, etc.) as observed by orbiting MRO-CRISM and MEx-OMEGA hyperspectral imaging spectrometers. At wavelengths shorter than approximately 2.7 micrometers, the strongest bands from interlayer H2O occur at approximately 1.4 and 1.9 micrometers from 2v1 and v1+v2, respectively, where v1 and v2 are the fundamental stretching and bending vibrations of the H2O molecule. Smectite MOH vibrations occur near 1.4 micrometers (stretching overtone) and in the region between 2.1 and 2.7 micrometers (stretching + bending combination). Because interlayer H2O can exchange with the martian environment, a number of studies have examined the strength of the interlayer H2O spectral features under Mars-like environmental conditions. The relationship between spectral properties and the underlying crystal structure of the smectites was not determined, and the extent of interlayer H2O removal was not established. We report combined visible and near-IR (VNIR), Mossbauer (MB), and powder X-ray diffraction (XRD) data for samples of the Fe-bearing smectite nontronite where the interlayer was collapsed by complete removal of interlayer H2O.

Morris, Richard V.↗

X-Ray Diffraction Wafer Mapping Method for Rhombohedral Super-Hetero-Epitaxy

A new X-ray diffraction (XRD) method is provided to acquire XY mapping of the distribution of single crystals, poly-crystals, and twin defects across an entire wafer of rhombohedral super-hetero-epitaxial semiconductor material. In one embodiment, the method is performed with a point or line X-ray source with an X-ray incidence angle approximating a normal angle close to 90 deg, and in which the beam mask is preferably replaced with a crossed slit. While the wafer moves in the X and Y direction, a narrowly defined X-ray source illuminates the sample and the diffracted X-ray beam is monitored by the detector at a predefined angle. Preferably, the untilted, asymmetric scans are of {440} peaks, for twin defect characterization.

Park, Yoonjoon↗

Oxygen and Magnesium Isotopic Compositions of Asteroidal Materials Returned from Itokawa by the Hayabusa Mission

The Hayabusa spacecraft made two touchdowns on the surface of Asteroid 25143 Itokawa on November 20th and 26th, 2005. The Asteroid 25143 Itokawa is classified as an S-type asteroid and inferred to consist of materials similar to ordinary chondrites or primitive achondrites [1]. Near-infrared spectroscopy by the Hayabusa spacecraft proposed that the surface of this body has an olivine-rich mineral assemblage potentially similar to that of LL5 or LL6 chondrites with different degrees of space weathering [2]. The spacecraft made the reentry into the Earth s atmosphere on June 12th, 2010 and the sample capsule was successfully recovered in Australia on June 13th, 2010. Although the sample collection processes on the Itokawa surface had not been made by the designed operations, more than 1,500 grains were identified as rocky particles in the sample curation facility of JAXA, and most of them were judged to be of extraterrestrial origin, and definitely from Asteroid Itokawa on November 17th, 2010 [3]. Although their sizes are mostly less than 10 microns, some larger grains of about 100 microns or larger were also included. The mineral assembly is olivine, pyroxene, plagioclase, iron sulfide and iron metal. The mean mineral compositions are consistent with the results of near-infrared spectroscopy from Hayabusa spacecraft [2], but the variations suggest that the petrologic type may be smaller than the spectroscopic results. Several tens of grains of relatively large sizes among the 1,500 grains will be selected by the Hayabusa sample curation team for preliminary examination [4]. Each grain will be subjected to one set of preliminary examinations, i.e., micro-tomography, XRD, XRF, TEM, SEM, EPMA and SIMS in this sequence. The preliminary examination will start from the last week of January 2011. Therefore, samples for isotope analyses in this study will start from the last week of February 2011. By the time of the LPSC meeting we will have measured the oxygen and magnesium isotopic composition of several grains. We will present the first results from the isotope analyses that will have been performed.

Yurimoto, H↗

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.↗

Cryogenic Origin for Mars Analog Carbonates in the Bockfjord Volcanic Complex Svalbard (Norway)

The Sverrefjell and Sigurdfjell eruptive centers in the Bockfjord Volcanic Complex (BVC) on Svalbard (Norway) formed by subglacial eruptions ca. 1 Ma ago. These eruptive centers carry ubiquitous magnesian carbonate deposits including dolomitemagnesite globules similar to those in the Martian meteorite ALH84001. Carbonates in mantle xenoliths are dominated by ALH84001 type carbonate globules that formed during quenching of CO2-rich mantle fluids. Lava hosted carbonates include ALH84001 type carbonate globules occurring throughout lava vesicles and microfractures and massive carbonate deposits associated with vertical volcanic vents. Massive carbonates include < or equal 5 cm thick magnesite deposits protruding downwards into clear blue ice within volcanic vents and carbonate cemented lava breccias associated with volcanic vents. Carbonate cements comprise layered deposits of calcite, dolomite, huntite, magnesite and aragonite associated with ALH84001 type carbonate globules lining lava vesicles. Combined Mossbauer, XRD and VNIR data show that breccia carbonate cements at Sverrefjell are analog to Comanche carbonates at Gusev crater.

