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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Substantial and overlooked greenhouse gas emissions from deep Arctic lake sediment - supporting data and code

This data package contains data, descriptions, and code-based analyses that were used to support conclusions drawn in “Substantial and overlooked greenhouse gas emissions from deep Arctic lake sediment”, by Freitas et al. (2025) (https://doi.org/10.1038/s41561-024-01614-y). The study evaluated greenhouse gas production along a deep sediment core (20 m) taken in 2018 from below Goldstream Lake, a field site approximately 15 km north of Fairbanks, Alaska.The file “ESSDive_NFreitas_2024_flmd.csv” includes an overview of all other csv files in this data package, namely: sediment descriptions (depth and type of sediment), sediment characterizations (bulk density, gravimetric water content, total carbon, etc.), calculated respiration and temperature sensitivity values associated with year-long incubations of the sediment core, and the R code used to process the dataset. Additional details regarding the content of these files and how the calculations were performed are described in the Methods section of this archive. The “data_dictionary_ESSDive_NFreitas_2024_dd.csv” is a data dictionary for all files included in the data package. Each row in the data dictionary represents a column name in a given file. The Next-Generation Ecosystem Experiments: Arctic (NGEE Arctic), was a research effort to reduce uncertainty in Earth System Models by developing a predictive understanding of carbon-rich Arctic ecosystems and feedbacks to climate. NGEE Arctic was supported by the Department of Energy's Office of Biological and Environmental Research. The NGEE Arctic project had two field research sites: 1) located within the Arctic polygonal tundra coastal region on the Barrow Environmental Observatory (BEO) and the North Slope near Utqiagvik (Barrow), Alaska and 2) multiple areas on the discontinuous permafrost region of the Seward Peninsula north of Nome, Alaska.Through observations, experiments, and synthesis with existing datasets, NGEE Arctic provided an enhanced knowledge base for multi-scale modeling and contributed to improved process representation at global pan-Arctic scales within the Department of Energy's Earth system Model (the Energy Exascale Earth System Model, or E3SM), and specifically within the E3SM Land Model component (ELM).Data package updates- August 2024: Title was updated, R code now includes a process for calculating potential production across the whole sediment column, the "sediment_column_production_potentials_ESSDive_NFreitas_2024.csv" is the associated data output file, and the file level metadata and data dictionaries were updated to reflect the contents of the additional csv file.- October 2024: Title was updated, and a statement was added to Step 2 of the Methods that describes that samples were collected (and exported) in a responsible manner and in accordance with relevant permits and local laws.- January 2025: Updated the associated manuscript details in the Abstract (manuscript title, publication date, DOI link) and in the Related References section (full citation).

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Metagenome-assembled genomes from topsoils collected during NEON campaign in East River, CO (06/14/2018-06/28/2018)

The Watershed Function Science Focus Area (WF SFA) at Lawrence Berkeley National Lab is working to build a mechanistic understanding of the distribution and dynamics of biogeochemical processes in mountainous watersheds and their response to perturbation. In June 2018, the NEON (National Ecological Observatory Network) Airborne Observatory Platform (AOP) performed a taskable airborne imaging campaign to collect visible to shortwave infrared (VSWIR) imaging spectroscopy and LiDAR data across 330 km2 in the Upper East River at Crested Butte, CO. We conducted a parallel ground sampling campaign to sample vegetation traits, as well as soil physical, chemical, and microbiological characteristics. We collected these samples from 438 sites across 12 locations spanning much of the elevation, topographic, and geologic variability across the study area. A subset of 250 samples were used for soil metagenomics which is presented here. In addition, at each site, vegetation samples were collected to measure species-specific leaf water content and leaf mass area, foliar elemental composition and foliar CN stable isotope ratios. Soil samples were collected to measure soil physical properties which include bulk density and soil texture analysis. A suite of soil chemical properties was measured from the samples collected at each site, including pH, organic matter, concentrations exchangeable cations, total elemental composition, and the concentrations of extractable N pools (e.g. total free amino acids, ammonium, nitrate, dissolved organic N, and total dissolved N). Additionally, we have measured soil microbial biomass CN stoichiometry. Here, we present 1982 metagenome-assembled genomes (MAGs) for the bacterial and archaeal community from topsoil collected from during NEON 2018 campaign. All metagenomes were sequenced at JGI (Joint Genome Institute) (GOLD Study ID: Gs0149986). Metagenomes were assembled using JGI Metagenome Workflow (10.1128/mSystems.00804-20). The dataset includes (1) zip files for 1982 MAG fasta files (neon_genomes1-5.tar.gz, split into 5 tarballs to keep tarballs under 0.5 GB), (2) neon_Gs0149986_samples_soilproperties_metagenomes.csv: the sample information together with the accession numbers for the underlying metagenomes and the associated soil physical and chemical measurements in NMDC (National Microbiome Data Collaborative) compliant format, (3) neon_Gs0149986.kml: location bounding box file for the sampled locations, (4) samples.csv: sample metadata file used to register Internationall Generic Sample Numbers (IGSNs), (5) flmd.csv: file level metadata file, and (6) dd.csv: data dictionary file. This work was supported by the Watershed Function Science Focus Area at Lawrence Berkeley National Laboratory funded by the US Department of Energy, Office of Science, Biological and Environmental Research under Contract No. DE-AC02-05CH11231.

