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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Chloroform Fumigation Extraction for Microbial Biomass and Dissolved Organic Carbon from SPRUCE, Marcell Experimental Forest, Minnesota, 2021, 2022, and 2024

This data set provides the results for chloroform fumigation extraction (CFE) of peat samples collected from ambient and experimental plots in the Spruce and Peatland Responses Under Environmental Change (SPRUCE) Experiment site in June and August of 2021, June of 2022, and June, August, and October of 2024. The SPRUCE Experiment site is in the Marcell Experimental Forest in northern Minnesota, USA. The data set includes values for microbial biomass carbon (MBC), microbial biomass nitrogen (MBN), dissolved organic carbon (DOC), dissolved nitrogen (DN), moisture content (MC, available for 2021 and 2022 only) and gravimetric water content (GWC) at 11 depth increments of two-meter peat cores taken from 12 sampling sites at SPRUCE (10 temperature treatment enclosures, 2 ambient temperature treatment enclosures). The sample analysis followed standard methods. The samples were analyzed using a Shimadzu Total Organic Carbon/Nitrogen (TOC/N) analyzer (TOC-V and TOC-L; 2021-2022) or an Elementar vario TOC Cube (2024), liquid catalytic oxidation combustion analyzers for total carbon and nitrogen analysis. This dataset contains two data files in comma separate (.csv) format. Additional metadata are provided: two data dictionaries and a file-level metadata file in comma separate (.csv) format and a user guide in PDF (*.pdf) format.

dissolved nitrogen↗
DOE OSTI2023

Geocatalytically generated methane from low-maturity coal and shale source rocks at low temperatures (80–120 °C) over 52 months

Geocatalytic methanogenesis has been proposed to contribute to methane generation from low-maturity coal and shale source rocks. This study contributes further evidence for geocatalytic methanogenesis from low-maturity source rocks based on long-term experiments lasting up to 52 months. Samples from the Upper Devonian New Albany Shale (R o 0.54 %) and Springfield Coal No. 2 (Pennsylvanian; R o 0.54 %) were heated in glass tubes at 80, 100, and 120 °C for 52 months. Sample aliquots from the Upper Cretaceous Second White Specks Formation (R o 0.42 %) were heated in gold tubes at 80 and 100 °C for 42 months at elevated hydrostatic pressures of 100 to 300 MPa. The product gases — methane (CH 4 ) and carbon dioxide (CO 2 ) — were collected and quantified, and gas yields were corrected for leakage from imperfectly closed pores in samples during heating. The results show that longer heating produced more CH 4 . The average CH 4 yields from New Albany Shale and Springfield Coal No. 2 are 0.47 and 3.0 μmol CH 4 per gram of total organic carbon (TOC) over 52 months of heating. Elevated hydrostatic pressure caused lower CH 4 yields from the Second White Specks Formation (3.82 to 1.20 μmol g –1 TOC), suggesting that pressure can retard methanogenesis. Maceral type critically controls the methanogenesis potential of low-maturity coal and shale source rocks. Finally, results of this study provide important insights to the origin of natural gas in low-maturity sedimentary basins.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2023

Combined chlorine dioxide–membrane distillation for the treatment of produced water

Membrane distillation (MD) is a promising technique for desalinating hypersaline brine, such as produced water (PW). To date, fouling and scaling have remained as major challenges for MD implementation. In this study, chlorine dioxide combined with induced air floatation (ClO 2 -IAF) was systematically investigated as a pretreatment prior to MD. First, the ClO 2 generation based on sodium chlorite and hydrochloric acid was optimized to maximize the on-demand ClO 2 production. The maximum production yield of 18.4% was obtained with 4wt.% NaClO 2 and 20wt.% HCl solutions, with a molar ratio of 1:1.25. Then, two real PW samples were pretreated, and removal efficiencies for total suspended solids (TSS), turbidity, iron, and total organic carbon (TOC) were comprehensively studied by varying the ClO 2 dosage between 6 and 91 mg/L. The ClO 2 -IAF pretreatment displayed TSS and turbidity removals above 90% and TOC removal close to 55%. Further, the PW constituents such as benzene, toluene, ethylbenzene, xylene (BTEX), and total petroleum hydrocarbons (TPH) were analyzed and quantified throughout the cascade of the treatments. The volatiles like BTEX were mainly removed by air floatation, while saturated hydrocarbons such as TPH were retained by the hydrophobic membrane. The MD long-term stability without any in-place cleaning was evaluated, and the membrane withstood for twenty two days without wetting, suggesting that optimizing oxidation pretreatment is critical for mitigating the fouling in MD. Results suggest that organic fouling in PW could be effectively reduced by the pretreatment, but further treatment is required to mitigate the scaling, which resulted in MD wetting.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Aperture size distribution, length, and preferential location of bed-parallel veins in shale

