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USGS1999

Iron reduction in the sediments of a hydrocarbon-contaminated aquifer

Sediments sampled at a hydrocarbon-contaminated, glacial-outwash, sandy aquifer near Bemidji, Minnesota, were analyzed for sediment-associated Fe with several techniques. Extraction with 0.5 M HCl dissolved poorly crystalline Fe oxides and small amounts of Fe in crystalline Fe oxides, and extracted Fe from phyllosilicates. Use of Ti-citrate-EDTA-bicarbonate results in more complete removal of crystalline Fe oxides. The average HCl-extractable Fe(III) concentration in the sediments closest to the crude-oil contamination (16.2 μmol/g) has been reduced by up to 30% from background values (23.8 μmol/g) as a result of Fe(III) reduction in contaminated anoxic groundwater. Iron(II) concentrations are elevated in sediments within an anoxic plume in the aquifer. Iron(II) values under the oil body (19.2 μmol/g) are as much as 4 times those in the background sediments (4.6 μmol/g), indicating incorporation of reduced Fe in the contaminated sediments. A 70% increase in total extractable Fe at the anoxic/oxic transition zone indicates reoxidation and precipitation of Fe mobilized from sediment in the anoxic plume. Scanning electron microscopy detected authigenic ferroan calcite in the anoxic sediments and confirmed abundant Fe(III) oxyhydroxides at the anoxic/oxic boundary. The redox biogeochemistry of Fe in this system is coupled to contaminant degradation and is important in predicting processes of hydrocarbon degradation.

Applied Geochemistry↗

USGS2003

The Pleistocene evolution of the East Antarctic Ice Sheet in the Prydz bay region: Stable isotopic evidence from ODP Site 1167

Ocean Drilling Program Leg 188, Prydz Bay, East Antarctica is part of a larger initiative to explore the Cenozoic history of the Antarctic Ice Sheet through direct drilling and sampling of the continental margins. In this paper, we present stable isotopic results from Ocean Drilling Program (ODP) Site 1167 located on the Prydz Channel Trough Mouth Fan (TMF), the first Antarctic TMF to be drilled. The foraminifer-based ??18O record is interpreted along with sedimentary and downhole logging evidence to reconstruct the Quaternary glacial history of Prydz Bay and the adjacent Lambert Glacier Amery Ice Shelf System (LGAISS). We report an electron spin resonance age date of 36. 9 ?? 3.3 ka at 0.45 m below sea floor and correlate suspected glacial-interglacial cycles with the global isotopic stratigraphy to improve the chronology for Site 1167. The ??18O record based on planktonic (Neogloboquadrina pachyderma (s.)) and limited benthic results (Globocassidulina crassa), indicates a trend of ice sheet expansion that was interrupted by a period of reduced ice volume and possibly warmer conditions during the early-mid-Pleistocene (0.9-1.38 Ma). An increase in ?? 18O values after ??? 900 ka appears to coincide with the mid-Pleistocene climate transition and the expansion of the northern hemisphere ice sheet. The ??18O record in the upper 50 m of the stratigraphic section indicates as few as three glacial-interglacial cycles, tentatively assigned as marine isotopic stages (MIS) 16-21, are preserved since the Brunhes/Matuyama paleomagnetic reversal (780 ka). This suggests that there is a large unconformity near the top of the section and/or that there may have been few extreme advances of the ice sheet since the mid-Pleistocene climate transition resulting in lowered sedimentation rates on the Prydz Channel TMF. The stable isotopic record from Site 1167 is one of the few available from the area south of the Antarctic Polar Front that has been linked with the global isotopic stratigraphy. Our results suggest the potential for the recovery of useful stable isotopic records in other TMFs. ?? 2003 Elsevier B.V. All rights reserved.

Global and Planetary Change↗

USGS2011

Copper localization, elemental content, and thallus colour in the copper hyperaccumulator lichen Lecanora sierrae from California

An unusual dark blue-green lichen, Lecanora sierrae , was discovered over 30 years ago by Czehura near copper mines in the Lights Creek District, Plumas County, Northern California. Using atomic absorption spectroscopy, Czehura found that dark green lichen samples from Warren Canyon contained 4% Cu in ash and suggested that its colour was due to copper accumulation in the cortex. The present study addressed the hypothesis that the green colour in similar material we sampled from Warren Canyon in 2008, is caused by copper localization in the thallus. Optical microscopy and electron microprobe analysis of specimens of L. sierrae confirmed that copper localization took place in the cortex. Elemental analyses of L. sierrae and three other species from the same localities showed high enrichments of copper and selenium, suggesting that copper selenates or selenites might occur in these lichens and be responsible for the unusual colour.