2018 NEON and 2025 CHESS Campaigns↗
DOE OSTI2026

Meteoric 10Be Flux Calibration Data for the East River Watershed, Colorado, USA

This data package contains tabular and geospatial data used to quantify and model meteoric beryllium-10 fluxes in the East River watershed, Colorado, USA. The tabular component includes calibration-site data from five glacial moraine sites and includes environmental variables used to evaluate spatial controls on meteoric 10Be delivery, including elevation, mean annual precipitation (MAP), mean snow depth, and mean snow water equivalent (SWE). These site-level data were used to compare observed fluxes with environmental gradients across the watershed and to evaluate the effects of erosion correction on flux estimates. The package also includes supporting slope and curvature values used to assess topographic inputs to the erosion analysis. A second component of the data package contains updated manuscript tables and regression outputs used to summarize the relationships between meteoric 10Be flux and environmental predictors. These tables include meteoric 10Be sample information and AMS results, site-level environmental values, site-level meteoric 10Be inventory and flux values, watershed-averaged predicted fluxes, soil bulk density measurements, fine-fraction values, soil pH measurements, and regression statistics including slope, intercept, coefficient of determination, and p-value. The regression products include both standard linear regressions and regressions in which the intercept is constrained to pass through zero, and they support the analyses presented in the companion manuscript. Together, these tabular files provide the numerical basis for the manuscript tables and the regression-based interpretation of meteoric 10Be flux variability in a snow-dominated mountain watershed. The geospatial component of the package consists of GeoTIFF raster files used to generate the map products presented in Figures 2 and 6 of the companion manuscript. These rasters represent watershed-scale spatial layers for environmental variables and regression-based predictions of meteoric 10Be flux. This dataset contains comma-separated values files (.csv), Microsoft Excel files (.xlsx), GeoTIFF raster files (.tif), and upporting metadata files, including CSV data dictionaries and readme text files (.csv, .txt). The tabular files can be opened with standard spreadsheet software, and the raster files can be viewed and analyzed in GIS software such as ArcGIS Pro or QGIS. Together, these files document the numerical and spatial datasets used to calibrate and predict meteoric 10Be delivery in the East River watershed.

East River↗
DOE OSTI2026

Soil carbon stocks from soil organic carbon at the Teller 47, Teller 27, and Kougarok 86 field sites, Seward Peninsula, Alaska, 2021 – 2023

Carbon stored in permafrost soils represents the largest terrestrial storage and hence has key significance for the global carbon cycle, yet the site-specific estimates of permafrost soil carbon are limited. To better understand permafrost carbon storage, soil organic content (SOC) was measured from soils collected at the Teller 27, Teller 47, and Kougarok 86 field sites on the Seward Peninsula, Alaska in the summers of 2019 and 2021-2023. Soil samples were collected from locations with and without near-surface permafrost to varied depths within the permafrost, where present. In addition to sample collection for soil organic carbon analysis, bulk density samples were also collected within each soil profile to allow for calculation of carbon stocks. Carbon to nitrogen ratios are also reported. Location data were collected at each observation point using a handheld GPS unit with waypoint averaging to reduce location measurement error to within 3 m. SOC was measured using elemental analysis in the laboratory. This dataset contains a *.csv file of soil carbon stocks, a *.kml file of measurement locations, a *.pdf user guide, a *.csv data dictionary, and a *.csv file level metadata.