Bed-parallel, calcite-filled veins (BPVs) are common in shale formations, and although they have been widely described in other studies, little is known about their population aperture size distribution. To address this knowledge gap, we analyzed BPV sizes in outcrops and cores from the Vaca Muerta Formation, Neuquén Basin, Argentina; in two cores from the Marcellus Formation, Appalachian Basin, northeast Pennsylvania; and in one core from the Wolfcamp Shale, Delaware Basin, West Texas. Nine out of ten aperture size populations follow a negative exponential distribution, with one following a weak power law. Bed-parallel vein size distribution and intensity vary among formations and within the same shale. We define three groups of distributions: (1) Vaca Muerta outcrops, with the highest BPV intensity and the largest BPVs (cumulative frequency of 4.9 BPVs per meter [BPVs/m] for apertures 0.265 mm to 8.7 cm); (2) Vaca Muerta cores with a similar BPV intensity overall but with no apertures wider than 1.2 cm; and (3) Vaca Muerta, Wolfcamp, and Marcellus cores with the fewest BPVs (cumulative frequency up to 0.63 BPVs/m) and very few wider than 1 cm. Aperture and length in two outcrop data sets are weakly positively correlated and follow power laws with exponents of 0.44 and 0.49. Mechanical interfaces at boundaries between different lithologies exert a strong control on BPV location, with 65–75% of observed interfaces having BPVs along them. Only 25–30% of the BPVs occur at observed material interfaces, however, and unless subtle, unobserved mechanical layering is present, other factors must also control location. BPV intensity and organic richness (TOC) from Vaca Muerta well logs are correlated in some instances but not in others, indicating TOC is not always a good proxy for BPV location or intensity. Furthermore, these findings provide useful information for modeling of hydraulic fracture treatments where BPVs may influence development of the stimulated fracture network, for example by limiting height growth.

58 GEOSCIENCES↗
DOE OSTI2021

Methane generation from low-maturity coals and shale source rocks at low temperatures (80–120 °C) over 14–38 months

This study contributes long-term (14 to 38 months) experimental evidence for geocatalytically mediated methanogenesis in immature to early mature shale and coal source rocks at temperatures from 80 to 120 °C. Borosilicate glass tubes with pre-outgassed coal and shale source rock chips and water were sealed under vacuum, sterilized, heated isothermally, and finally opened in connection with a vacuum line where headspace gases methane (CH 4 ) and carbon dioxide (CO 2 ) were collected. The possibility of admitting pre-existing CH 4 from closed pores into product gases during heating experiments was evaluated by comparative ball milling of original and heated rock chips, followed by quantitation of released gases with a novel closed-circuit laser-based SARAD RTM2200 gas detector system with sub-µmol sensitivity. The yields of produced CH 4 from individual source rocks were corrected by subtracting the amounts of pre-existing CH 4 from formerly closed pores in original source rocks that had leaked during long-term heating. Different shales and coals express contrasting propensities to geocatalytically generate CH 4 and CO 2 , with CH 4 yields ranging from 0.1 to 5.5 µmol g-1 total organic carbon (TOC). CH 4 yields from two petrographically different samples of Springfield Coal with comparable thermal maturity suggest that liptinite expresses a far higher propensity for methanogenesis, but liberates less CO 2 than vitrinite. Shale from the Second White Specks Formation generated approximately 10 times more CH 4 than New Albany Shale per g of TOC, further suggesting complex controls on CH 4 generation during catalytic methanogenesis. Higher temperature can enhance the activities of catalytic methanogenesis. Here, the extrapolation of laboratory-based reaction rates to natural conditions in organic-rich buried sediments suggests that geocatalytic methanogenesis can be fast enough in some source rocks to generate economically sizeable gas plays from immature to early mature source rocks over geologic time.

03 NATURAL GAS↗
DOE OSTI2026

Treatment of Lagoon Dairy Manure Wastewater via Iron Electrocoagulation, Microfiltration, and Adsorption