Lichenologist↗

USGS2016

Assessing open-system behavior of 14C in terrestrial gastropod shells

In order to assess open-system behavior of radiocarbon in fossil gastropod shells, we measured the 14 C activity on 10 aliquots of shell material recovered from Illinoian (~190–130 ka) and pre-Illinoian (~800 ka) loess and lacustrine deposits in the Midwestern USA. Eight of the 10 aliquots yielded measurable 14 C activities that ranged from 0.25 to 0.53 percent modern carbon (pMC), corresponding to apparent 14 C ages between 48.2 and 42.1 ka. This small level of open-system behavior is common in many materials that are used for 14 C dating (e.g. charcoal), and typically sets the upper practical limit of the technique. Two aliquots of gastropod shells from the Illinoian-aged Petersburg Silt (Petersburg Section) in central Illinois, USA, however, yielded elevated 14 C activities of 1.26 and 1.71 pMC, which correspond to apparent 14 C ages of 35.1 and 32.7 ka. Together, these results suggest that while many fossil gastropods shells may not suffer from major (>1%) open-system problems, this is not always the case. We then examined the mineralogy, trace element chemistry, and physical characteristics of a suite of fossil and modern gastropod shells to identify the source of contamination in the Petersburg shells and assess the effectiveness of these screening techniques at identifying samples suitable for 14 C dating. Mineralogical (XRD) and trace element analyses were inconclusive, which suggests that these techniques are not suitable for assessing open-system behavior in terrestrial gastropod shells. Analysis with scanning electron microscopy (SEM), however, identified secondary mineralization (calcium carbonate) primarily within the inner whorls of the Petersburg shells. This indicates that SEM examination, or possibly standard microscope examination, of the interior of gastropod shells should be used when selecting fossil gastropod shells for 14 C dating.

Radiocarbon↗

USGS2013

Hanawaltite, Hg1+6Hg2+[Cl,(OH)]2O3 - A new mineral from the Clear Creek claim, San Benito County, California: Description and crystal structure

Hanawaltite, ideally Hg 1+ 6 Hg 2+ O 3 Cl 2 , is orthorhombic, Pbma (57), with unit-cell parameters refined from powder data: a =11.790(3), b =13.881(4), c =6.450(2) Å, V =1055.7(6) Å 3 , a : b : c =0.8494:1:0.4647, Z =4. The strongest six lines of the X-ray powder-diffraction pattern [ d in Å ( I )( hkl )] are: 5.25 (80)(111), 3.164 (60)(231), 3.053 (100)(041), 2.954 (70)(141), 2.681 (50)(401), and 2.411 (50)(232,341). The mineral is an extremely rare constituent in a small prospect pit near the long-abandoned Clear Creek mercury mine, New Idria district, San Benito County, California. It was found on a single-fracture surface where it is intimately associated with calomel, native mercury, cinnabar, montroydite, and quartz. Individual crystals are subhedral to anhedral, platy to somewhat bladed, and average about 50 μm in longest dimension. The largest known crystal is approximately 0.3×0.3 mm in size and is striated parallel [001]. Hanawaltite is opaque to translucent (on very thin edges), black to very dark brown–black in color, with a black to dark red–brown streak. Other physical properties include: metallic luster; cleavage {001} good; uneven fracture; brittle; nonfluorescent; H <5; calculated density (for the empirical formula) 9.51 g/cm 3 . In polished section, hanawaltite is moderately to strongly bireflectant and is pleochroic white ( R I ) to blue–white ( R 2 ). In reflected plane-polarized light, it is white with orange–red internal reflections in very thin grains and at grain margins. The anisotropy is strong with bright metallic blue rotation tints. Measured reflectance values, in air and in oil, are tabulated. Electron-microprobe analysis yielded Hg 2 O 82.46, HgO 14.27, Cl 3.33, H 2 O [0.34], sum [100.40], less O=Cl 0.75, total [99.65] wt. %, corresponding to Hg 1+ 6.00 Hg 2+ 1.00 [Cl 1.43 (OH) 0.57 ] Σ2.00 O 3.00 , based on O+Cl=5. After the crystal structure was determined, the original microprobe value for Hg 2 O, 96.2, was partitioned in a ratio of 6Hg 2 O:HgO and (OH) was calculated, such that Cl+(OH)=2. The hanawaltite structure consists of undulatory [Hg–Hg] 2+ ribbons which roughly parallel (100). The diatomic [Hg–Hg] 2+ groups have anion tails which, in turn, serve as cross linkages between dimer ribbons through [Hg 2+ O 2 Cl 2 ] planar rhombs. The structure is compared to that of other mercury oxychlorides and each is found to have its own unique structural features. This structural diversity is attributed to the inherent ability of mercury to adopt either metallic or ionic types of bonds. The mineral name honors the late Dr. J. D. (Don) Hanawalt (1903–1987), who was a pioneer in the field of X-ray powder diffraction.