EARTH SCIENCE > CRYOSPHERE > FROZEN GROUND↗
DOE OSTI2026

Dated soil C–N–P profiles, water quality, and chamber fluxes across Ohio and Michigan wetlands (2024–2025)

This dataset includes dated soil core chemistry (bulk density, phosphorus, nitrogen and carbon concentrations), water quality, and chamber flux measurements collected from wetlands in the Midwest United States—12 sites in Ohio, one site in Indiana, one site in Michigan—collected in the spring or summer of 2024 or 2025, all in (.csv) format. These data were generated to examine how wetland restoration, management activities, and time since restoration affect biogeochemical processes, carbon sequestration, nutrient accumulation, water quality, and greenhouse gas emissions. Specifically, these data aim to investigate how restored wetlands differ from natural wetlands in terms of carbon, nitrogen, phosphorus dynamics, as well as carbon dioxide and methane fluxes. Also included are surface and porewater quality parameters and chamber flux measurements across these different wetlands. Sampling was conducted at various sites representing a range of restoration stages, from about 4 years post-restoration up to 105 years post-restoration, and also includes a natural wetland used as a reference in Michigan. These data can be used to determine carbon sequestration rates, nutrient cycling, and to enhance our understanding of biogeochemical responses to wetland restoration in temperate ecosystems. This data package contains (1) a csv file (Water_Quality.csv) containing water quality data (dissolved organic carbon, total dissolved nitrogen, and temperature) organized by location; (2) a csv file (Soil_C_N_P_Seq.csv) containing carbon, nitrogen, and phosphorus concentrations at each soil level and time of each soil level, as well as their sequestration rates; (3) a csv file (CH4_CO2_Flux.csv) including methane and carbon dioxide fluxes that were measured with a chamber; (4) a file-level metadata (FLMD.csv) file that lists each file contained in the dataset with associated metadata; (5) a data dictionary (DD.csv) file that contains terms/column headers used throughout the files along with a definition, units, and data type; and (6) a locations metadata file (Location_metadata.csv).

Earth Science > Atmosphere > Atmospheric Chemistry↗
DOE OSTI2019

Root-soil depth profile in Luquillo Experimental Forest, Puerto Rico, February, 2019

With an objective of associating the distribution of roots in the soil profile with functional attributes related to phosphorus nutrition, 1-m cores were collected from sites in the Luquillo Experimental Forest, Puerto Rico, in February, 2019. The sampled sites were ridge and valley locations at El Verde and Icacos with soils that differ in parent material and phosphorus fertility. Depth profiles of soil physical characteristics (bulk density, moisture content, and particle size distribution), phosphorus content (total phosphorus, organic phosphorus, and resin or available phosphorus), soil and root-associated phosphatase activity, and fine-root traits (biomass, specific root length and area, and phosphorus content) were determined.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2019

Preparation and electrical conductivity of graphitic carbon-infused copper alloys

By electron-beam (e-beam) melting, we prepared 0.4 wt% carbon-infused copper (CuCv4), and a copper control without carbon addition (CuCv0). Scanning electron microscopy and helium ion microscopy (HIM) were performed on the as-solidified surface, fracture surface, and ion-polished surface of the CuCv4 sample. The results revealed that graphitic carbon flakes cover the as-solidified surface, and carbon nanoparticles and clusters exist in the fracture and ion-polished surfaces. HIM on the ion-polished surface revealed a unique ripple-shaped feature, which is possibly associated with the infusion of carbon nanoribbons in the copper matrix. The bulk densities were measured to be 8.86 and 8.53 g/cm 3 , which correspond to relative densities of 98.9% and 96.4% for the CuCv0 and CuCv4 samples, respectively. Also, apparent electrical conductivities were measured to be 56.9 and 57.5 MS/m, respectively, for the e-beam melted CuCv0 and CuCv4 samples. These values correspond to true electrical conductivities of 100.5% IACS (International Annealed Copper Standard) and 107.4% IACS after correction for the porosity. Thus, our results reveal remarkable promise of using covetic copper for the next generation conductors in energy applications from microelectronic devices to high-power transmission cables.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Measuring Rotation and Manure Effects in an Iowa Farm Soil Health Assessment

