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At least 181 records · Page 10

Correlative X-ray micro-nanotomography with scanning electron microscopy at the Advanced Light Source

Geological samples are inherently multi-scale. Understanding their bulk physical and chemical properties requires characterization down to the nano-scale. A powerful technique to study the three-dimensional microstructure is X-ray tomography, but it lacks information about the chemistry of samples. To develop a methodology for measuring the multi-scale 3D microstructure of geological samples, correlative X-ray micro- and nanotomography were performed on two rocks followed by scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS) analysis. The study was performed in five steps: (i) micro X-ray tomography was performed on rock sample cores, (ii) samples for nanotomography were prepared using laser milling, (iii) nanotomography was performed on the milled sub-samples, (iv) samples were mounted and polished for SEM analysis and (v) SEM imaging and compositional mapping was performed on micro and nanotomography samples for complimentary information. Correlative study performed on samples of serpentine and basalt revealed multiscale 3D structures involving both solid mineral phases and pore networks. Significant differences in the volume fraction of pores and mineral phases were also observed dependent on the imaging spatial resolution employed. This highlights the necessity for the application of such a multiscale approach for the characterization of complex aggregates such as rocks. Information acquired from the chemical mapping of different phases was also helpful in segmentation of phases that did not exhibit significant contrast in X-ray imaging. Adoption of the protocol used in this study can be broadly applied to 3D imaging studies being performed at the Advanced Light Source and other user facilities.

58 GEOSCIENCES↗

Evolved Gas Analyses of Mudstones from the Vera Rubin Ridge

The Sample Analysis at Mars (SAM) instrument suite on the Mars Science Laboratory (MSL) rover has been essential in understanding volatile-bearing phases in Gale Crater materials. SAM’s evolved gas analysis mass spectrometry (EGA-MS) has detected H2O, CO2, O2, H2, SO2, H2S, HCl, NO, and other trace gases, including organic fragments, in many samples. The identity and evolution temperature of evolved gases can support CheMin instrument mineral detection and place constraints on trace volatile-bearing phases or phases difficult to characterize with X-ray diffraction (e.g., amorphous phases). For the past ~500 sols, MSL has been exploring the Vera Rubin Ridge (VRR), which exhibits a striking hematite signature in orbital remote sensing data, in order to understand the depositional and diagenetic history recorded in the rocks and how it relates to the underlying Murray Formation. Four rock samples were drilled, one from the Blunts Point Member (Duluth, DU), one from the Pettegrrove Point Member (Stoer, ST), and two from the Jura Member. The Jura Member displays differences in color, summarized as grey and red, and a key goal was to constrain the cause of this color difference and the associated implications for depositional or post-depositional conditions. To investigate, a grey (Highfield, HF) and a red (Rock Hall, RH) Jura sample were drilled. Here we will give an overview of results from SAM EGA-MS analyses of VRR materials, with some comparisons to analyses of samples of the underlying Murray.

McAdam, A. C.↗

Asteroid-meteorite connection: Regolith effects implied by lunar reflectance spectra

The effect of soil formation on the spectral characteristics of asteroids were estimated in situ properties of materials affected by the space environment other than those associated with agglutinates. In his initial survey of the reflectance properties of lunar samples, J.B. Adams measured a few chips from the exterior and interior of Apollo rocks. For Apollo 12 basalts 12053-12063 , the exterior and interior spectra exhibited strong absorption bands which were very similar in nature; the exterior fragment was a bit brighter, which was attributed to microbrecciation. Mature lunar soils measured undisturbed surface areas at the landing sites. It was hypothesized that freshly exposed material at fresh impact craters should be comparable to powdered rock samples in the laboratory. This expected trend seemed to be true with the early reflectance data, but as the more complete near-infrared data has become available it is clear that there is no simple correspondence of rock type (laboratory powder or chip measurement) to freshly exposed surface material (telescopic measurements of fresh crater classes).

