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USGS1987

APPLICATIONS OF CATHODOLUMINESCENCE OF QUARTZ AND FELDSPAR TO SEDIMENTARY PETROLOGY.

Cathodoluminescence (CL), the emission of visible light during electron bombardment, was first used in sandstone petrology in the mid-1960's. CL techniques are especially useful for determining the origin and source of quartz and feldspar, two of the most common constituents in clastic rocks. CL properties of both minerals are dependent on their temperature of crystallization, duration of cooling, and/or history of deformation. Detrital quartz and feldspar are typically derived from igneous and metamorphic sources and luminesce in the visible range whereas authigenic quartz and feldspar form at low temperatures and do not luminesce. Quantification of luminescent and non-luminescent quartz and feldspar with the scanning electron microscope, electron microprobe, or a commercial CL device can allow for the determination of origin, diagenesis, and source of clastic rocks when used in conjunction with field and other petrographic analyses.

Scanning Micros↗

USGS1987

PROTON MICROPROBE ANALYSIS OF TRACE-ELEMENT VARIATIONS IN VITRINITES IN THE SAME AND DIFFERENT COAL BEDS.

The PIXE (proton-induced X-ray emission) microprobe can be used for nondestructive, in-situ analyses of areas as small as those analyzed by the electron microprobe, and has a sensitivity of detection as much as two orders of magnitude better than the electron microprobe. Preliminary studies demonstrated that PIXE provides a capability for quantitative determination of elemental concentrations in individual coal maceral grains with a detection limit of 1-10 ppm for most elements analyzed. Encouraged by the earlier results, we carried out the analyses reported below to examine trace element variations laterally (over a km range) as well as vertically (cm to m) in the I and J coal beds in the Upper Cretaceous Ferron Sandstone Member of the Mancos Shale in central Utah, and to compare the data with the data from two samples of eastern coals of Pennsylvanian age.

Scanning Micros↗

USGS1993

Surface chemical effects on colloid stability and transport through natural porous media

Surface chemical effects on colloidal stability and transport through porous media were investigated using laboratory column techniques. Approximately 100 nm diameter, spherical, iron oxide particles were synthesized as the mobile colloidal phase. The column packing material was retrieved from a sand and gravel aquifer on Cape Cod, MA. Previous studies have indicated enhanced stability and transport of iron oxide particles due to specific adsorption of some inorganic anions on the iron oxide surface. This phenomenon was further evaluated with an anionic surfactant, sodium dodecyl sulfate. Surfactants constitute a significant mass of the contaminant loading at the Cape Cod site and their presence may contribute to colloidal transport as a significant transport mechanism at the site. Other studies at the site have previously demonstrated the occurrence of this transport mechanism for iron phosphate particles. Photon correlation spectroscopy, micro-electrophoretic mobility, and scanning electron microscopy were used to evaluate particle stability, mobility and size. Adsorption of negatively charged organic and inorganic species onto the surface of the iron oxide particles was shown to significantly enhance particle stability and transport through alterations of the electrokinetic properties of the particle surface. Particle breakthrough generally occurred simultaneously with tritiated water, a conservative tracer. The extent of particle breakthrough was primarily dependent upon colloidal stability and surface charge.

Massachusetts↗

USGS2007

Spectroscopic evidence for uranium bearing precipitates in vadose zone sediments at the Hanford 300-area site

Uranium (U) solid-state speciation in vadose zone sediments collected beneath the former North Process Pond (NPP) in the 300 Area of the Hanford site (Washington) was investigated using multi-scale techniques. In 30 day batch experiments, only a small fraction of total U (???7.4%) was released to artificial groundwater solutions equilibrated with 1% pCO2. Synchrotron-based micro-X-ray fluorescence spectroscopy analyses showed that U was distributed among at least two types of species: (i) U discrete grains associated with Cu and (ii) areas with intermediate U concentrations on grains and grain coatings. Metatorbernite (Cu[UO2]2[PO 4]2??8H2O) and uranophane (Ca[UO 2]2[SiO3(OH)]2?? 5H 2O) at some U discrete grains, and muscovite at U intermediate concentration areas, were identified in synchrotron-based micro-X-ray diffraction. Scanning electron microscopy/energy dispersive X-ray analyses revealed 8-10 ??m size metatorbernite particles that were embedded in C-, Al-, and Si-rich coatings on quartz and albite grains. In ??- and bulk-X-ray absorption structure (??-XAS and XAS) spectroscopy analyses, the structure of metatorbernite with additional U-C and U-U coordination environments was consistently observed at U discrete grains with high U concentrations. The consistency of the ??- and bulk-XAS analyses suggests that metatorbernite may comprise a significant fraction of the total U in the sample. The entrapped, micrometer-sized metatorbernite particles in C-, Al-, and Si-rich coatings, along with the more soluble precipitated uranyl carbonates and uranophane, likely control the long-term release of U to water associated with the vadose zone sediments. ?? 2007 American Chemical Society.

