ALBERT

Description: The Rocknest aeolian deposit is similar to aeolian features analyzed by the Mars Exploration Rovers (MER) Spirit and Opportunity. The fraction of sand 〈150 micron in size contains approx. 55% crystalline material consistent with a basaltic heritage, and approx. 45% X-ray amorphous material. The amorphous component of Rocknest is Fe-rich and Si-poor, and is the host of the volatiles (H2O, O2, SO2, CO2, and Cl) detected by the Surface Analysis at Mars (SAM) instrument and of the fine-grained nanophase oxide (npOx) component first described from basaltic soils analyzed by MER. The similarity between soils and aeolian materials analyzed at Gusev crater, Meridiani Planum and Gale crater implies locally sourced, globally similar basaltic materials, or globally and regionally sourced basaltic components deposited locally at all three locations.

Description: 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.

Description: The search for evidence of extant or extinct life on Mars will initially be a search for evidence of present or past conditions supportive of life (e.g., evidence of water), not for life itself. Definitive evidence of past or present water activity lies in the discovery of: * Hydrated minerals: The "rock type" hosting the hydrated minerals could be igneous, metamorphic, or sedimentary, with only a minor hydrated mineral phase. Therefore, the identification of minor phases is important. * Clastic sediments: Clastic sediments are commonly identified by the fact that they contain minerals of disparate origin that could only have come together as a mechanical mixture. Therefore, the identification of all minerals present in a mixture to ascertain mineralogical source regions is important. * Hydrothermal precipitates and chemical sediments: Some chemical precipitates are uniquely identified only by their structure. For example, Opal A, Opal CT, tridymite, crystobalite, high and low Quartz all have the same composition (SiO2) but different crystal structures indicative of different environments - from hydrothermal hydrothermal formation to low temperature precipitation. Other silica types such as stishovite can provide evidence of shock metamorphism. Therefore, identification of crystal structures and structural polymorphs is important. The elucidation of the nature of the Mars soil will require the identification of mineral components that can unravel its history and the history of the Mars atmosphere.

Description: A miniature CHEMIN XRD/XRF (X-Ray Diffraction/X-Ray Fluourescence) instrument is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed in order to enable XRD analysis on an extraterrestrial body is how best to obtain a representative sample powder for analysis. For XRD powder diffraction analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a 2-dimensional detector as used in the CHEMIN instrument will produce good results with poorly prepared powders, the quality of the data will improve if the sample is fine-grained and randomly oriented. An Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL is an effective mechanism of sampling rock to produce cores and powdered cuttings. It requires low axial load (〈 5N) and thus offers significant advantages for operation from lightweight platforms and in low gravity environments. The USDC is lightweight (〈0.5kg), and can be driven at low power (〈5W) using duty cycling. It consists of an actuator with a piezoelectric stack, ultrasonic horn, free-mass, and drill bit. The stack is driven with a 20 kHz AC voltage at resonance. The strain generated by the piezoelectric is amplified by the horn by a factor of up to 10 times the displacement amplitude. The tip impacts the free-mass and drives it into the drill bit in a hammering action. The free-mass rebounds to interact with the horn tip leading to a cyclic rebound at frequencies in the range of 60-1000 Hz. It does not require lubricants, drilling fluid or bit sharpening and it has the potential to operate at high and low temperatures using a suitable choice of piezoelectric material. To assess whether the powder from an ultrasonic drill would be adequate for analyses by an XRD/XRF spectrometer such as CHEMIN, powders obtained from the JPL ultrasonic drill were analyzed and the results were compared to carefully prepared powders obtained using a laboratory bench scale Retsch mill.

Description: Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

Description: A miniature XRD/XRF (X-ray diffraction / X-ray fluorescence) instrument, CHEMIN, is currently being developed for definitive mineralogic analysis of soils and rocks on Mars. One of the technical issues that must be addressed to enable remote XRD analysis is how best to obtain a representative sample powder for analysis. For powder XRD analyses, it is beneficial to have a fine-grained sample to reduce preferred orientation effects and to provide a statistically significant number of crystallites to the X-ray beam. Although a two-dimensional detector as used in the CHEMIN instrument will produce good results even with poorly prepared powder, the quality of the data will improve and the time required for data collection will be reduced if the sample is fine-grained and randomly oriented. A variety of methods have been proposed for XRD sample preparation. Chipera et al. presented grain size distributions and XRD results from powders generated with an Ultrasonic/Sonic Driller/Corer (USDC) currently being developed at JPL. The USDC was shown to be an effective instrument for sampling rock to produce powder suitable for XRD. In this paper, we compare powder prepared using the USDC with powder obtained with a miniaturized rock crusher developed at JPL and with powder obtained with a rotary tungsten carbide bit to powders obtained from a laboratory bench-scale Retsch mill (provides benchmark mineralogical data). These comparisons will allow assessment of the suitability of these methods for analysis by an XRD/XRF instrument such as CHEMIN.