Pieters, C. M.↗

SPADE: A Rock Crushing and Sample Handling System Developed for Mars Missions

Access to the interior of rocks on Mars is an important goal for understanding Mars petrology and geologic history. The spectral signature of the potentially diverse mineralogy of rocks on Mars is veiled by the ubiquitous dust and may be further hidden by weathered rind. We have developed a rock crusher and sample distribution system under the auspices of NASA s PIDDP program. We call it the SPADE : the Sample Processing and Distribution Experiment. Its purpose is to access the interiors of rocks on Mars and prepare samples for analysis by a suite of in situ instruments.

Hansen, Candice J.↗

Laboratory evaluation of cyclic underground hydrogen storage in the Temblor sandstone of the San Joaquin Basin, California

Underground Hydrogen Storage (UHS) in depleted oil and gas reservoirs could provide a cost-effective solution to balance seasonal fluctuations in renewable energy generation. However, data and knowledge on UHS at subsurface conditions are limited so it is difficult to estimate how effective this type of storage could be. In this study, we perform high pressure experiment to measure the effectiveness of cyclic hydrogen (H 2 ) storage in a specimen of Temblor sandstone retrieved from the San Joaquin Basin of California. Our experiment mimics reservoir pressure conditions to measure H 2 -brine relative permeability and fluid-rock interactions over the course of ten charging and discharging cycles. Initial gas breakthrough occurred at 15 % to 25 % H2 saturation in the specimen with 3 % NaCl brine as the resident fluid. Continuing injecting to 4 pore volumes (PV) of H 2 yielded an asymptotic H 2 saturation of 38 % to 41 %, a level often referred to as the irreducible gas saturation based on two-phase flow. The boundary condition in this study mimics the near wellbore region, which experiences bi-directional H 2 flow. This bi-directional flow led to evaporative drying of the specimen resulting in 94 % H 2 saturation at the end of 10th cycle. This indicates that cyclic flow and evaporative drying can lead to more efficient reservoir storage where a larger fraction of the reservoir porosity is usable to store H 2 . The produced gas stream consisted of H 2 mixed with 8 % to 22 % H 2 O, indicating formation dry-out by evaporation. Meanwhile, produced water chemistry indicated calcite and silicate dissolution, with calcite sourced from fossil fragments. This led to a loss of cementation and weakened the rock sample. Combined, our results indicate dry-out, compaction, increased H 2 saturation, rock weakening, and permeability loss during cyclic UHS. Overall, we anticipate that the combined effects should lead to higher than anticipated UHS storage efficiency per volume of sandstone reservoir rock.

08 HYDROGEN↗

Application of a modified method of ultrasonic measurements for determination of elastic moduli of rocks

The velocities of elastic waves with quasi-longitudinal and quasi-transverse polarizations in a spherical rock sample have been measured. The experimental values of velocities are used to calculate 21 elastic moduli of the sample. For comparison, the effective elastic properties of the sample are simulated based on the data on the crystallographic textures of rock-forming minerals obtained by neutron diffraction. It is shown that the largest discrepancy between the model predictions and experimental velocity values is observed for transversely polarized waves.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Indigenous Organic Molecular Biosignatures are Detectable via ToF-SIMS of a Kerogen-rich Jurassic Clay

Time of Flight - Secondary Ion Mass Spectrometry (ToF-SIMS) is a Mass Spectrometry (MS) imaging technique that can be used in conjunction with traditional organic geochemical analysis (organics extracted from a crushed sample) in order to determine how molecules observed in the organic extracts were incorporated into a particular rock sample. This type of analysis may be used on samples collected as part of Mars Sample Return (MSR) in order to determine if potential organic compounds were indigenous to Mars or whether they are contaminants.Here we show that Organic Molecular Biosignatures (OMBs including steranes and derivatives of a carotenoid) are detectable via ToF-SIMS within a Jurassic mudstone. The OMBs are only detectable in areas with high organic carbon, likely kerogen, indicating that they are indigenous to the rock. We conclude that: I) Indigenous OMBs are detectable via ToF-SIMS in ancient, kerogen-rich samples; II) the presence of a molecular ion strengthens the interpretation of ToF-SIMS spectra of complex natural material, and III) the spatial co-occurrence of kerogen and potentially indigenous OMBs in ancient sediments is a valid test of their character. These conclusions are directly relevant to MSR sample selection as well as the analysis of MSR samples upon return.