California↗

USGS2021

Approach for quantifying rare Earth elements at low keV

The challenges of analyzing bastnaesite (REECO3F) and hydroxylbastnaesite (REECO3OH) include beam sensitivity, quantification of light elements in a heavy element matrix, the presence of elements that cannot be analyzed with EPMA (H), and the use of x-ray lines whose physical constants are not well known. To overcome some of these challenges, Ca, La, Ce, Pr, Nd, and Sm were analyzed at 15 keV accelerating voltage and the light elements (C, O, F) were analyzed at 7 keV accelerating voltage. This approach is ideal for samples that are homogeneous within the volume analyzed. However, for the bastnaesite of interest, this solution is unsatisfactory as backscattered electron imaging reveals chemical variations at scales of less than 1 m (fig. 1). Monte Carlo simulations and wavescans of the REE M family of x-rays were evaluated to determine the best analytical approach. Monte Carlo simulations using Casino v2.42 were ran on a substrate of CeCO3F with a density of 5.00 g/cm3 at 15 keV and 7 kCV accelerating voltage. Depth distribution curves, φ(ρz), reveal x-ray generation at 15 keV for the Ce L shell x-rays approaches 1.0 m whereas the depth of Ce M shell x-ray generation at 7 keV is less than 0.4 m. Similarly, the K shell x-ray generation depth for C, O, and F at 7 keV is also less than 0.4 m. These simulations demonstrate an accelerating voltage of 7 keV or less and use of the REE M x-rays is necessary to acquire chemical information from the same volume of material for the light and heavy elements. Bastnaesite contains all REE and therefore one must consider the energy of the highest x-ray line of interest, namely the Lu M at 1.83 kV, to achieve an overvoltage (Eo/Ec) of over 2. Bastnaesite is also an insulator and requires a conductive coating, therefore 7 keV was used to avoid contributions of the coating material to the analysis given the above constraints. The USNM REE phosphate standards, Edinburgh REE glasses, CeO2, LaB6, and the metals of Sm, Dy, Gd, Er, and Yb were selected to evaluate the peak overlaps of the M family x-ray lines. The materials were coated with ~ 5nm iridium with a Leica ACE600 prior to analysis. Full spectrometer wavescans were collected at 7 keV accelerating voltage, 50 nA beam current, and 20 um beam diameter on a JEOL 8530F Plus using TAP and TAPL crystals. The step size was 0.109 mm along the length of the spectrometer with a dwell of 3 seconds at each step. M and M lines are broad and not individually resolved for the light REE but become more separated and sharper with increasing atomic number. M and M lines for each REE are also present across the spectrometer range further complicating peak interference corrections. The peak positions and overall shape for the Ce M and M lines vary with the coordination of the element. Significant shifts in position and shape were not observed when comparing the Ce M peaks of CeO2 and CePO4. Similar results were seen when comparing the available REE metal to the phosphate (Sm, Dy, Gd, Er, Yb). These wavescans suggest the use of the M or M lines if matrix matched standards are not available.