Core Ideas Farms with known management histories contribute to soil health research. Rotation‐based systems may increase soil organic carbon when combined with appropriate tillage. Inherent soil properties must be considered in soil health assessments. Rotation effects were more noticeable than manure effects on soil health groupings. Data from on‐farm sites with known management histories are needed to quantify soil biological, chemical, and physical properties influencing carbon stocks and soil health. Surface (0–15 cm) and deep core (0–122 cm) soil samples were collected from fields under two rotations in Boone County, IA. The first was a 5‐yr corn [ Zea mays (L.)], soybean [ Glycine max (L.) Merr.], corn, oat [ Avena sativa (L.)], and alfalfa [ Medicago sativa (L.)] rotation to which 0, 18, or 36 Mg ha −1 of a manure/biosolids mixture was applied prior to planting corn. The second was an 8‐yr rotation with 6 yr of mixed grass and legume pasture followed by corn and an oat crop within which the pasture mixture was reestablished. Soil samples were collected evenly across the predominant soil map units (SMUs). Bulk density (BD), soil organic C (SOC), water‐stable aggregates (WSA), microbial biomass carbon (MBC), pH, Mehlich‐3 and diethylenetriaminepentaacetic acid (DTPA) extractable nutrients, electrical conductivity (EC), and nitrogen (total‐, NH 4 –, and NO 3 –N) were measured. Surface SOC data were consistent with Soil Survey values for the various SMUs. Crop rotation effects were more noticeable than manure/biosolid application rate effects. Data from this study were combined with previously published SOC data in Iowa. Results suggest extended rotation systems or those with cover crops may increase SOC 8 ± 4 g kg −1 compared to corn–soybean rotations (33 vs. 25 g kg −1 ). This study provides on‐farm reference values for soil health assessment tools and draws attention to the importance of inherent soil properties for these assessments.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2019

Impacts of Nitrogen Rate and Landscape Position on Soils and Switchgrass Root Growth Parameters

Core Ideas Nitrogen rate did not affect soil properties for Oklahoma, South Dakota, and Virginia. Landscape position affected soil properties under higher slope. Nitrogen rate affected root N, surface area, and weight for the total profile. Landscape position affected the root C and N. Switchgrass roots can increase C accumulation and reduce risk of N loss in soils. ABSTRACT Switchgrass ( Panicum virgatum L.) has been recognized as a potential bioenergy feedstock, and can positively impact soils and the environment. The experimental sites were established in 2008 at three locations with each in Oklahoma (OK), South Dakota (SD), and Virginia (VA) to assess the impacts of N fertilization rate (N rate; low, 0 kg ha −1 ; high, 112 kg ha −1 ) and landscape position (shoulder, backslope, and footslope) on select soil properties and root growth parameters. Data indicate that N rate did not affect soil bulk density (BD), pH, electrical conductivity (EC), soil organic carbon (SOC), and total nitrogen (TN) for any of five depths. Landscape position impacted some of these properties by depth, depending on location. The N rate influenced root weight (RW), root surface area (RSA), and root total nitrogen (RTN) for the total profile (0–100‐cm depth) depending on local site conditions. The landscape position impacted RW, root total carbon (RTC), and RTN for total profile according to different site conditions. The interactions of landscape position by N rate on switchgrass root parameters were significant. The findings in this study indicate that the root system of switchgrass could improve soils and increase C accumulation and reduce the risk of N loss to benefit the environment.

09 BIOMASS FUELS↗
DOE OSTI2019

Do Cover Crops and Corn Residue Removal Affect Soil Thermal Properties?

Soil thermal properties govern the transport and storage of heat in the soil. How management practices such as crop residue removal and cover crop (CC) use affect these soil properties is not well understood. For example, CCs could provide physical cover and improve soil properties after main crop residue removal and thus ameliorate the negative effects of residue removal on soil thermal properties. We measured changes in soil thermal properties including soil thermal conductivity, thermal diffusivity, volumetric heat capacity, and related properties under corn (Zea mays L.) residue removal with and without winter cereal rye (Secale cereale L.) under a 6-yr irrigated no-till continuous corn experiment on a silt loam in south central Nebraska. Cover crops did not affect thermal properties, but corn residue removal reduced field thermal conductivity by 12 to 41% and volumetric heat capacity by 6 to 49% during the growing season for the 0- to 5-cm depth. Residue removal also reduced laboratory thermal conductivity by 19% at –0.03-MPa and by 28% at –1.5-MPa matric potential. Residue removal also reduced volumetric heat capacity in the laboratory by 23% at both matric potentials in the 0- to 10-cm depth. Neither residue removal nor CC affected thermal diffusivity. Thermal conductivity was more strongly correlated with soil water content than with bulk density and soil organic C. Altogether, CC had no effect on thermal properties, but corn residue removal could reduce the soil’s ability to conduct heat relative to no removal.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2012