Dairy manure wastewater generated by flushing barn cow waste contains nutrients, pathogens, and organic and inorganic contaminants. This study utilized a process consisting of iron electrocoagulation (Fe-EC), microfiltration (MF), and activated carbon (AC) adsorption to treat farm wastewater and explore the reclamation of clean water for irrigation and livestock consumption. Significant removal (>99.9%) of chemical oxygen demand (COD), total organic carbon (TOC), phosphorus (P), turbidity, and microorganisms, as well as ions including magnesium, calcium, sulfur, and silica was achieved by the combined EC-MF-AC process. Specifically, a charge loading of ∼37,500 C/L in a continuous-flow EC configuration, followed by MF, achieved more than 95% removal of TOC and COD. Characterization of produced flocs and foam via scanning-electron microscopy with energy-dispersal spectroscopy and Fourier transform infrared spectroscopy confirmed the removal of ions, including calcium, sulfur, and silica. A key finding was the electrocatalytic conversion of nitrogen species to ammonia gas through the intermediate reduction of nitrate/nitrite, which led to ∼60% total nitrogen (TN) removal. AC treatment further improved TN removal to ∼70%. The Fe-EC process also eradicated >99.9% of bacteria. Preliminary process cost assessment, based on recycled materials for EC electrodes, showed significant cost savings (∼2 times) compared to commercial electrodes.

Dutta, Swapnamoy [ORNL]↗
DOE OSTI2025

Orbital Engineering Band Degeneracy in a Dual-Square Carbon-Oxide Framework

Electron band degeneracies in momentum space give rise to exotic quantum phenomena that have sparked intense interest in condensed matter physics and materials science. Nodal-lines─isolines in k-space formed by the incidental touching of two bands that share the same energy but belong to discrete eigenstates─arise in the presence of symmetries that preclude effective hybridization. Despite recent advances in the design, bottom-up assembly, and engineering of exotic electronic states in graphene nanomaterials, the extension of this approach to access synthetic two-dimensional (2D) quantum materials derived from metal- or covalent-organic frameworks (COFs) has lagged behind. Here we present a molecular orbital engineering approach for designing and fabricating an edge-centered dual square lattice within a π-conjugated 2D-tetraoxa[8]circulene (2D-TOC) COF. First-principles calculations and scanning tunnelling spectroscopy reveal the emergence of Frontier states at the center of a 3 × 3 lattice that give rise to Dirac nodal-lines in 2D-TOC. Our findings not only provide a general guide for the design of conjugated COFs with custom tailored electronic properties from molecular fragments but enable the exploration of emergent topological phenomena in synthetic 2D materials with potential application for high-speed, low-power data processing, transmission, and storage.

Dirac nodal line semimetal↗
DOE OSTI2021

Floodplain Wetland Channel Planform, Cross-Sectional Morphology, and Sediment Characteristics Along an Estuarine to Tidal River Gradient

The formation of wetland channel networks on coastal river floodplains is affected by spatial transitions in tidal-fluvial processes. This study evaluated sedimentation patterns in tidal marshes on the 147-km tidal Columbia River and its 87-km estuary and characterized the cross-sectional geometry and planform morphometry of tidal wetlands along the estuarine to riverine gradient. Tidal marshes were predominantly depositional (median 0.7 cm yr-1, primarily silt), consistent with late-Holocene rates. Marsh sediment accretion rate increased with annual maximum 7-day average daily maximum water depth. Elevation was negatively correlated with accretion rate in the tidal river and positively correlated with total organic carbon (TOC%) in the tidal river and estuary. TOC% was greater in the estuary and, like percent fines, greater farther from the main-channel Columbia River. For four single-channel and six channel-network planforms of tidal marsh, shrub-dominated, and forested wetlands: (1) Spatial patterns of cross-sectional morphology conformed to typical coastal wetland morphology in estuarine reaches up to the tidal river. (2) Reach-based and common slope linear models for channel perimeter on wetland area were predictive in the estuary (R2 > 0.81) and differed between island (n = 144) and mainland (n = 164) wetlands. No planform linear models were predictive for the entire study area or the tidal river. No models for channel outlets were acceptable. (3) Channel perimeter, surface area, and outlets were all highly variable within and among estuarine–riverine reaches. Analyses of sediment, cross-section, and planform support the use of a “natural network paradigm” for wetland-restoration design on tidal river floodplains.

channel morphology↗
DOE OSTI2022

Real-time measurement of parametric influences on the refractive index and length changes in silica optical fibers

In this paper, we present a simple cascaded Fabry-Perot interferometer (FPI) that can be used to measure in real-time the refractive index (RI) and length variation in silica optical fibers caused due to external physical parameters, such as temperature, strain, and radiation. As a proof-of-concept, we experimentally demonstrate real-time monitoring of temperature effects on the RI and length and measure the thermo-optic coefficient (TOC) and thermal expansion coefficient (TEC) by using the cascaded FPI within a temperature range of 21–486°C. The experimental results provide a TEC of 5.53 × 10 −7 /°C and TOC of 4.28 × 10 −6 /°C within the specified temperature range. Such a simple cascaded FPI structure will enable the design of optical sensors to correct for measurement errors by understanding the change in RI and length of optical fiber caused by environment parameters.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2022