Microscopy and Microanalysis↗

USGS2010

Hubble Space Telescope observations of Europa in and out of eclipse

Europa is a prime target for astrobiology and has been prioritized as the next target for a National Aeronautics and Space Administration flagship mission. It is important, therefore, that we advance our understanding of Europa, its ocean and physical environment as much as possible. Here, we describe observations of Europa obtained during its orbital eclipse by Jupiter using the Hubble Space Telescope. We obtained Advanced Camera for Surveys Solar Blind Channel far ultraviolet low-resolution spectra that show oxygen line emission both in and out of eclipse. We also used the Wide-Field and Planetary Camera-2 and searched for broad-band optical emission from fluorescence of the surface material, arising from the very high level of incident energetic particle radiation on ices and potentially organic substances. The high-energy particle radiation at the surface of Europa is extremely intense and is responsible for the production of a tenuous oxygen atmosphere and associated FUV line emission. Approximately 50% of the oxygen emission lasts at least a few hours into the eclipse. We discuss the detection limits of the optical emission, which allow us to estimate the fraction of incident energy reradiated at optical wavelengths, through electron-excited emission, Cherenkov radiation in the ice and fluorescent processes. ?? 2010 Cambridge University Press.

Conference Paper↗

USGS2002

Sources and magnitude of bias associated with determination of polychlorinated biphenyls in environmental samples

Recently compiled data on the composition of commercial Aroclor mixtures and ECD (electron capture detector) response factors for all 209 PCB congeners are used to develop estimates of the bias associated with determination of polychlorinated blphenyis. During quantitation of multlcomponent peaks by congener-specific procedures error is introduced because of variable ECD response to isomeric PCBs. Under worst case conditions, the magnitude of this bias can range from less than 2% to as much as 600%. Multicomponent peaks containing the more highly and the lower chlorinated congeners experience the most bias. For this reason, quantitation of Σ PCB in Aroclor mixtures dominated by these species (e.g. 1016) are potentially subject to the greatest error. Comparison of response factor data for ECDs from two laboratories shows that the sign and magnitude of calibration bias for a given multicomponent peak is variable and depends, in part, on the response characteristics of individual detectors. By using the most abundant congener (of each multicomponent peak) for purposes of calibration, one can reduce the maximum bias to less than 55%. Moreover, due to cancellation of errors, the bias resulting from summation of all peak concentrations (i.e. Σ PCB) becomes vanishingly small (<1.2%). In contrast, bias associated with determination of Σ PCB as Aroclor equivalents by the traditional Aroclor method is potentially large (>200%) and highly variable in sign and magnitude. In this case, bias originates not only from the incomplete chromatographic resolution of PCB congeners but also the overlapping patterns of the Aroclor mixtures. Together these results illustrate the advantages of the congener-specific method of PCB quantitation over the traditional Aroclor Method and the extreme difficulty of estimating bias incurred by the latter procedure on a post hoc basis.

Analytical Chemistry↗

USGS2002

Determination of nanogram per liter concentrations of volatile organic compounds in water by capillary gas chromatography and selected ion monitoring mass spectrometry and its use to define groundwater flow directions in Edwards Aquifer, Texas

A method has been developed to measure nanogram per liter amounts of selected volatile organic compounds (VOCs) including dichlorodifluoromethane, trichlorofluoromethane, cis-1,2-dichloroethene, trichloroethene, tetrachloroethene, and the isomers of dichlorobenzene in water. The method uses purge-and-trap techniques on a 100 mL sample, gas chromatography with a megabore capillary column, and electron impact, selected ion monitoring mass spectrometry. Minimum detection levels for these compounds ranged from 1 to 4 ng/L in water. Recoveries from organic-free distilled water and natural groundwater ranged from 70.5% for dichlorodifluoromethane to 107.8% for 1,4-dichlorobenzene. Precision was generally best for cis-1,2-dichloroethene, tetrachloroethene, and the dichlorobenzene isomers and worst for dichlorodifluoromethane and trichlorofluoromethane. Blank data indicated persistent, trace-level introduction of dichlorodifluoromethane, 1,4-dichlorobenzene, and tetrachloroemene to samples during storage and shipment at concentrations less than the method reporting limits. The largest concentrations of the selected VOCs in 27 water samples from the Edwards aquifer near San Antonio, TX, were from confined-zone wells near an abandoned landfill. The results defined a zone of water with no detectable VOCs in nearly all of the aquifer west of San Antonio and from part of the confined zone beneath San Antonio.