Environmental Science & Technology↗

USGS2018

KG²B, a collaborative benchmarking exercise for estimating the permeability of the Grimsel granodiorite - Part 2: modeling, microstructures and complementary data

Measuring and modelling the permeability of tight rocks remains a challenging task. In addition to the traditional sources of errors that affect more permeable formations (e.g. sample selection, non-representative specimens, disturbance introduced during sample acquisition and preparation), tight rocks can be particularly prone to solid–fluid interactions and thus more sensitive to the methods, procedures and techniques used to measure permeability. To address this problem, it is desirable to collect, for a single material, measurements obtained by different methods and pore fluids. For that purpose, a benchmarking exercise involving 24 laboratories was organized for measuring and modelling the permeability of a single low-permeability material, the Grimsel granodiorite. The objectives of the benchmark were: (i) to compare the results for a given method, (ii) to compare the results between different methods, (iii) to analyse the accuracy of each method, (iv) to study the influence of experimental conditions (especially the nature of pore fluid), (v) to discuss the relevance of indirect methods and models and finally (vi) to suggest good practice for low-permeability measurements. To complement the data set of permeability measurements presented in a companion paper, we focus here on (i) quantitative analysis of microstructures and pore size distribution, (ii) permeability modelling and (iii) complementary measurements of permeability anisotropy and poroelastic parameters. Broad ion beam—scanning electron microscopy, micro-computerized tomography, mercury injection capillary pressure (MICP) and nuclear magnetic resonance (NMR) methods were used to characterize the microstructures and provided the input parameters for permeability modelling. Several models were used: (i) basic statistical models, (ii) 3-D pore network and effective medium models, (iii) percolation model using MICP data and (iv) free-fluid model using NMR data. The models were generally successful in predicting the actual range of measured permeability. Statistical models overestimate the permeability because they do not adequately account for the heterogeneity of the crack network. Pore network and effective medium models provide additional constraints on crack parameters such as aspect ratio, aperture, density and connectivity. MICP and advanced microscopy techniques are very useful tools providing important input data for permeability estimation. Permeability measured—orthogonal to foliation is lower that—parallel to foliation. Combining the experimental and modelling results provide a unique and rich data set.

Geophysical Journal International↗

USGS2019

Authigenic mineral texture in submarine 1979 basalt drill core, Surtsey volcano, Iceland

Micrometer-scale maps of authigenic microstructures in submarine basaltic tuff specimens from a 1979 Surtsey volcano, Iceland, drill core acquired 15 years after eruptions terminated provide fresh perspectives for deciphering the initial alteration of oceanic basalt in a low temperature hydrothermal system. A novel investigative approach integrates synchrotron source X-ray microdiffraction (µXRD), X-ray microfluoresence (µXRF), micro-computed tomography (µCT), and scanning transmission electron microscopy (S/TEM) coupled with Raman spectroscopy to create finely resolved spatial frameworks that record a continuum of alteration in glass and olivine. Micro-analytical maps of vesicular and fractured lapilli in specimens from 157.1, 137.9, and 102.6 m depth, and borehole temperatures of 83, 93.9 and 141.3 °C measured in 1980, respectively, record the production of nanocrystalline clay mineral, zeolites, and Al-tobermorite in diverse microenvironments. Nanocrystalline clay mineral (nontronite) and zeolite (amicite) texture in linear microstructures have concentrically-oriented crystallographic preferred orientation. Raman spectra indicating degraded organic carbonaceous matter are associated with nanocrystalline clay mineral in 10–25 nm, sub-circular nanoscale cavities in altered glass at 137.9 m depth and in a concentrically-layered, crystallographically-oriented linear microstructure in altered olivine at 102.6 m. These features have little resemblance to previously described alteration features in basalt. Irregular alteration fronts between fresh and altered glass at 157.1 depth, however, show a resemblance to microchannels in older basalts. The integrated analyses describe the complex organization of previously unrecognized mineral textures in very young basalt and provide a foundational mineralogical reference for longitudinal, time-lapse characterizations of palagonitized basalt in oceanic environments.