Analysis of the Tank 6F Final Characterization Samples-2012 (U)

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) to provide sample preparation and analysis of the Tank 6F final characterization samples to determine the residual tank inventory prior to grouting. Fourteen residual Tank 6F solid samples from three areas on the floor of the tank were collected and delivered to SRNL between May and August 2011. These Tank 6F samples were homogenized and combined into three composite samples based on a proportion compositing scheme and the resulting composite samples were analyzed for radiological, chemical and elemental components. Additional measurements performed on the Tank 6F composite samples include bulk density and water leaching of the solids to account for water soluble components. The composite Tank 6F samples were analyzed and the data reported in triplicate. Sufficient quality assurance standards and blanks were utilized to demonstrate adequate characterization of the Tank 6F samples. The main evaluation criteria were target detection limits specified in the technical task request document. While many of the target detection limits were met for the species characterized for Tank 6F some were not met. In a few cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. The isotopes whose detection limits were not met in all cases included Sn-126, Sb-126, Sb-126m, Eu-152, Cm-243 and Cf-249. SRNL, in conjunction with the customer, reviewed all of these cases and determined that the impacts of not meeting the target detection limits were acceptable. Based on the analyses of variance (ANOVA) for the inorganic constituents of Tank 6F, all the inorganic constituents displayed heterogeneity. The inorganic results demonstrated consistent differences across the composite samples: lowest concentrations for Composite Sample 1, intermediate-valued concentrations for Composite Sample 2, and highest concentrations for Composite Sample 3. The Hg and Mo results suggest possible measurement outliers. However, the magnitudes of the differences between the Hg 95% upper confidence limit (UCL95) results with and without the outlier and the magnitudes of the differences between the Mo UCL95 results with and without the outlier do not appear to have practical significance. It is recommended to remove the potential measurement outliers. Doing so is conservative in the sense of producing a higher UCL95 for Hg and Mo than if the potential outliers were included in the calculations. In contrast to the inorganic results, most of the radionuclides did not demonstrate heterogeneity among the three Tank 6F composite sample characterization results.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2012

Analysis of the Tank 5F Final Characterization Samples-2011 (U)

The Savannah River National Laboratory (SRNL) was requested by SRR to provide sample preparation and analysis of the Tank 5F final characterization samples to determine the residual tank inventory prior to grouting. Two types of samples were collected and delivered to SRNL: floor samples across the tank and subsurface samples from mounds near risers 1 and 5 of Tank 5F. These samples were taken from Tank 5F between January and March 2011. These samples from individual locations in the tank (nine floor samples and six mound Tank 5F samples) were each homogenized and combined in a given proportion into 3 distinct composite samples to mimic the average composition in the entire tank. These Tank 5F composite samples were analyzed for radiological, chemical and elemental components. Additional measurements performed on the Tank 5F composite samples include bulk density and water leaching of the solids to account for water soluble species. With analyses for certain challenging radionuclides as the exception, all composite Tank 5F samples were analyzed and reported in triplicate. The target detection limits for isotopes analyzed were based on customer desired detection limits as specified in the technical task request documents. SRNL developed new methodologies to meet these target detection limits and provide data for the extensive suite of components. While many of the target detection limits were met for the species characterized for Tank 5F, as specified in the technical task request, some were not met. In a few cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. The Technical Task Request allows that while the analyses of these isotopes is needed, meeting the detection limits for these isotopes is a lower priority than meeting detection limits for the other specified isotopes. The isotopes whose detection limits were not met in all cases included the following: Al-26, Sn-126, Sb-126, Sb-126m, Eu-152 and Cf-249. SRNL, in conjunction with the plant customer, reviewed all these cases and determined that the impacts were negligible.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

Statistical Analysis of Tank 5 Floor Sample Results (U)