Analytical Chemistry↗

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↗

USGS2022

Brief oil exposure reduces fitness in wild Gulf of Mexico mahi-mahi (Coryphaena hippurus)

The Deepwater Horizon (DWH) disaster released 3.19 million barrels of crude oil into the Gulf of Mexico (GOM) in 2010, overlapping the habitat of pelagic fish populations. Using mahi-mahi ( Coryphaena hippurus )─a highly migratory marine teleost present in the GOM during the spill─as a model species, laboratory experiments demonstrate injuries to physiology and behavior following oil exposure. However, more than a decade postspill, impacts on wild populations remain unknown. To address this gap, we exposed wild mahi-mahi to crude oil or control conditions onboard a research vessel, collected fin clip samples, and tagged them with electronic tags prior to release into the GOM. We demonstrate profound effects on survival and reproduction in the wild. In addition to significant changes in gene expression profiles and predation mortality, we documented altered acceleration and habitat use in the first 8 days oil-exposed individuals were at liberty as well as a cessation of apparent spawning activity for at least 37 days. These data reveal that even a brief and low-dose exposure to crude oil impairs fitness in wild mahi-mahi. These findings offer new perspectives on the lasting impacts of the DWH blowout and provide insight about the impacts of future deep-sea oil spills.

Environmental Science and Technology↗

USGS2024

Predicting redox conditions in groundwater at a national scale using random forest classification

Redox conditions in groundwater may markedly affect the fate and transport of nutrients, volatile organic compounds, and trace metals, with significant implications for human health. While many local assessments of redox conditions have been made, the spatial variability of redox reaction rates makes the determination of redox conditions at regional or national scales problematic. In this study, redox conditions in groundwater were predicted for the contiguous United States using random forest classification by relating measured water quality data from over 30,000 wells to natural and anthropogenic factors. The model correctly predicted the oxic/suboxic classification for 78 and 79% of the samples in the out-of-bag and hold-out data sets, respectively. Variables describing geology, hydrology, soil properties, and hydrologic position were among the most important factors affecting the likelihood of oxic conditions in groundwater. Important model variables tended to relate to aquifer recharge, groundwater travel time, or prevalence of electron donors, which are key drivers of redox conditions in groundwater. Partial dependence plots suggested that the likelihood of oxic conditions in groundwater decreased sharply as streams were approached and gradually as the depth below the water table increased. The probability of oxic groundwater increased as base flow index values increased, likely due to the prevalence of well-drained soils and geologic materials in high base flow index areas. The likelihood of oxic conditions increased as topographic wetness index (TWI) values decreased. High topographic wetness index values occur in areas with a propensity for standing water and overland flow, conditions that limit the delivery of dissolved oxygen to groundwater by recharge; higher TWI values also tend to occur in discharge areas, which may contain groundwater with long travel times. A second model was developed to predict the probability of elevated manganese (Mn) concentrations in groundwater (i.e., ≥50 μg/L). The Mn model relied on many of the same variables as the oxic/suboxic model and may be used to identify areas where Mn-reducing conditions occur and where there is an increased risk to domestic water supplies due to high Mn concentrations. Model predictions of redox conditions in groundwater produced in this study may help identify regions of the country with elevated groundwater vulnerability and stream vulnerability to groundwater-derived contaminants.

contiguous United States↗

USGS2015

Predicting redox conditions in groundwater at a regional scale

Defining the oxic-suboxic interface is often critical for determining pathways for nitrate transport in groundwater and to streams at the local scale. Defining this interface on a regional scale is complicated by the spatial variability of reaction rates. The probability of oxic groundwater in the Chesapeake Bay watershed was predicted by relating dissolved O 2 concentrations in groundwater samples to indicators of residence time and/or electron donor availability using logistic regression. Variables that describe surficial geology, position in the flow system, and soil drainage were important predictors of oxic water. The probability of encountering oxic groundwater at a 30 m depth and the depth to the bottom of the oxic layer were predicted for the Chesapeake Bay watershed. The influence of depth to the bottom of the oxic layer on stream nitrate concentrations and time lags (i.e., time period between land application of nitrogen and its effect on streams) are illustrated using model simulations for hypothetical basins. Regional maps of the probability of oxic groundwater should prove useful as indicators of groundwater susceptibility and stream susceptibility to contaminant sources derived from groundwater.