Geochemistry, Geophysics, Geosystems↗

USGS2009

The weathering of a sulfide orebody: Speciation and fate of some potential contaminants

Various potentially toxic trace elements such as As, Cu, Pb and Zn have been remobilized by the weathering of a sulfide orebody that was only partially mined at Leona Heights, California. As a result, this body has both natural and anthropogeni- cally modified weathering profiles only 500 m apart. The orebody is located in a heavily urbanized area in suburban Oakland, and directly affects water quality in at least one stream by producing acidic conditions and relatively high concentrations of dissolved elements (e.g., ??500 ??g/L Cu, ??3700 ??g/L Zn). Micrometric-scale mineralogical investigations were performed on the authigenic metal-bearing phases (less than 10 ??m in size) using electron-probe micro-analysis (EPMA), micro-Raman, micro X-ray absorption spectroscopy (??XAS), scanning X-ray diffraction ((??SXRD) and scanning X-ray fluorescence (??-SXRF) mapping techniques. Those measurements were coupled with classical mineralogical laboratory techniques, X-ray diffraction (XRD) and scanning electron microscopy (SEM). Authigenic metal-bearing phases identified are mainly sulfates (jarosite, epsomite, schwertmannite), Fe (oxy-)hydroxides (goethite, hematite and poorly crystalline Fe products) and poorly crystalline Mn (hydr-)oxides. Sulfates and Fe (oxy-)hydroxides are the two main secondary products at both sites, whereas Mn (hydr-) oxides were only observed in the samples from the non-mining site. In these samples, the various trace elements show different affinities for Fe or Mn compounds. Lead is preferentially associated with Mn (hydr-)oxides and As with Fe (oxy-)hydroxides or sulfates. Copper association with Mn and Fe phases is questionable, and the results obtained rather indicate that Cu is present as individual Cu-rich grains (Cu hydroxides). Some ochreous precipitates were found at both sites and correspond to a mixture of schwertmannite, goethite and jarosite containing some potentially toxic trace elements such as Cu, Pb and Zn. According to the trace element distribution and relative abundance of the unweathered sulfides, this orebody still represents a significant reservoir of potential contaminants for the watershed, especially at the non-mining site, as a much greater proportion of sulfides is left to react and because of the lower porosity at this site.

Canadian Mineralogist↗

USGS2015

Evaluating habitat associations of a fish assemblage at multiple spatial scales in a minimally disturbed stream using low‐cost remote sensing

Habitat heterogeneity at multiple scales is a major factor affecting fish assemblage structure. However, assessments that examine these relationships at multiple scales concurrently are lacking. The lack of assessments at these scales is a critical gap in understanding as conservation and restoration efforts typically work at these levels. A combination of low‐cost side‐scan sonar surveys, aerial imagery using an unmanned aerial vehicle, and fish collections were used to evaluate the relationship between physicochemical and landscape variables at various spatial scales (e.g. micro‐mesohabitat, mesohabitat, channel unit, stream reach) and stream–fish assemblage structure and habitat associations in the South Llano River, a spring‐fed second‐order stream on the Edwards Plateau in central Texas during 2012–2013. Low‐cost side‐scan sonar surveys have not typically been used to generate data for riverscape assessments of assemblage structure, thus the secondary objective was to assess the efficacy of this approach. The finest spatial scale (micro‐mesohabitat) and the intermediate scale (channel unit) had the greatest explanatory power for variation in fish assemblage structure. Many of the fish endemic to the Edwards Plateau showed similar associations with physicochemical and landscape variables suggesting that conservation and restoration actions targeting a single endemic species may provide benefits to a large proportion of the endemic species in this system. Low‐cost side‐scan sonar proved to be a cost‐effective means of acquiring information on the habitat availability of the entire river length and allowed the assessment of how a full suite of riverscape‐level variables influenced local fish assemblage structure.