Amundsen, H. E. F.↗

In Situ Strategy of the 2011 Mars Science Laboratory to Investigate the Habitability of Ancient Mars

The ten science investigations of the 2011 Mars Science Laboratory (MSL) Rover named "Curiosity" seek to provide a quantitative assessment of habitability through chemical and geological measurements from a highly capable robotic' platform. This mission seeks to understand if the conditions for life on ancient Mars are preserved in the near-surface geochemical record. These substantial payload resources enabled by MSL's new entry descent and landing (EDL) system have allowed the inclusion of instrument types nevv to the Mars surface including those that can accept delivered sample from rocks and soils and perform a wide range of chemical, isotopic, and mineralogical analyses. The Chemistry and Mineralogy (CheMin) experiment that is located in the interior of the rover is a powder x-ray Diffraction (XRD) and X-ray Fluorescence (XRF) instrument that provides elemental and mineralogical information. The Sample Analysis at Mars (SAM) suite of instruments complements this experiment by analyzing the volatile component of identically processed samples and by analyzing atmospheric composition. Other MSL payload tools such as the Mast Camera (Mastcam) and the Chemistry & Camera (ChemCam) instruments are utilized to identify targets for interrogation first by the arm tools and subsequent ingestion into SAM and CheMin using the Sample Acquisition, Processing, and Handling (SA/SPaH) subsystem. The arm tools include the Mars Hand Lens Imager (MAHLI) and the Chemistry and Alpha Particle X-ray Spectrometer (APXX). The Dynamic Albedo of Neutrons (DAN) instrument provides subsurface identification of hydrogen such as that contained in hydrated minerals

Mahaffy, Paul R.↗

Chemical and Mineralogical Characterization of Acid-Sulfate Alteration of Basaltic Material on Mauna Kea Volcano, Hawaii: Jarosite and Hydrated Halloysite

Sulfates have been identified on the martian surface during robotic surface exploration and by orbital remote sensing. Measurements at Meridiani Planum (MP) by the Alpha-Particle X-ray Spectrometer (APXS) and Mossbauer (MB) instruments on the Mars Exploration Rover Opportunity document the presence of a ubiquitous sulfate-rich outcrop (20-40% SO3) that has jarosite as an anhydrous Fe3+-sulfate [1- 3]. The presence of jarosite implies a highly acidic (pH <3) formation environment [4]. Jarosite and other sulfate minerals, including kieserite, gypsum, and alunite have also been identified in several locations in orbital remote sensing data from the MEx OMEGA and MRO CRISM instruments [e.g. 5-8]. Acid sulfate weathering of basaltic materials is an obvious pathway for formation of sulfate-bearing phases on Mars [e.g. 4, 9, 10]. In order to constrain acid-sulfate pathways on Mars, we are studying the mineralogical and chemical manifestations of acid-sulfate alteration of basaltic compositions in terrestrial environments. We have previously shown that acidsulfate alteration of tephra under hydrothermal conditions on the Puu Poliahu cone (summit region of Mauna Kea volcano, Hawaii) resulted in jarosite and alunite as sulfate-bearing alteration products [11-14]. Other, more soluble, sulfates may have formed, but were leached away by rain and melting snow. Acidsulfate processes on Puu Poliahu also formed hematite spherules similar (except in size) to the hematite spherules observed at MP as an alteration product [14]. Phyllosilicates, usually smectite }minor kaolinite are also present as alteration products [13]. We discuss here an occurrence of acid-sulfate alteration on Mauna Kea Volcano (Hawaii). We report VNIR spectra (0.35-2.5 microns ASD spectrometer), Mossbauer spectra (MER-like ESPI backscatter spectrometer), powder XRD (PANalytical), and major element chemical compositions (XRF with LOI and Fe redox) for comparison to similar data acquired or to be acquired by MRO-CRISM and MEx OMEGA, MERMB, MSL-CheMin, and MER and MSL APXS, respectively.