Determination of the nonlinear thermo-optic coefficient of silicon nitride and oxide using an effective index method

There is little literature characterizing the temperature-dependent thermo-optic coefficient (TOC) for low pressure chemical vapor deposition (LPCVD) silicon nitride or plasma enhanced chemical vapor deposition (PECVD) silicon dioxide at temperatures above 300 K. In this study, we characterize these material TOC’s from approximately 300-460 K, yielding values of (2.51 ± 0.08) · 10 −5 K −1 for silicon nitride and (5.67 ± 0.53) · 10 −6 K −1 for silicon oxide at room temperature (300 K). We use a simplified experimental setup and apply an analytical technique to account for thermal expansion during the extraction process. We also show that the waveguide geometry and method used to determine the resonant wavelength have a substantial impact on the precision of our results, a fact which can be used to improve the precision of numerous ring resonator index sensing experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Dissolved Inorganic Carbon and Dissolved Organic Carbon Data for the East River Watershed, Colorado (2015-2025)

This data package contains mean values for dissolved organic carbon (DOC) and dissolved inorganic carbon (DIC) for water samples taken from the East River Watershed in Colorado. The East River is part of the Watershed Function Scientific Focus Area (WFSFA) located in the Upper Colorado River Basin, United States. DOC and DIC concentrations in water samples were determined using a TOC-VCPH analyzer (Shimadzu Corporation, Japan). DOC was analyzed as non-purgeable organic carbon (NPOC) by purging HCl-acidified samples with carbon-free air to remove DIC prior to measurement. After the acidified sample has been sparged, it is injected into a combustion tube filled with oxidation catalyst heated to 680 oC. The DOC in samples is combusted to CO2 and measured by a non-dispersive infrared (NDIR) detector. The peak area of the analog signal produced by the NDIR detector is proportional to the DOC concentration of the sample. DIC was determined by acidifying the samples with HCl first, and then purging with carbon-free air to release CO2 for analysis by NDIR detector. Total dissolved nitrogen (TDN) was analyzed using a Shimadzu Total Nitrogen Module (TNM-L) combined with the TOC-L analyzer (Shimadzu Corporation, Japan). TNM-L is a non-specific measurement of total nitrogen (TN). All nitrogen species in samples are combusted to nitrogen monoxide and nitrogen dioxide, then reacted with ozone to form an excited state of nitrogen dioxide. Upon returning to ground state, light energy is emitted. Then, TDN is measured using a chemiluminescence detector. All data reported are the mean values upon minimum of three replicate measurements, with a relative standard deviation < 3%. All samples were analyzed under a rigorous quality assurance and quality control (QA/QC) process. This data package contains (1) a zip file (dic_npoc_data_2014-2025.zip) containing a total of 337 files: 336 data files of DIC and NPOC data from across the Lawrence Berkeley National Laboratory (LBNL) Watershed Function Scientific Focus Area (SFA) which is reported in .csv files per location and a locations.csv (1 file) with latitude and longitude for each location; (2) a file-level metadata (v6_20250901_flmd.csv) file that lists each file contained in the dataset with associated metadata; (3) a data dictionary (v6_20250901_dd.csv) file that contains terms/column_headers used throughout the files along with a definition, units, and data type; and (4) PDF and docx files for the determiniation of Method Detection Limits (MDLs) for DIC and NPOC data, which has been updated in 2026-08. Missing values within the anion data files are noted as either "-9999" or "0.0" for not detectable (N.D.) data. There are a total of 113 locations containing DIC/NPOC data. Update on 2020-10-07: Updated the data files to remove times from the timestamps, so that only dates remain. The data values have not changed. Update on 2021-04-11: Added Determination of Method Detection Limits (MDLs) for DIC, NPOC and TDN Analyses document, which can be accessed as a PDF or with Microsoft Word.Update on 6/10/2022: versioned updates to this dataset was made along with these changes: (1) updated dissolved inorganic carbon and dissolved organic carbon data for all locations up to 2021-12-31, (2) removal of units from column headers in datafiles, (3) added row underneath headers to contain units of variables, (4) restructure of units to comply with CSV reporting format requirements, (5) added -9999 for empty numerical cells, and (6) the addition of the file-level metadata (flmd.csv) and data dictionary (dd.csv) were added to comply with the File-Level Metadata Reporting Format. Update on 2022-09-09: Updates were made to reporting format specific files (file-level metadata and data dictionary) to correct swapped file names, add additional details on metadata descriptions on both files, add a header_row column to enable parsing, and add version number and date to file names (v2_20220909_flmd.csv and v2_20220909_dd.csv). Update on 2023-08-08: Updates were made to both the data files and reporting format specific files. New available anion data was added, up until 2023-01-05. The file level metadata and data dictionary files were updated to reflect the additional data added. Update on 2024-03-11: Updates were made to both the data files and reporting format specific files. New available anion data was added, up until 2023-11-21. Further, revisions to the data files were made to remove incorrect data points (from 1970 and 2001). The reporting format specific files were updated to reflect the additional data added. Revised versions of the PDF and docx files for determination of MDLs for DIC and NPOC were added to replace previous versions. Update on 2025-05-15: Updates were made to both the data files and reporting format specific files. New available DIC and NPOC data was added, up until the end of WY2024 (September 30, 2024). International Generic Sample Numbers (IGSNs), when registered, were added to the data files. The reporting format specific files were updated to reflect the additional data added. Update on 2026-09-01: Updates were made to both the data files and reporting format specific files. New available DIC and NPOC data was added, up until the end of WY2025 (September 30, 2025). Updated versions, as of 2026-08-10, of the PDF and docx files for determination of MDLs for DIC and NPOC data were added to this dataset.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Total metals, sulfur and organic carbon data; Slate River floodplain, Crested Butte, CO; March 2021-October 2021