Texas↗

USGS2020

Organic petrography of Leonardian (Wolfcamp A) mudrocks and carbonates, Midland Basin, Texas: The fate of oil-prone sedimentary organic matter in the oil window

To better understand evolution of oil-prone sedimentary organic matter to petroleum and expulsion from source rock, we evaluated organic petrographic features of Leonardian Wolfcamp A repetitive siliceous and calcareous mudrock and fine-grained carbonate lithofacies cycles occurring in the R. Ricker #1 core from Reagan County, Midland Basin, Texas. The objectives of the petrographic investigation were to estimate thermal maturity, identify organic matter types and abundances, and identify the presence or absence of migrated hydrocarbons in organic-lean carbonate layers. An integrated analytical program included geochemical screening [total organic carbon (TOC) content by LECO, programmed pyrolysis by hydrocarbon analyzer with kinetics (HAWK) including analysis of solvent-extracted samples], X-ray diffraction mineralogy, organic petrography, scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS) including correlative light and electron microscopy (CLEM), and micro-Fourier transform infrared spectroscopy (μ-FTIR) analyses of solid bitumen. The data indicate all samples are early to middle oil window thermal maturity with solid bitumen reflectance (BR o ) values of 0.55–0.86% and T max of 440–455 °C. Organic matter is predominantly solid bitumen (as identified by optical microscopy) in all lithofacies with minor contributions from inertinite. Solid bitumen abundance decreases from siliceous mudrock (TOC >3.0 wt%) to calcareous mudrock (TOC 1.0 to 3.0 wt%) to fine-grained carbonate (TOC <1.0 wt%) lithofacies. Interpretations of petrographic data suggest siliceous and calcareous mudrocks are source rock lithofacies and contain solid bitumen (with petroleum generation potential) that is residual (what remains) from conversion of an original Type II sedimentary organic matter. In turn, fine-grained carbonates are interpreted as reservoir lithofacies which contained little or no original oil-prone sedimentary organic matter and at present-day contain only a minor component of migrated solid petroleum sourced from adjacent siliceous and calcareous mudrock lithofacies. This work helps to document petroleum generation and migration processes, improve unconventional reservoir characterization and better define areas of oil window thermal maturity in an area critical to United States hydrocarbon production.

Texas↗

USGS2025

Combining scanning electron microscopy, X-ray diffraction, and X-ray fluorescence to characterize shear zones at the Pogo gold deposit, Alaska

This study employs a multi-method analytical approach to characterize the mineralogical, geochemical, and textural properties of fault rocks from the Pogo gold mine in the Yukon-Tanana Upland, central Alaska. Specifically, we examine cataclasites, to document the structural and geochemical evolution of shear zones and their associations with gold mineralization. To investigate the shear zone, we integrate portable X-ray fluorescence (pXRF), scanning electron microscopy-based automated mineralogy (SEM-AM), X-ray diffraction (XRD), and high-resolution micro-X-ray fluorescence (micro-XRF) mapping. These methods collectively provide insights into bulk and trace element chemistry, mineralogical composition, and deformation-related textures across multiple scales. Handheld pXRF enables rapid geochemical screening, guiding SEM-AM and XRD analyses to ensure consistent mineralogical interpretation. X-ray diffraction identifies and quantifies crystalline phases, while SEM-AM produces high-resolution mineral maps, revealing mineral abundances, grain-scale textures, and gold associations. Micro-XRF mapping further refines our understanding by showing visual trace element distributions at sub-millimetre resolution. By integrating these techniques, we improve our understanding of the nature and geochemistry of Pogo shear zones, their role in gold mineralization, and support metallurgical processing strategies. This approach enhances exploration models and resource characterization for structurally complex gold deposits.