Description: Mineral identification is a critical component of Mars Astrobiological missions. Chemical or elemental data alone are not definitive because a single elemental or chemical composition or even a single bonding type can represent a range of substances or mineral assemblages. Minerals are defined as unique structural and compositional phases that occur naturally. There are about 15,000 minerals that have been described on Earth, all uniquely identifiable via diffraction methods. There are likely many minerals yet undiscovered on Earth, and likewise on Mars. If an unknown phase is identified on Mars, it can be fully characterized by structural (X-ray Diffraction, XRD) and elemental analysis (X-ray Fluorescence, XRF) without recourse to other data because XRD relies on the principles of atomic arrangement for its determinations. XRD is the principal means of identification and characterization of minerals on Earth.

Description: Mineralogical analysis is a critical component of planetary surface exploration. Chemical data alone leave serious gaps in our understanding of the surfaces of planets where complex minerals may form in combination with H, S, and halogens. On such planets (e.g., Mars) a single chemical composition may represent a range of mineral assemblages. For example, Viking chemical analyses of excavated duricrust indicate that Mg and S are correlated and ~10% MgSO4 (anhydrous weight) is a likely cementing agent. Pathfinder chemical data support a similar abundance of MgSO4 in the most altered materials. However, there are many possible Mg-sulfates with widely varying hydration states (including dehydrated and 1-, 2-, 3-, 4-, 5-, 6-, and 7-hydrates). In addition, other sulfate minerals such as gypsum (CaSO4 .2H2O) and other salts containing Cl may also exist. X-ray diffraction (XRD) has the ability to decipher mixtures of these phases that would be difficult, if not impossible to unravel using only chemical or spectral data.

Description: The Mars Science Laboratory rover, Curiosity, landed at Gale crater in August 2012 and has been investigating a sequence of dominantly fluviolacustrine sediments deposited 3.6-3.2 billion years ago. Curiosity collects quantitative mineralogical data with the CheMin XRD/XRF instrument and quantitative chemical data with the APXS and ChemCam instruments. These datasets show stratigraphic mineralogical and geochemical variability that suggest a complex aqueous history. The Murray Formation, primarily composed of fine-laminated mudstone, has been studied in detail since the arrival at the Pahrump Hills in September 2014. CheMin data from four samples show variable amounts of iron oxides, phyllosilicates, sulfates, amorphous and crystalline silica, and mafic silicate minerals. Geochemical data throughout the section show that there is significant variability in Zn, Ni, and Mn concentrations. Mineralogical and geochemical trends with stratigraphy suggest one of possibly several aqueous episodes involved alteration in an open system under acidic pH, though other working hypotheses may explain these and other trends. Data from the Murray Formation contrast with those collected from the Sheepbed mudstone located approximately 60 meters below the base of the Murray Formation, which showed evidence for diagenesis in a closed system at circumneutral pH. Ca-sulfates filled late-stage veins in both mudstones.

Description: The CheMin X-ray diffraction (XRD) instrument onboard the Mars Science Laboratory rover Curiosity in Gale Crater, Mars, discovered smectite in drill fines of the Sheepbed mudstone at Yellowknife Bay (YNB). The mudstone has a basaltic composition, and the XRD powder diffraction pattern shows smectite 02l diffraction bands peaking at 4.59 A for targets John Klein and Cumberland, consistent with tri-octahedral smectites (saponite). From thermal analysis, the saponite abundance is ~20 wt. %. Among terrestrial analogues we have studied, ferrian saponite from Griffith Park (Los Angeles, CA) gives the best match to the position of the 02l diffraction band of YNB saponites. Here we describe iron-rich saponites from a terrestrial perspective, with a focus on Griffith saponite, and discuss their implications for the mineralogy of Sheepbed saponite and its formation pathways. Iron-rich saponite: Iron-rich saponite on the Earth is recognized as a low-temperature (〈100 C), authigenic alteration product of basalt [e.g., 4-16]. In the discussion that follows, we reference the position of the 02l band because it is a measure of the unit cell 'b' dimension of the octahedral layer and thus the cations (including Fe redox state) in the octahedral layer. Ordinarily, the 06l band near 1.5 A is used to determine the 'b' dimension of smectite, but this band is not accessible with MSL CheMin instrument. For reference, a ferrosaponite (i.e., Fe2+ saponite) studied by [15] has a 02l spacing of 4.72 A and Fe3+/Fe = 0.27 [15]. Samples of terrestrial ferrosaponite, however, are reported to oxidize on the timescale of days when removed from their natural environment and not protected from oxidation. The Griffith saponite is Mg-rich ferrian saponite, and sample AMNH 89172 has an 02l spacing of 4.59 A (same as the Sheepbed saponites) and Fe3+/Fe = 0.64 [3]. This similarity suggests that Sheepbed saponites are ferrian (incompletely oxidized ferrosaponite). More oxidized Griffith saponites (Fe3+/Fe 〉 0.90) have somewhat smaller 02l d-spacings and also show Mossbauer evidence for an XRD amorphous Fe-bearing phase (e.g., ferrihydrite, hisingerite, superparamagnetic ferric oxides, etc.). The Griffith saponite occurs as vesicle fills, as replacements of olivine, and as replacements of mesostasis (basaltic glass). Similar occurrence modes are reported elsewhere. Hisingerite has been proposed by [13] as the alteration product of ferrian saponite whose precursor by oxidation was ferrosaponite.