Pasterski, Michael↗

A Nationwide Study of REEs in Geothermal and Produced Waters: Final Results

This study sampled and analyzed water from around the United States. Activities that enhanced this work included the co-collection of rock samples, the statistical analysis of the data with an ESOM, and evaluation of extraction by three promising methods. These activities led to five conclusions (1) REEs sometimes occur in continental groundwater in excess of 1000-times their seawater concentrations. (2) REEs exist as a trace (ng/L) component in all analyzed samples. (3) The traditional distinction of light (Z=57-64) and heavy (Z=65-71) REEs in rock-mineral chemistry applies to aqueous chemistry. (4) REE content is not significantly controlled by lithology, reservoir temperature, nor salinity. (5) REE concentration, both in sampled basins and neural network predictions of potential, appears to be spatially co-associated, with the basin mattering more than formation. These five conclusions have advanced the scientific understanding of REEs in subsurface geothermal systems. These conclusions suggest that future work study three questions. (1) What is the spatially–dependent variable that controls REE concentration? (2) Does the output of the ESOM change significantly as input samples are grown in both number and spatial extent? (3) Compared with next-gen analytical techniques, under what metrics does the current method for aqueous REE analysis perform well, and under what metrics is it surpassed? Some of these questions are being investigated in new projects that grew from this work, others would benefit from government support.

15 GEOTHERMAL ENERGY↗

Lead isotope systematics of some igneous rocks from the Egyptian Shield

Lead isotope data on whole-rock samples and two feldspar separates for a variety of Pan-African (late Precambrian) igneous rocks for the Egyptian Shield are presented. It is pointed out that the eastern desert of Egypt is a Late Precambrian shield characterized by the widespread occurrence of granitic plutons. The lead isotope ratios may be used to delineate boundaries between Late Precambrian oceanic and continental environments in northeastern Africa. The samples belong to three groups. These groups are related to a younger plutonic sequence of granites and adamellites, a plutonic group consisting of older tonalites to granodiorites, and the Dokhan volcanic suite.

Gillespie, J. G.↗

On the strength of transversely isotropic rocks: On the strength of transversely isotropic rocks

Accurate prediction of strength in rocks with distinct bedding planes requires knowledge of the bedding plane orientation relative to the load direction. Thermal softening adds complexity to the problem since it is known to have significant influence on the strength and strain localization properties of rocks. In this paper, we utilize a recently proposed thermoplastic constitutive model appropriate for rocks exhibiting transverse isotropy in both the elastic and plastic responses to predict their strength and strain localization properties. Recognizing that laboratory-derived strengths can be influenced by material and geometric inhomogeneities of the rock samples, we consider both stress-point and boundary-value problem simulations of rock strength behavior. Both plane strain and 3D loading conditions are considered. Results of the simulations of the strength of a natural Tournemire shale and a synthetic transversely isotropic rock suggest that the mechanical model can reproduce the general U-shaped variation of rock strength with bedding plane orientation quite well. We show that this variation could depend on many factors, including the stress loading condition (plane strain versus 3D), degree of anisotropy, temperature, shear-induced dilation versus shear-induced compaction, specimen imperfections, and boundary restraints, among others.

42 ENGINEERING↗

Spectral characterization of igneous rocks in the 8- to 12-micron region

This paper investigates the crystal-chemistry basis for the variation in spectral behavior of ingneous rocks, with the purpose of developing relationships useful for applications in the lithologic characterization of terrestrial and extraterrestrial surfaces. A new parameter is proposed for characterizing general rock and mineral type. The parameter, SCFM, defined as the ratio SiO2/(SiO2 + CaO + FeO + MgO), reflects the degree of depolymerization of the silica tetrahedra in both fine-grained and coarse-grained igneous rocks, and is a good descriptor of the composition of these rocks. Using spectra obtained in the laboratory on coarse-particulate mineral and solid-rock samples, the SCFM parameter was used to assess the effects of variations in the rock composition on the location, number, and width of spectral bands. A regression analysis of bands varying in width from 0.2 micron to 1.4 microns versus the SCFM value resulted in correlation coefficients ranging from 0.88 to 0.97.