Alaska↗

USGS1973

Bottom features and processes related to drifting ice on the Arctic shelf, Alaska

Early investigations of artic shelf regions led to the hypothesis that certain micro-relief forms are related to the action of grounded ice (for example, Rex, 1955). Since the introduction of side-scan sonar as a tool for ocean-floor surveys, a number of workers have described the occurrence of linear bottom features produced by grounded ice. Such features have been found on modern polar shelves (Skinner, 1971; Pelletier and Shearer, 1972; Kovacs, 1972; Reimnitz and Barnes, 1972; Brooks, 1973), and as relict features (Berkson and Clay, 1973; Belderson and Wilson, 1973; Belderson and others, 1973). Studies of core samples, high resolution seismic profiles, and diving observations indicate that the sediments of the Beaufort Sea Shelf are highly distorted by the action of grounding ice, and that the recurrence rate of gouging is very high. It has also become evident that grounding ice is contributing considerably to the sediment transport processes of modern Arctic shelves. Sediments from similar environments exposed on the continents today should also contain the record of ice gouging and related processes. Thus it has become apparent that drifting ice is an important agent influencing the sedimentary structures and the sediment transport regime of Arctic shelves today and has been in the past. The diagrams presented here, with supporting evidence in the form of side-scan sonar records, and ice and bottom photos, demonstrate the most prevalent processes and types of bottom features observed on the continental shelf off northern Alaska. As the map shows, most of the shelf is affected by these processes today.

Alaska↗

USGS2026

Oil in the Alaska North Slope gas hydrate reservoir: Micro-CT and flow simulation insights into permeability

Gas hydrate-bearing sands on the Alaska North Slope (ANS) host minor volumes of crude oil whose impact on formation permeability has never been quantified relative to a gas hydrate reservoir system. Here, we combine in situ pressure-core microcomputed-tomography (μ-CT), thermogravimetric analysis (TGA), gas-chromatography–mass-spectrometry (GC–MS), scanning-electron microscopy coupled with energy-dispersive spectroscopy (SEM-EDS), and Stokes-flow simulation to (i) quantify oil saturation, (ii) infer its source, and (iii) evaluate its influence on permeability after gas-hydrate dissociation. μ-CT and SEM-EDS imaging identify the host sediment as silty, with some grain-coating clay present. Eight representative 300 3 -voxel subvolumes extracted from a preserved pressure core (Core 15P-3c, from the B1 sand (unit B), HYDRATE 02 Geo Data Well (GDW), 886.96–887.29 m measured depth, MD) exhibit porosities of 0.34–0.37 and an average oil saturation of 0.09 ± 0.03, in comparison to an independent TGA-based estimate of 0.16. GC-MS fingerprints obtained from an adjacent depressurized core (Core 17P-1, 891.37–891.44 m MD), together with oil pore habit revealed by μ-CT, suggest that the oil is partly native but also includes contributions from mineral oil-based drilling fluid contamination. Further analysis of oil–porewater interactions and flushing tests confirms that native oil saturation in the analyzed samples ranges from 0.04 to 0.08 with an average of approximately 0.06, and the oil is highly immobile. Flow simulations demonstrate that the native oil saturation of ≈0.06 reduces permeability by approximately 50% due to both pore blockage and increased flow-path tortuosity. These findings reveal the potential presence of native oil within the ANS gas hydrate reservoir and suggest that future simulation models may need to account for its impact on permeability to improve long-term performance predictions of gas and water production.

Alaska↗

USGS1997

Determining concentrations of 2-bromoallyl alcohol and dibromopropene in ground water using quantitative methods

A method for determining levels of 2-bromoallyl alcohol and 2,3-dibromopropene from ground-water samples using liquid/liquid extraction followed by gas chromatography/mass spectrometry is described. Analytes were extracted from the water using three aliquots of dichloromethane. The aliquots were combined and reduced in volume by rotary evaporation followed by evaporation using a nitrogen stream. The extracts were analyzed by capillary-column gas chromatography/mass spectrometry in the full-scan mode. Estimated method detection limits were 30 nanograms per liter for 2-bromoallyl alcohol and 10 nanograms per liter for 2,3-dibromopropene. Recoveries were determined by spiking three matrices at two concentration levels (0.540 and 5.40 micrograms per liter for 2-bromoallyl alcohol; and 0.534 and 5.34micro-grams per liter for dibromopropene). For seven replicates of each matrix at the high concentration level, the mean percent recoveries ranged from 43.9 to 64.9 percent for 2-bromoallyl alcohol, and from 87.5 to 99.3 percent for dibromopropene. At the low concentration level, the mean percent recoveries ranged from 43.8 to 95.2 percent for 2-bromoallyl alcohol, and from 71.3 to 84.9 percent for dibromopropene.