Sampling has been completed for the characterization of the residual material on the floor of Tank 5 in the F-Area Tank Farm at the Savannah River Site (SRS), near Aiken, SC. The sampling was performed by Savannah River Remediation (SRR) LLC using a stratified random sampling plan with volume-proportional compositing. The plan consisted of partitioning the residual material on the floor of Tank 5 into three non-overlapping strata: two strata enclosed accumulations, and a third stratum consisted of a thin layer of material outside the regions of the two accumulations. Each of three composite samples was constructed from five primary sample locations of residual material on the floor of Tank 5. Three of the primary samples were obtained from the stratum containing the thin layer of material, and one primary sample was obtained from each of the two strata containing an accumulation. This report documents the statistical analyses of the analytical results for the composite samples. The objective of the analysis is to determine the mean concentrations and upper 95% confidence (UCL95) bounds for the mean concentrations for a set of analytes in the tank residuals. The statistical procedures employed in the analyses were consistent with the Environmental Protection Agency (EPA) technical guidance by Singh and others [2010]. Savannah River National Laboratory (SRNL) measured the sample bulk density, nonvolatile beta, gross alpha, and the radionuclide1, elemental, and chemical concentrations three times for each of the composite samples. The analyte concentration data were partitioned into three separate groups for further analysis: analytes with every measurement above their minimum detectable concentrations (MDCs), analytes with no measurements above their MDCs, and analytes with a mixture of some measurement results above and below their MDCs. The means, standard deviations, and UCL95s were computed for the analytes in the two groups that had at least some measurements above their MDCs. The identification of distributions and the selection of UCL95 procedures generally followed the protocol in Singh, Armbya, and Singh [2010]. When all of an analyte's measurements lie below their MDCs, only a summary of the MDCs can be provided. The measurement results reported by SRNL are listed, and the results of this analysis are reported. The data were generally found to follow a normal distribution, and to be homogenous across composite samples.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

Analysis of the Tank 6F Final Characterization Samples-2012

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) to provide sample preparation and analysis of the Tank 6F final characterization samples to determine the residual tank inventory prior to grouting. Fourteen residual Tank 6F solid samples from three areas on the floor of the tank were collected and delivered to SRNL between May and August 2011. These Tank 6F samples were homogenized and combined into three composite samples based on a proportion compositing scheme and the resulting composite samples were analyzed for radiological, chemical and elemental components. Additional measurements performed on the Tank 6F composite samples include bulk density and water leaching of the solids to account for water soluble components. The composite Tank 6F samples were analyzed and the data reported in triplicate. Sufficient quality assurance standards and blanks were utilized to demonstrate adequate characterization of the Tank 6F samples. The main evaluation criteria were target detection limits specified in the technical task request document. While many of the target detection limits were met for the species characterized for Tank 6F some were not met. In a few cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. The isotopes whose detection limits were not met in all cases included Sn-126, Sb-126, Sb-126m, Eu-152, Cm- 243 and Cf-249. SRNL, in conjunction with the customer, reviewed all of these cases and determined that the impacts of not meeting the target detection limits were acceptable. Based on the analyses of variance (ANOVA) for the inorganic constituents of Tank 6F, all the inorganic constituents displayed heterogeneity. The inorganic results demonstrated consistent differences across the composite samples: lowest concentrations for Composite Sample 1, intermediate-valued concentrations for Composite Sample 2, and highest concentrations for Composite Sample 3. The Hg and Mo results suggest possible measurement outliers. However, the magnitudes of the differences between the Hg 95% upper confidence limit (UCL95) results with and without the outlier and the magnitudes of the differences between the Mo UCL95 results with and without the outlier do not appear to have practical significance. It is recommended to remove the potential measurement outliers. Doing so is conservative in the sense of producing a higher UCL95 for Hg and Mo than if the potential outliers were included in the calculations. In contrast to the inorganic results, most of the radionuclides did not demonstrate heterogeneity among the three Tank 6F composite sample characterization results.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

LANL Response to SRS Requirement G-ESR-G-00035 Item 11 Bed Temperature, Revision 4