Walter, Louis S.↗

Space Weathering of Lunar Rocks

All materials exposed at the lunar surface undergo space weathering processes. On the Moon, boulders make up only a small percentage of the exposed surface, and areas where such rocks are exposed, like central peaks, are often among the least space weathered regions identified from remote sensing data. Yet space weathered surfaces (patina) are relatively common on returned rock samples, some of which directly sample the surface of larger boulders. Because, as witness plates to lunar space weathering, rocks and boulders experience longer exposure times compared to lunar soil grains, they allow us to develop a deeper perspective on the relative importance of various weathering processes as a function of time.

Noble, S. K.↗

Lateral Variations in Lunar Weathering Patina on Centimeter to Nanometer Scales

All materials exposed at the lunar surface undergo space weathering processes. On the Moon, boulders make up only a small percentage of the exposed surface, and areas where such rocks are exposed, like central peaks, are often among the least space weathered regions identified from remote sensing data. Yet space weathered surfaces (patina) are relatively common on returned rock samples, some of which directly sample the surface of larger boulders. Because, as witness plates to lunar space weathering, rocks and boulders experience longer exposure times compared to lunar soil grains, they allow us to develop a deeper perspective on the relative importance of various weathering processes as a function of time.

Noble, S. K.↗

Cosmogenic 3 He exposure dating in mafic rocks by “Virtual mineral separation” of pyroxene

We describe a “virtual mineral separation” method for measuring the cosmogenic 3 He concentration in pyroxene in mafic rocks that consist mainly of plagioclase and pyroxene, without physically separating the minerals. This approach is significantly faster and more cost-effective than the conventional method, which requires physical separation and purification of pyroxene grains by time-consuming and labor-intensive crushing, acid cleaning, magnetic separation, HF etching, and handpicking under a microscope. The premise of the method is that helium diffusivity is much higher in plagioclase than in pyroxene, so controlled preheating of a mixed whole-rock sample can degas 3 He from plagioclase while retaining all 3 He in pyroxene. A second heating step releases all 3 He from pyroxene for measurement. To then obtain a 3 He concentration in pyroxene rather than the whole rock, we determine the pyroxene weight fraction in the sample using X-ray computed tomography (CT). A comparison of 3 He concentrations in pyroxene measured using virtual mineral separation with those measured in the same samples by physical mineral separation in previous work shows no evidence of systematic bias between the methods. Virtual mineral separation greatly simplifies the workflow for 3 He exposure-dating of mafic rocks, reduces time, effort, and cost, and permits measurements on very small samples. This enables new emerging applications of exposure dating, such as quantifying stochastic surface processes, ecosystem studies, and potential subglacial bedrock exposure dating.

Geosciences↗

Comparison of single crack propagation in lunar analogue glass and the failure strength of rocks

New data of crack propagation in lunar analogue glass provides important input for the construction of deformation maps (maps which delineate the rates and principal means of material deformation under various environmental conditions) applicable to the lunar crust. Comparison of single crack propagation data obtained on flat plates of glass and failure strength data obtained on fine grained rock samples show that single crack propagation velocities are directly related to the failure strength of rocks. The chemical reaction between water and silicon-oxygen bonds at the crack tip seems to be of first order. This greatly simplifies extrapolation to low partial pressures of H2O

Soga, N.↗

A Model-based Approach to Developing the Concept of Operations for Potential Mars Sample Return

Mars Sample Return (MSR) is a proposed multi-agency effort that would return soil and rock samples from the surface of Mars to Earth. Both the complexity of the potential missions, as well as the involvement of multiple geographically distributed organizations, presents a challenge from an information management perspective. In this paper, a Model-based Systems Engineering (MBSE) approach to developing the Concept of Operations of a potential Mars Sample Return effort using the System Modeling Language(SysML) is presented.

Muirhead, Brian↗