Open-File Report↗

USGS1978

Ice-gouged microrelief on the floor of the eastern Chukchi Sea, Alaska: a reconnaissance survey

Side-scan sonar and bathymetric records obtained from 1,800 km of trackline from the eastern Chukchi Sea continental shelf, between water depths of 20 and 70 m show the ubiquitous presence of furrow-like linear depressions produced by gouging of the sea bed by ice keels. These sea bed micro-features are regionally widespread but are not uniformly distributed. Furthermore, the microrelief, texture, and lithologic structure of sea bed sediments have been significantly modified by the disruptive processes associated with ice gouge formation. An analysis of some 10,.200 individual gouges shows that the density of ice gouges increases with increasing latitude, increasing slope gradients, and decreasing water depth. Across the northern half of the shelf few trackline segments are free of ice gouges; in the southern portion numerous segments contain no ice gouges. However, ice gouges extend at least as far south as Cape Prince of Wales Shoal. Densities of over 200 gouges per km of trackline are not uncommon in water depths less than 30 m ,but no values higher than 50 km are encountered in water deeper than 50 m. No ice gouges have been observed in water depths exceeding 58 m. Saturation ice gouge densities (greater than 300/Pan) occur along the eastern side 6f Barrow Sea Valley and the northeast flank of Hanna Shoal. Maximum gouge incision depths per km of trackline are greatest in water 36 to 50 m deep . A maximum incision depth of 4.5 m occurs in the 35-40 m water depth interval. Individual ice gouge events wider than 100 m, most produced by multi-keeled ice fragments, are found between 31 and 45 m depths. The dominant azimuth of gouge furrows shows no preferred orientation on the Chukchi Sea shelf; only locally does bathmetric control of the trend of gouges appear. The occurrence of current-produced bedforms within individual ice gouges suggests an interaction between slow-moving grounded or gouging ice keels and swift currents. In other cases, current-produced bedforms, interpreted as being in equilibrium with existing flow regimes, lie adjacent to ice gouges, suggesting contemporary ice gouging to water depths of at least 43 m.

Open-File Report↗

USGS2014

An integrated approach to the Taxonomic identification of prehistoric shell ornaments

Shell beads appear to have been one of the earliest examples of personal adornments. Marine shells identified far from the shore evidence long-distance transport and imply networks of exchange and negotiation. However, worked beads lose taxonomic clues to identification, and this may be compounded by taphonomic alteration. Consequently, the significance of this key early artefact may be underestimated. We report the use of bulk amino acid composition of the stable intra-crystalline proteins preserved in shell biominerals and the application of pattern recognition methods to a large dataset (777 samples) to demonstrate that taxonomic identification can be achieved at genus level. Amino acid analyses are fast (<2 hours per sample) and micro-destructive (sample size <2 mg). Their integration with non-destructive techniques provides a valuable and affordable tool, which can be used by archaeologists and museum curators to gain insight into early exploitation of natural resources by humans. Here we combine amino acid analyses, macro- and microstructural observations (by light microscopy and scanning electron microscopy) and Raman spectroscopy to try to identify the raw material used for beads discovered at the Early Bronze Age site of Great Cornard (UK). Our results show that at least two shell taxa were used and we hypothesise that these were sourced locally.

PLoS ONE↗

USGS2024

Interlamellar adsorption of carbon dioxide by smectites

The adsorption of CO 2 at low temperature (∼ −70°C) on thin films of homoionic smectites was studied by X-ray diffraction and by i.r. absorption. An increase in the d 001 spacings of these clay films upon adsorption of CO 2 was observed. In addition, a dichroic effect was readily discernible by comparing the i.r. spectra at two different orientations of the smectite films; i.e. with the film normal and tilted 35° with respect to the i.r. beam. The CO 2 stretching vibration at 2350 cm −1 was used for the i.r. study. These observations conclusively show that CO 2 intercalates the smectite structure rather than being adsorbed only in pores between clay tactoids—the limiting process proposed by other investigators. Adsorption isotherm data from earlier surface area studies are re-examined here through application of the Dubinin equation. Again, intercalation is demonstrated by convergence of the plotted experimental data for smectites containing large monovalent interlayer cations toward a pore volume that is near the calculated theoretical value for a monolayer of intercalated CO 2 . Scanning electron photomicrographs of Li- and Cs- smectites provide additional evidence that aggregation differences are not responsible for the large observed difference in BET surface areas obtained for these smectites with CO 2 as the adsorbate. At low magnification, visual differences in macro-aggregates are apparent, but at high magnification no significant differences are observed in the micro-structure of individual aggregates where the major amount of gas adsorption really occurs.