Los Alamos National Laboratory has identified a number of plutonium-bearing materials that will be placed in interim storage in 3013 containers per requirements of DOE-STD-3013- 2004, or DOE-STD-3013-2012. Before these items can be considered for storage at Savannah River Site, 20 points of agreement, described in Savannah River Site (SRS) document G-ESR-G-00035, Revision 1, must be documented and provided to SRS for review. These agreements include documentation that the requirements of the 3013 Standard are met and the storage facility’s safety envelope is not compromised. Point 11 of the 20 points is the requirement that material be stabilized at 950°C for a minimum of two hours prior to packaging. This report addresses the Point 11 requirement, describing the controls used during stabilization to ensure that the material is properly stabilized using either a batch (calciner boat) or continuous process (Advanced Recovery and Integrated Extraction System [ARIES] direct metal oxidation unit 2 [DMO-2] and recycle oxide calcination). These controls include verification of the furnace controller thermocouple profile and verification of the profiles for the two thermocouples located in the bed and/or calciner tube hot zone. Revision 4 to this document only modifies the ARIES DMO-2 process controls. Batch processing requirements are unchanged. Changes to the DMO-2 process include use of alternate augers with differing pitch values and reduction of the minimum powder bulk density value. The new DMO-3 unit requirements are covered in a separate document.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2014

Carbon Dioxide Sealing Capacity: Textural or Compositional Controls? (Final Scientific/Technical Report)

This research project is aiming to assess the carbon dioxide sealing capacity of most common seal-rocks, such as shales and non-fractured limestones, by analyzing the role of textural and compositional parameters of those rocks. We hypothesize that sealing capacity is controlled by textural and/or compositional parameters of caprocks. In this research, we seek to evaluate the importance of textural and compositional parameters affecting the sealing capacity of caprocks. The conceptual framework involves two testable end-member hypotheses concerning the sealing capacity of carbon dioxide reservoir caprocks. Better understanding of the elements controlling sealing quality will advance our knowledge regarding the sealing capacity of shales and carbonates. Due to relatively low permeability, shale and non-fractured carbonate units are considered relatively impermeable formations which can retard reservoir fluid flow by forming high capillary pressure. Similarly, these unites can constitute reliable seals for carbon dioxide capture and sequestration purposes. This project is a part of the comprehensive project with the final aim of studying the caprock sealing properties and the relationship between microscopic and macroscopic characteristics of seal rocks in depleted gas fields of Oklahoma Panhandle. Through this study we examined various seal rock characteristics to infer about their respective effects on sealing capacity in special case of replacing reservoir fluid with super critical carbon dioxide (scCO 2 ). To assess the effect of textural and compositional properties on scCO 2 maximum retention column height we collected 30 representative core samples in caprock formations in three counties (Cimarron, Texas, Beaver) in Oklahoma Panhandle. Core samples were collected from various seal formations (e.g., Cherokee, Keys, Morrowan) at different depths. We studied the compositional and textural properties of the core samples using several techniques. Mercury Injection Porosimetry (MIP), Scanning Electron Microscopy SEM, and Sedigraph measurements are used to assess the pore-throat-size distribution, sorting, texture, and grain size of the samples. Also, displacement pressure at 10% mercury saturation (Pd) and graphically derived threshold pressure (P c ) were determined by MIP technique. SEM images were used for qualitative study of the minerals and pores texture of the core samples. Moreover, EDS (Energy Dispersive X-Ray Spectrometer), BET specific surface area, and Total Organic Carbon (TOC) measurements were performed to study various parameters and their possible effects on sealing capacity of the samples. We found that shales have the relatively higher average sealing threshold pressure (P c ) than carbonate and sandstone samples. Based on these observations, shale formations could be considered as a promising caprock in terms of retarding scCO 2 flow and leakage into above formations. We hypothesized that certain characteristics of shales (e.g., 3 fine pore size, pore size distribution, high specific surface area, and strong physical chemical interaction between wetting phase and mineral surface) make them an efficient caprock for sealing super critical CO 2 . We found that the displacement pressure at 10% mercury saturation could not be the ultimate representative of the sealing capacity of the rock sample. On the other hand, we believe that graphical method, introduced by Cranganu (2004) is a better indicator of the true sealing capacity. Based on statistical analysis of our samples from Oklahoma Panhandle we assessed the effects of each group of properties (textural and compositional) on maximum supercritical CO 2 height that can be hold by the caprock. We conclude that there is a relatively strong positive relationship (+.40 to +.69) between supercritical CO 2 column height based on P c and hard/ soft mineral content index (ratio of minerals with Mohs hardness more than 5 over minerals with Mohs hardness less than 5) in both shales and limestone samples. Average median pore radius and porosity display a strong negative correlation with supercritical CO 2 retention column height. Also, increasing bulk density is positively correlated with the supercritical CO 2 retention column height. One of the most important factors affecting sealing capacity and consequently the height of supercritical CO 2 column is sorting of the pore throats. We observed a strong positive correlation between pore throat sorting and height of CO 2 retention column, especially in shales. This correlation could not be observed in limestone samples. It suggests that the pore throat sorting is more controlling the sealing capacity in shales and shales with well sorted pore throats are the most reliable lithology as seal. We observed that Brunauer–Emmett–Teller (BET) surface area shows a very strong correlation with CO 2 retention column height in limestone samples while BET surface area did not display significant correlation in shales. Pore structure based on SEM micrographs exhibits strong correlation with CO 2 retention column height in limestones. Both intercrystalline and vuggy structures have negative correlations while intergranular texture has positive correlation in limestone with respect to CO 2 retention column height. Textural effects observed on SEM micrographs did not show statistically significant correlation with supercritical CO 2 retention column height in shale samples. Finally, we showed that increasing hard/soft mineral index is strongly correlated with the displacement pressure in limestone samples. Vuggy texture displays a relatively strong and negative correlation with displacement pressure values at 10% mercury saturation in shale samples.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2014