This data package includes processed and undiluted measurements for metal, sulfur and organic carbon concentrations from pore water (groundwater) samples from the Slate River floodplain of Crested Butte, CO, a focus field site for the SLAC Floodplain Hydro-Biogeochemistry SFA. The data was generated as part of the work targeting the overarching research question for the SLAC SFA: How do ubiquitous subsurface interfaces mediate molecular-scale biogeochemical processes and groundwater quality in floodplains and watersheds? Samples were collected between March and October of 2021. These measurements were all recorded at the Environmental Measurements Facility (EM-1) at Stanford University in Stanford, CA. Groundwater samples were extracted from a network of installed rhizon (Rhizosphere Research Products, part no. 19.60.21F, 0.6 micrometer mesh size) and piezometer wells within the river floodplain. All water samples were shaded from sun exposure during extraction from the subsurface and preserved at 2C until measured at EM-1.Analysis by ICP-MS:Measurements for total metals were performed on an inductively coupled plasma optical emission spectrometer (ICP-OES; iCAP 6300, Thermo Scientific, Cambridge, U.K.). Calibration standards were prepared from the mulit element stock solution (Sigma-Aldrich Multielement standard for ICP, St. Louis, MO) using matrix matched to sample solutions (2% HNO3). Calibration curves included 5 points with correlation coefficients of >0.99. The QC protocol includes a continuing calibration blank and quality control samples that are analyzed just after calibration and again every 20 samples and at the completion of the run. Acceptable QC responses must be between 90-110% of the certified value. Analysis by Total Organic Carbon:Dissolved organic carbon concentrations were quantified on a total organic carbon (TOC) analyzer (TOC-L, Shimadzu, Kyoto, Japan) running the NPOC method. Standard curves were developed using an Organic Carbon Standard from RICCA Chemical Company (Arlington,TX). A series of 4 to 6 standards were automatically diluted by the instrument in a concentration range that spans that of the samples. A blank sample was run just after the calibration curve and at the end of the run. A QC sample was run every 25 samples. Acceptable QC responses must be between 90-110% of the certified value.All files are in csv format.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2023

Total metals, carbon, nitrogen & anion concentration data; Slate River & East River floodplains, Crested Butte, CO; May 2022-October 2022