Clays and Clay Minerals↗

USGS2022

Growth of complex volcanic ash aggregates in the Tierra Blanca Joven eruption of Ilopango Caldera, El Salvador

Aggregation processes control both the residence time and dispersal of volcanic ash during eruptions yet remain incompletely understood. The products of aggregation vary from simple ash clusters to large, complexly layered accretionary lapilli. Here we detail the micro-stratigraphy of a single population of accretionary lapilli that grew during the ∼431 CE Tierra Blanca Joven eruption from Ilopango Caldera, El Salvador. The accretionary lapilli were sampled 10 km from the caldera source within a sequence of ash-rich pyroclastic density current deposits and intercalated fall material, known as unit D, which is traceable >40 km from Ilopango. Scanning electron microscopy and image analysis reveal common facies that form distinct layers within the accretionary lapilli. Each facies is distinguished by quantitative and qualitative variations in particle size distribution , porosity, and particle fabric. We infer that these textures resulted from aggregation conditions that differed in terms of liquid water availability, particle concentration and grain size distributions. In our proposed model, a characteristic sequence of facies accreted from core to rim in the accretionary lapilli during passage through ash clouds generated by vent-derived plumes and pyroclastic density currents. The accretionary lapilli are mostly composed of smaller aggregates (ash clusters, ash pellets) and grew predominantly by accretion of already-formed aggregates, rather than by grain-by-grain accretion of individual particles. This finding is consistent with observations of rapid aggregate growth in volcanic plumes, suggesting a common evolutionary pathway for accretionary lapilli formation across diverse eruptions.

Ilopango caldera↗

USGS2023

A novel non-destructive workflow for examining germanium and co-substituents in ZnS

A suite of complementary techniques was used to examine germanium (Ge), a byproduct critical element, and co-substituent trace elements in ZnS and mine wastes from four mineral districts where germanium is, or has been, produced within the United States. This contribution establishes a comprehensive workflow for characterizing Ge and other trace elements, which captures the full heterogeneity of samples through extensive pre-characterization. This process proceeded from optical microscopy, to scanning electron microscopy and cathodoluminescence (CL) imaging, to electron microprobe analysis, prior to synchrotron-based investigations. Utilizing non-destructive techniques enabled reanalysis, which proved essential for verifying observations and validating unexpected results. In cases where the Fe content was <0.3 wt% in ZnS, cathodoluminescence imaging proved to be an efficient means to qualitatively identify trace element zonation that could then be further explored by other micro-focused techniques. Micro-focused X-ray diffraction was used to map the distribution of the non-cubic ZnS polymorph, whereas micro-focused X-ray fluorescence (μ-XRF) phase mapping distinguished between Ge 4+ hosted in primary ZnS and a weathering product, hemimorphite [Zn 4 Si 2 O 7 (OH) 2 ·H 2 O]. Microprobe data and μ-XRF maps identified spatial relationships among trace elements in ZnS and implied substitutional mechanisms, which were further explored using Ge and copper (Cu) X-ray absorption near-edge spectroscopy (XANES). Both oxidation states of Ge (4+ and 2+) were identified in ZnS along with, almost exclusively, monovalent Cu. However, the relative abundance of Ge oxidation states varied among mineral districts and, sometimes, within samples. Further, bulk XANES measurements typically agreed with micro-focused XANES (μ-XANES) spectra, but unique micro-environments were detected, highlighting the importance of complementary bulk and micro-focused measurements. Some Ge μ-XANES utilized a high energy resolution fluorescence detector, which improved spectral resolution and spectral signal-to-noise ratio. This detector opens new opportunities for exploring byproduct critical elements in complex matrices. Overall, the non-destructive workflow employed here can be extended to other byproduct critical elements to more fully understand fundamental ore enrichment processes, which have practical implications for critical element exploration, resource quantification, and extraction.

Frontiers in Earth Science↗