Maryland, New York, Pennsylvania, Virginia↗

USGS2015

Role of anaerobic ammonium oxidation (anammox) in nitrogen removal from a freshwater aquifer

Anaerobic ammonium oxidation (anammox) couples the oxidation of ammonium with the reduction of nitrite, producing N 2 . The presence and activity of anammox bacteria in groundwater were investigated at multiple locations in an aquifer variably affected by a large, wastewater-derived contaminant plume. Anammox bacteria were detected at all locations tested using 16S rRNA gene sequencing and quantification of hydrazine oxidoreductase ( hzo ) gene transcripts. Anammox and denitrification activities were quantified by in situ 15 NO 2 – tracer tests along anoxic flow paths in areas of varying ammonium, nitrate, and organic carbon abundances. Rates of denitrification and anammox were determined by quantifying changes in 28 N 2 , 29 N 2 , 30 N 2 , 15 NO 3 – , 15 NO 2 – , and 15 NH 4 + with groundwater travel time. Anammox was present and active in all areas tested, including where ammonium and dissolved organic carbon concentrations were low, but decreased in proportion to denitrification when acetate was added to increase available electron supply. Anammox contributed 39–90% of potential N 2 production in this aquifer, with rates on the order of 10 nmol N 2 –N L –1 day –1 . Although rates of both anammox and denitrification during the tracer tests were low, they were sufficient to reduce inorganic nitrogen concentrations substantially during the overall groundwater residence times in the aquifer. These results demonstrate that anammox activity in groundwater can rival that of denitrification and may need to be considered when assessing nitrogen mass transport and permanent loss of fixed nitrogen in aquifers.

Environmental Science & Technology↗

USGS2026

Widespread occurrence of Magnéli phases in wildland-urban interface fire ashes

The increasing activity of wildland–urban interface (WUI) fires has raised concerns regarding the potential environmental and human health impacts of residual ash remaining after burning. In this study, we investigated the concentration and speciation of titanium in WUI fire ash. Total titanium concentrations in WUI fire ash ranged from 0.53 to 80 g kg –1 . Synchrotron-based macro- and microscale X-ray absorption near-edge structure (XANES and μXANES, respectively) spectroscopy were used to quantify the relative abundance of major Ti phases in the fire ash, and the results were corroborated by high resolution-transmission electron microscopy (HR-TEM) measurements. Rutile (α-TiO 2 ), anatase (β-TiO 2 ), ilmenite (FeTiO 3 ), and titanium(III) oxide (Ti 2 O 3 ) were detected in all 20 ashes investigated by XANES and accounted for 0.26–0.83, 0.19–0.83, 0.33, and 0.17–0.72 of the spectral weight, respectively. Deeper analysis by μXANES of one sample demonstrated that Ti-bearing particles occurred as a mixture of rutile (α-TiO 2 ), anatase (β-TiO 2 ), ilmenite (FeTiO 3 ), and titanium(III) oxide Ti 2 O 3, with the absence of a pure Ti 2 O 3 phase. The presence of Ti 2 O 3 in the WUI fire ash is ascribed to the reduction of rutile and anatase to Magnéli titania (Ti n O 2 n– 1 , n = 4–9), which is estimated to be the dominant phase of titanium in the 20 WUI fire ashes investigated by XANES. The occurrence of Magnéli titania was corroborated by HR-TEM. Our findings demonstrate the impact of WUI fires on titanium speciation; fires convert titanium dioxides (e.g., rutile and anatase) to reduced titanium phases (e.g., Magnéli titania). Based on HR-TEM analyses, most of the titanium-bearing particles were less than 500 nm in size. Magnéli particles have been shown to be more toxic than rutile and anatase and have been linked to reduced lung function. Therefore, this study provides critical insights into the pollution characteristics and potential health risks of WUI fire ashes and associated particles, which are currently poorly understood.

California↗

USGS2018

Effect of calcium on the bioavailability of dissolved uranium(VI) in plant roots under circumneutral pH

We integrated field measurements, hydroponic experiments, microscopy, and spectroscopy to investigate the effect of Ca(II) on dissolved U(VI) uptake by plants in 1 mM HCO 3 – solutions at circumneutral pH. The accumulation of U in plants (3.1–21.3 mg kg –1 ) from the stream bank of the Rio Paguate, Jackpile Mine, New Mexico served as a motivation for this study. Brassica juncea was the model plant used for the laboratory experiments conducted over a range of U (30–700 μg L –1 ) and Ca (0–240 mg L –1 ) concentrations. The initial U uptake followed pseudo-second-order kinetics. The initial U uptake rate ( V 0 ) ranged from 4.4 to 62 μg g –1 h –1 in experiments with no added Ca and from 0.73 to 2.07 μg g –1 h –1 in experiments with 12 mg L –1 Ca. No measurable U uptake over time was detected for experiments with 240 mg L –1 Ca. Ternary Ca–U–CO 3 complexes may affect the decrease in U bioavailability observed in this study. Elemental X-ray mapping using scanning transmission electron microscopy–energy-dispersive spectrometry detected U–P-bearing precipitates within root cell walls in water free of Ca. These results suggest that root interactions with Ca and carbonate in solution affect the bioavailability of U in plants. This study contributes relevant information to applications related to U transport and remediation of contaminated sites.