Graff, Trevor G.↗

Space Shuttle Columbia Post-Accident Analysis and Investigation

Although the loss of the Space Shuttle Columbia and its crew was tragic, the circumstances offered a unique opportunity to examine a multitude of components which had experienced one of the harshest environments ever encountered by engineered materials: a break up at a velocity in excess of Mach 18 and an altitude exceeding 200,000 feet (63 KM), resulting in a debris field 645 miles/l,038 KM long and 10 miles/16 KM wide. Various analytical tools were employed to ascertain the sequence of events leading to the disintegration of the Orbiter and to characterize the features of the debris. The testing and analyses all indicated that a breach in a left wing reinforced carbon/carbon composite leading edge panel was the access point for hot gasses generated during re-entry to penetrate the structure of the vehicle and compromise the integrity of the materials and components in that area of the Shuttle. The analytical and elemental testing utilized such techniques as X-Ray Diffraction (XRD), Energy Dispersive X-Ray (EDX) dot mapping, Electron Micro Probe Analysis (EMPA), and X-Ray Photoelectron Spectroscopy (XPS) to characterize the deposition of intermetallics adjacent to the suspected location of the plasma breach in the leading edge of the left wing, Fig. 1.

McDanels, Steven J.↗

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.↗

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.↗

Fischer-Tropsch Cobalt Catalyst Improvements with the Presence of TiO2, La2O3, and ZrO2 on an Alumina Support

The objective of this study was to evaluate the effect of titanium oxide, lanthanum oxide, and zirconium oxide on alumina supported cobalt catalysts. The hypothesis was that the presence of lanthanum oxide, titanium oxide, and zirconium oxide would reduce the interaction between cobalt and the alumina support. This was of interest because an optimized weakened interaction could lead to the most advantageous cobalt dispersion, particle size, and reducibility. The presence of these oxides on the support were investigated using a wide range of characterization techniques such as SEM, nitrogen adsorption, x-ray diffraction (XRD), temperature programmed reduction (TPR), temperature programmed reduction after reduction (TPR-AR), and hydrogen chemisorptions/pulse reoxidation. Results indicated that both La2O3 and TiO2 doped supports facilitated the reduction of cobalt oxide species in reference to pure alumina supported cobalt catalysts, however further investigation is needed to determine the effect of ZrO2 on the reduction profile. Results showed an increased corrected cluster size for all three doped supported catalysts in comparison to their reference catalysts. The increase in reduction and an increase in the cluster size led to the conclusion that the support-metal interaction weakened by the addition of TiO2 and La2O3. It is also likely that the interaction decreased upon presence of ZrO2 on the alumina, but further research is necessary. Preliminary results have indicated that the alumina-supported catalysts with titanium oxide and lanthanum oxide present are of interest because of the weakened cobalt support interaction. These catalysts showed an increased extent of reduction, therefore more metallic cobalt is present on the support. However, whether or not there is more cobalt available to participate in the Fischer-Tropsch synthesis reaction (cobalt surface atoms) depends also on the cluster size. On one hand, increasing cluster size alone tends to decrease the active site density; on the other hand, by increasing the size of the cobalt clusters, there is less likelihood of forming oxidized cobalt complexes (cobalt aluminate) during Fischer-Tropsch synthesis. Thus, from the standpoint of stability, improving the extent of reduction while increasing the particle size slightly may be beneficial for maintaining the sites, even if there is a slight decrease in overall initial active site density.

Klettlinger, Jennifer Lindsey Suder↗

Insights into the Sulfur Mineralogy of Martian Soil at Rocknest, Gale Crater, Enabled by Evolved Gas Analyses

The first solid samples analysed by the Chemistry and Mineralogy (CheMin) instrument and Sample Analysis at Mars (SAM) instrument suite on the Mars Science Laboratory (MSL) consisted of < 150 m fines sieved from aeolian bedform material at a site named Rocknest. All four samples of this material analyzed by SAM s evolved gas analysis mass spectrometry (EGA-MS) released H2O, CO2, O2, and SO2 (Fig. 1), as well as H2S and possibly NO. This is the first time evolved SO2 (and evolved H2S) has been detected from thermal analysis of martian materials. The identity of these evolved gases and temperature (T) of evolution can support mineral detection by CheMin and place constraints on trace volatile-bearing phases present below the CheMin detection limit or difficult to characterize with XRD (e.g., X-ray amorphous phases). Constraints on phases responsible for evolved CO2 and O2 are detailed elsewhere [1,2,3]. Here, we focus on potential constraints on phases that evolved SO2, H2S, and H2O during thermal analysis.

McAdam, A.↗

Basaltic Soil of Gale Crater: Crystalline Component Compared to Martian Basalts and Meteorites

A significant portion of the soil of the Rocknest dune is crystalline and is consistent with derivation from unweathered basalt. Minerals and their compositions are identified by X-ray diffraction (XRD) data from the CheMin instrument on MSL Curiosity. Basalt minerals in the soil include plagioclase, olivine, low- and high-calcium pyroxenes, magnetite, ilmenite, and quartz. The only minerals unlikely to have formed in an unaltered basalt are hematite and anhydrite. The mineral proportions and compositions of the Rocknest soil are nearly identical to those of the Adirondack-class basalts of Gusev Crater, Mars, inferred from their bulk composition as analyzed by the MER Spirit rover.