This data package includes processed and undiluted measurements for metal, total carbon, total nitrogen, and anion concentrations from pore water (groundwater) and surface water samples from the Slate River and East River floodplains of Crested Butte, CO, focus field sites for the SLAC Floodplain Hydro-Biogeochemistry SFA. The data was generated as part of the work targeting the overarching research question for the SLAC SFA: How do ubiquitous subsurface interfaces mediate molecular-scale biogeochemical processes and groundwater quality in floodplains and watersheds? Samples were collected between May and October of 2022. These measurements were all recorded at the Arizona Laboratory for Emerging Contaminants (ALEC) at the University of Arizona located in Tucson, AZ. Groundwater samples were extracted from a network of installed rhizon (Rhizosphere Research Products, part no. 19.60.21F, 0.6 micrometer mesh size) and piezometer wells within the river floodplain. All water samples were shaded from sun exposure during extraction from the subsurface and preserved at 4C until measured at ALEC.Analysis by ICP-MS (metals):Measurements for total metals were made on the Agilent 7700x ICP-MS (for total metals) – Agilent Technologies, Santa Clara, CA. The analytical QA/QC protocol was adapted from US EPA Method 200.8 for analysis by ICP-MS. Calibration standards were prepared from multi-element stock solutions (SPEX Certiprep, Metuchen, NJ). Calibration curves include at least 7 points with correlation coefficients > 0.995. The QC protocol includes a continuing calibration blank (CCB), a continuing calibration verification (CCV) solution and at least one quality control sample (QCS) to be analyzed just after calibration and again after every 12 samples and at the completion of the run. The QCS solutions are from an independent source, such as NIST SRM 1643e - Trace elements in water, or QCS solutions from High Purity Standards (Charleston, SC). Acceptable QC responses must be between 90 and 110% of the certified value. Lastly, a suitable internal standard (usually Rh, In, Ga or Ge) is added using on-line addition into the sample line and mixing tee.Analysis by Shimadzu TOC-L (TOC/TN):The TOC-L system is a combustion technique where liquid samples are injected and combusted into CO2 for carbon detection by non-dispersive infrared (NDIR) and NO for detection by chemiluminescence. A calibration curve using five standard solutions between 0.1 and 7 ppm for carbon and 0.05 and 3.5 ppm for nitrogen is made for each type of measurement with a linearity >0.99. All samples, standards, and QC’s are prepared in 24mL scintillation vials that have been baked for 4hrs at 475 Cº and made using RO water (18.2mΩ). QC’s include a calibration blank check (CCB), continuing calibration check (CCC), and a certified reference material check (CRM). All QC’s are within ±10% error and are run before and after each batch of samples. Samples are diluted and rerun if any measurement concentrations are above the highest standard.Analysis by Ion Chromatography (Anions):The instrument used is the Thermo Scientific Dionex ICS-6000 using AS+AG22 column set for anion analysis with sodium carbonate eluent. A calibration curve using five standard solutions between 5 and 250 umol/L is made with a linearity >0.99. Standards and QC’s are prepared in 15mL polypropylene conical tubes, pipetted along with the samples into 1.5mL polypropylene vials. Dilutions are made using RO water (18.2mΩ). QC’s include a calibration blank check (CCB), continuing calibration check (CCC), and a certified reference material check (CRM). All QC’s are within ±10% error and are run before and after each batch of samples. Samples are diluted and rerun if any measurement concentrations are above the highest standard.All files are in csv format.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2023

Water chemistry in flume channel and hyporheic zone (i.e., porewater) associated with: “Rethinking Aerobic Respiration in the Hyporheic Zone Under Variation in Carbon and Nitrogen Stoichiometry”

Dissolved oxygen (DO), total organic carbon (TOC), total nitrogen (TN), molecular data for organic matter, and biochemical reactions for surface water and porewater (i.e., hyporheic zone) collected from a water recirculating flume located at the University of Texas, Austin. The flume contained real river water from Lower Colorado River(Austin, TX) and clean sand. Hyporheic exchange in the flume was induced through The study aims to understand relationships between aerobic metabolism of organic matter and molecular characteristics of organic matter, such as thermodynamic signature and nitrogen content, through the extent of the hyporheic zone at 10 cm- resolution, and through time. During the experiment, organic matter (dry leaves) was added to the flume and removed after 24 hours. The water samples were collected before the addition of leaves, at the time of removal of leaves, and at hour 72. The water samples were analyzed using ultrahigh resolution Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS) and total organic carbon (TOC) and total nitrogen (TN) analysis. Dissolved oxygen content throughout the surface water and the hyporheic zone of the flume was measured with a large planar optode. This data package is associated with the publication ’ Rethinking Aerobic Respiration in the Hyporheic Zone Under Variation in Carbon and Nitrogen Stoichiometry’ published in Environmental Science and Technology (Turețcaia et al., 2023 https://doi.org/10.1021/acs.est.3c04765). The dataset is comprised of five folders (1) Diss_O2_pic, (2) input_files (3) output_files; (4) python_code; and (5) R_code . Diss_O2_pic contains siximages of dissolved oxygen distribution in a bedform at hours 0, 24, and 72 of the experiment conducted in a large recirculation flume. Images are in separate R and G channels (i.e., RGB). The input_files contains (1) a csv file with FTICR peaks identified within each sample, (2) a csv file with molecular information pertinent to FTICR data with Gibbs free energy calculations adjusted for environmental temperature, (3) a csv file containing concentrations of non-purgeable organic carbon measured throughout the experiment , (4) a csv file containing concentrations of total nitrogen measured throughout the experiment, (5) a csv file containing total biochemical reactions (i.e., transformations) identified in the dataset, (6) a csv containing transformation profiles, and (7) a csv file containing transformations with formulas, and (8) a jpg file with schematic representation of locations for sample collection. The output_files contains (1) and xlsx file containing percent biochemical reactions containing nitrogen identified across all 39 sample, (2) a csv file of merged FTICR data and molecular information files, (3) a csv files containing average Gibbs free energy within sampling domains and at each sampling location, (4) a csv file with average concentrations of dissolved oxygen across sampling locations at hour 0, (5) a csv file with average concentrations of dissolved oxygen across sampling locations at hour 24, (6) a csv file with average concentrations of dissolved oxygen across sampling locations at hour 72, (7) a csv file with percent chemical classes identified across sampling locations at hour 0, (8) a csv file with percent chemical classes identified across sampling locations at hour 24, (9) a csv file with percent chemical classes identified across sampling locations at hour 72, and (10) a csv file containing percent nitrogen containing biochemical reactions identified across sampling locations at hours 0, 24, and 72. The python_code contains seven ipynb files which are Jupyter Notebooks used for data analysis and figures generation. The R_code contains 3 R files with R code used for data analysis and figures generation. This data package contains the processed data used in the associated manuscript. This data has not been previously published.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Electron beam treatment for the removal of 1,4-dioxane in water and wastewater