Environmental Science & Technology↗

USGS2007

Characteristics of fly ashes from full-scale coal-fired power plants and their relationship to mercury adsorption

Nine fly ash samples were collected from the particulate collection devices (baghouse or electrostatic precipitator) of four full-scale pulverized coal (PC) utility boilers burning eastern bituminous coals (EB-PC ashes) and three cyclone utility boilers burning either Powder River Basin (PRB) coals or PRB blends,(PRB-CYC ashes). As-received fly ash samples were mechanically sieved to obtain six size fractions. Unburned carbon (UBC) content, mercury content, and Brunauer-Emmett-Teller (BET)-N2 surface areas of as-received fly ashes and their size fractions were measured. In addition, UBC particles were examined by scanning electron microscopy, high-resolution transmission microscopy, and thermogravimetry to obtain information on their surface morphology, structure, and oxidation reactivity. It was found that the UBC particles contained amorphous carbon, ribbon-shaped graphitic carbon, and highly ordered graphite structures. The mercury contents of the UBCs (Hg/UBC, in ppm) in raw ash samples were comparable to those of the UBC-enriched samples, indicating that mercury was mainly adsorbed on the UBC in fly ash. The UBC content decreased with a decreasing particle size range for all nine ashes. There was no correlation between the mercury and UBC contents of different size fractions of as-received ashes. The mercury content of the UBCs in each size fraction, however, generally increased with a decreasing particle size for the nine ashes. The mercury contents and surface areas of the UBCs in the PRB-CYC ashes were about 8 and 3 times higher than UBCs in the EB-PC ashes, respectively. It appeared that both the particle size and surface area of UBC could contribute to mercury capture. The particle size of the UBC in PRB-CYC ash and thus the external mass transfer was found to be the major factor impacting the mercury adsorption. Both the particle size and surface reactivity of the UBC in EB-PC ash, which generally had a lower carbon oxidation reactivity than the PRB-PC ashes, appeared to be important for the mercury adsorption. ?? 2007 American Chemical Society.

Energy and Fuels↗

USGS2013

A USANS/SANS study of the accessibility of pores in the Barnett Shale to methane and water

Shale is an increasingly important source of natural gas in the United States. The gas is held in fine pores that need to be accessed by horizontal drilling and hydrofracturing techniques. Understanding the nature of the pores may provide clues to making gas extraction more efficient. We have investigated two Mississippian Barnett Shale samples, combining small-angle neutron scattering (SANS) and ultrasmall-angle neutron scattering (USANS) to determine the pore size distribution of the shale over the size range 10 nm to 10 μm. By adding deuterated methane (CD 4 ) and, separately, deuterated water (D 2 O) to the shale, we have identified the fraction of pores that are accessible to these compounds over this size range. The total pore size distribution is essentially identical for the two samples. At pore sizes >250 nm, >85% of the pores in both samples are accessible to both CD 4 and D 2 O. However, differences in accessibility to CD 4 are observed in the smaller pore sizes (~25 nm). In one sample, CD 4 penetrated the smallest pores as effectively as it did the larger ones. In the other sample, less than 70% of the smallest pores (<25 nm) were accessible to CD 4 , but they were still largely penetrable by water, suggesting that small-scale heterogeneities in methane accessibility occur in the shale samples even though the total porosity does not differ. An additional study investigating the dependence of scattered intensity with pressure of CD 4 allows for an accurate estimation of the pressure at which the scattered intensity is at a minimum. This study provides information about the composition of the material immediately surrounding the pores. Most of the accessible (open) pores in the 25 nm size range can be associated with either mineral matter or high reflectance organic material. However, a complementary scanning electron microscopy investigation shows that most of the pores in these shale samples are contained in the organic components. The neutron scattering results indicate that the pores are not equally proportioned in the different constituents within the shale. There is some indication from the SANS results that the composition of the pore-containing material varies with pore size; the pore size distribution associated with mineral matter is different from that associated with organic phases.

Texas↗