Treiman, A. H.↗

The Amorphous Component in Martian Basaltic Soil in Global Perspective from MSL and MER Missions

The mineralogy instrument CheMin onboard the MSL rover Curiosity analyzed by transmission XRD [1] the <150 microns size fraction of putative global basaltic martian soil from scoops 4 and 5 of the Rocknest aeolian bedform (sol 81-120). Here, we combine chemical (APXS) and mineralogical (Mossbauer; MB) results from the MER rovers with chemical (APXS) and mineralogical (CheMin) results from Curiosity to constrain the relative proportions of amorphous and crystalline components, the bulk chemical composition of those components, and the

Morris, R. V.↗

Effect of PdO on TiO(sub2) Loading on Chemochromic Detection of Hydrogen

Safety is always a concern in all applications that utilize hydrogen (H(sub2)) in one form or the other. Hydrogen leaks are invisible and odorless. In addition, blending odorants or additives into hydrogen in a manner similar to natural gas is generally undesirable for certain applications including proton exchange membrane fuel cells. To facilitate detection of the location of hydrogen leaks, a special chemochromic H(sub2) sensing material that employs titania (Ti0(sub2)) supported palladium oxide (PdO) pigments encapsulated within a special silicone matrix has been developed at the Florida Solar Energy Center (FSEC). Several batches of PdO H(sub2) sensing pigments were synthesized using various Ti0(sub2) supports and their hydrogen detection activity determined. TEM and Particle size distribution analysis showed that smaller particles with hemispherical crystalline structure produced faster coloration kinetics when exposed to H(sub2) gas. However, uniformly distributed PdO particles on the Ti0(sub2) surface displayed greater color contrast, quantified by delta epsilon measurements. XRD analysis indicated that the crystalline phase of Ti0(sub2) had no effect on the chemochromic performance of the pigments in laboratory environment.

Mohajeri, Nahid↗

Estimation of Supraglacial Dust and Debris Geochemical Composition via Satellite Reflectance and Emissivity

We demonstrate spectral estimation of supraglacial dust, debris, ash and tephra geochemical composition from glaciers and ice fields in Iceland, Nepal, New Zealand and Switzerland. Surface glacier material was collected and analyzed via X-ray fluorescence spectroscopy (XRF) and X-ray diffraction (XRD) for geochemical composition and mineralogy. In situ data was used as ground truth for comparison with satellite derived geochemical results. Supraglacial debris spectral response patterns and emissivity-derived silica weight percent are presented. Qualitative spectral response patterns agreed well with XRF elemental abundances. Quantitative emissivity estimates of supraglacial SiO2 in continental areas were 67% (Switzerland) and 68% (Nepal), while volcanic supraglacial SiO2 averages were 58% (Iceland) and 56% (New Zealand), yielding general agreement. Ablation season supraglacial temperature variation due to differing dust and debris type and coverage was also investigated, with surface debris temperatures ranging from 5.9 to 26.6 C in the study regions. Applications of the supraglacial geochemical reflective and emissive characterization methods include glacier areal extent mapping, debris source identification, glacier kinematics and glacier energy balance considerations.

Casey, Kimberly Ann↗

Calcium-Magnesium-Aluminosilicate (CMAS) Reactions and Degradation Mechanisms of Advanced Environmental Barrier Coatings

The thermochemical reactions between calcium-magnesium-aluminosilicate- (CMAS-) based road sand and several advanced turbine engine environmental barrier coating (EBC) materials were studied. The phase stability, reaction kinetics and degradation mechanisms of rare earth (RE)-silicates Yb2SiO5, Y2Si2O7, and RE-oxide doped HfO2 and ZrO2 under the CMAS infiltration condition at 1500 C were investigated, and the microstructure and phase characteristics of CMAS-EBC specimens were examined using Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD). Experimental results showed that the CMAS dissolved RE-silicates to form crystalline, highly non-stoichiometric apatite phases, and in particular attacking the silicate grain boundaries. Cross-section images show that the CMAS reacted with specimens and deeply penetrated into the EBC grain boundaries and formed extensive low-melting eutectic phases, causing grain boundary recession with increasing testing time in the silicate materials. The preliminary results also showed that CMAS reactions also formed low melting grain boundary phases in the higher concentration RE-oxide doped HfO2 systems. The effect of the test temperature on CMAS reactions of the EBC materials will also be discussed. The faster diffusion exhibited by apatite and RE-doped oxide phases and the formation of extensive grain boundary low-melting phases may limit the CMAS resistance of some of the environmental barrier coatings at high temperatures.

Ahlborg, Nadia L.↗