Electron beam (e-beam) treatment uses accelerated electrons to form oxidizing and reducing radicals when applied to water without the use of external chemicals. In this study, electron beam treatment was used to degrade 1,4-dioxane in several water matrices. Removal improved in the progressively cleaner water matrices and removals as high as 94% to 99% were observed at a dose of 2.3 kGy in secondary effluent. 1,4-dioxane removal was confirmed to be primarily through hydroxyl radical oxidation. The calculated electrical energy per order was found to be 0.53, 0.26, and 0.08 kWh/m 3 /order for secondary effluent (Avg. total organic carbon (TOC) 9.25 mg/L), granular activated carbon effluent (TOC 3.46 mg/L), and ultrapure water, respectively, with a 70% generation and transfer efficiency applied.

1,4-dioxane↗
DOE OSTI2022

Tuscaloosa Marine Shale Laboratory

The Tuscaloosa Marine Shale (TMS) in Louisiana and Mississippi is an Upper Cretaceous source rock formation sandwiched between the sands of the upper and lower Tuscaloosa sections. The TMS is believed to be the source rock for underlying prolific Tuscaloosa sand formation. The TMS has an unproven estimate of 7,000,000,000 bbls of recoverable oil while its current total average production is about 3,000 bbls of oil per day in 2017. In 2013 and 2014, more than 80 wells were drilled horizontally into the TMS that were fractured using multi-stage fracturing technology. The results from this have been mixed, but recent production for several wells show an appealing initial oil production rate of more than 1000 bbl/day. The preliminary core analysis by industry partners and a few literature studies shows that the TMS is one of the most clay-rich and sensitive shales to water. Due to these and other technical problems, there is high risk for the economic development of TMS compared to other shale plays. The experiences of major industrial players in the TMS show the necessity of open and collaborative efforts to better understand the critical gaps in the development of this challenging and potentially highly economic shale play to enable more cost-efficient and environmentally-sound recovery from this unconventional liquid-rich shale play. The overall objective of this project is to form a consortium of science and industry partners to address the following six major objectives using scientific and technical approaches: 1. To improve wellbore integrity by better understanding the sources of the wellbore instability issues, proposing innovative mud and cement design for the TMS. 2. To improve formation evaluation using laboratory techniques for the evaluation of mineralogical composition, organic content, and produced-water chemistry as well as well log and geophysical analysis. 3. To determine the role of geologic discontinuities on fracture growth and shale creep behavior using digital image correlation technique. 4. To investigate the application of stable CO 2 foam and super-hydrophobic proppants for improved reservoir stimulation. 5. To better understand the nature of water/hydrocarbon/CO 2 flow in clay and organic-rich formation and the role of water/fluid interaction on recovery. 6. To prepare better socio-economic environment for TMS development by community engagement. Subsequently, the TMS virtual laboratory conducted testing and analysis of various properties of rock and formation fluids from the TMS, including but not limited to the following: Analyzing reports and logs to better understand the source of wellbore instability in TMS wells; Experiments to design a customized cement based on TMS requirements; Experiments to obtain the mineralogical and geochemical composition of TMS samples; Seismic analysis of TMS geophysical data to better predict total organic carbon (TOC) content and brittleness in TMS; Well log analysis to better estimate the TOC and geo-mechanical properties of TMS; Experiments on formation water to understand the chemistry of produced water; Experiments to determine the role of lamination and natural fractures on fracture propagation or rock deformation using digital image correlation technique in in-direct tensile tests, semi-circular bend test and creep tests Experiments to determine the stability and rheological properties of nanoparticle-stabilized CO 2 foam in TMS rock samples; Experiments to determine fluid dynamics in un-propped TMS fractures and the role of nano-coating of proppants on fluid dynamics in fractures with proppants; Micro-fluidics experiments to enhance the understanding of fluid dynamics in tight liquidrich pores with high clay content; Socio-economic studies to better engage communities in TMS development.

58 GEOSCIENCES↗
DOE OSTI2022

Produced Water and Waste Heat-aided Blowdown Water Treatment: Using Chemical and Energy Synergisms for Value Creation

The project objective was to develop a cooling blowdown water (BDW) treatment process utilizing produced water (PW) and low-grade heat to maximize water reuse and saleable by-product generation while reducing chemical and energy footprints of the treatment. The proposed treatment process consists of mixing, softening, organics and suspended solids removal, reverse osmosis (RO), thermal desalination, and brine electrolysis. BDW samples collected from a local coal-fired power plant and PW samples from two shale gas production wells were used in this study. Each treatment unit was first designed and tested to quantify its treatment efficiency, and its chemical and energy requirements. In addition, a process model was developed and model simulations were conducted based on the experimental results and literature data to optimize the treatment process. A techno-economic analysis was conducted to quantify chemical and energy savings as well as production of 10-lb brine as a saleable product. With the field-collected BDW and PW samples, mixing experiments determined a volumetric mixing ratio 10:1 (BDW:PW) resulted in the best performance of multivalent ions removal and largest chemical savings for softening. Softening of the BDW/PW mixtures using alkaline chemicals (Na 2 CO 3 and NaOH) achieved 95%-100% removal of scaling-forming cations (Ca, Mg, Fe, Ba, Sr) and 60% of silicon, and 10% of total organic carbon (TOC). The mixing and softening treatments yielded an effluent with total dissolved solids (TDS) concentration of 23 g/L. Activated carbon (AC) filtration removed TOC to a low level (< 3 mg/L) and further removed remaining scale-forming divalent metals and silica from the softened water. The AC filtration resulted in a slight reduction of TDS from 23 g/L to 20 g/L, leaving behind only mostly monovalent ions (i.e., sodium and chloride) in the filtered water. These pretreatments yielded a feed water that met the criteria of the downstream reverse osmosis (RO) to prevent membrane fouling. A cross-flow RO system was used to further concentrate the TDS of the AC effluent. Various factors including TDS, pH, and applied pressure were examined and optimal conditions were determined for the co-treatment process. An integrated process consisting of mixing, softening, AC filtration and RO was used to treat a continuous flow (0.25 – 1.2 L/min, or 0.07 – 0.32 gpm) and successfully generated RO permeate as product water (TDS < 0.5 g/L) for reuse in cooling operation, and a concentrate (TDS ~ 45 g/L) to be further treated in a thermal desalination unit. These flow rates meet the FOA’s criterion of 0.01 – 1 gpm. Overall, the co-treatment of BDW/PW allowed shorter ramp-up time compared to treatment of BDW alone. It resulted in 40% and 55% savings of Na 2 CO 3(s) and NaOH, respectively, compared to treating the BDW and PW individually for the same level of softening. The co-treatment also resulted in a 29% energy saving compared to treatment of BDW only for the level of TDS concentration. A thermal desalination system was designed using CFD simulations and manufactured in the WVU Innovation Hub for further treatment of the RO concentrate to generate 10-lb brine. The system has a design flow rate of 2 gpm and has been successfully tested. A bench-scale brine electrolysis system was developed for on-site generation of chlorine/hypochlorite (Cl 2 /OCl - ) and caustic soda (NaOH) as useful chemicals for the co-treatment process. Using salt solutions (0.5 M and 1 M), the system achieved faradaic efficiencies of 93%-97% and 70%-77% for caustic soda and chlorine/hypochlorite generation, respectively. An economic analysis showed that the electricity costs for on-site generation of these chemicals were significantly lower than the chemical prices offered by suppliers. An industrial-scale process model consisting of mixing, softening, AC filtration, RO, thermal desalination, and brine electrolysis was developed using the Aspen Plus V9 in conjunction with Aspen Custom Modeler V9. The model serves as a solvable Aspen Plus model and as basis to form the costing infrastructure. In addition, techno-economic analysis considering capital, operating, and transportation costs was conducted. An optimization solution showed that produced water for mixing is still advantageous in low quantities. The optimum solution approaches a leveled cost of water (LCW) of 2 $/m 3 which becomes cost competitive with nominal water treatment prices.

20 FOSSIL-FUELED POWER PLANTS↗