Interactive Effects of Climate Change and Decomposer Communities on the Stabilization of Wood-Derived Carbon Pools: Catalyst for a New Study

Globally, forest soils store ~two-thirds as much carbon (C) as the atmosphere. Although wood makes up the majority of forest biomass, the importance of wood contributions to soil C pools is unknown. Even with recent advances in the mechanistic understanding of soil processes, integrative studies tracing C input pathways and biological fluxes within and from soils are lacking. Therefore, our research objectives were to assess the impact of different fungal decay pathways (i.e., white-rot versus brown-rot)—in interaction with wood quality, soil temperature, wood location (i.e., soil surface and buried in mineral soil), and soil texture—on the transformation of woody material into soil CO 2 efflux, dissolved organic carbon (DOC), and soil C pools. The use of 13 C-depleted woody biomass harvested from the Rhinelander, WI free-air carbon dioxide enrichment (Aspen-FACE) experiment affords the unique opportunity to distinguish the wood-derived C from other soil C fluxes and pools. We established 168 treatment plots across six field sites (three sand and three loam textured soil). Treatment plots consisted of full-factorial design with the following treatments: 1. Wood chips from elevated CO 2 , elevated CO 2 + O 3 , or ambient atmosphere AspenFACE treatments; 2. Inoculated with white rot (Bjerkandera adusta) or brown rot (Gloeophyllum sepiarium) pure fungal cultures, or the original suite of endemic microbial community on the logs; and 3. Buried (15cm in soil as a proxy for coarse roots) or surface applied wood chips. We also created a warming treatment using open-topped, passive warming chambers on a subset of the above treatments. Control plots with no added wood (“no chip control”) were incorporated into the research design. Soils were sampled for initial δ 13 C values, CN concentrations, and bulk density. A subset of plots were instrumented with lysimeters for sampling soil water and temperature data loggers for measuring soil temperatures. To determine the early pathways of decomposition, we measured soil surface CO 2 efflux, dissolved organic C (DOC), and DO 13 C approximately monthly over two growing seasons from a subsample of the research plots. To determine the portion of soil surface CO 2 efflux attributable to wood-derived C, we used Keeling plot techniques to estimate the associated δ 13 C values of the soil CO 2 efflux. We measured the δ 13 CO 2 once during the peak of each growing season. Initial values for soil δ 13 C values and CN concentrations averaged across the six sites were -26.8‰ (standard error = 0.04), 2.46% (se = 0.11), and 0.15% (se = 0.01), respectively. The labeled wood chips from the Aspen FACE treatments had an average δ13C value of -39.5‰ (se 0.10). The >12 ‰ isotopic difference between the soil and wood chip δ 13 C values provides the basis for tracking the wood-derived C through the early stages of decomposition and subsequent storage in the soil. Across our six research sites, average soil surface CO 2 efflux ranged from 1.04 to 2.00 g CO 2 m -2 h -1 for the first two growing seasons. No wood chip controls had an average soil surface CO 2 efflux of 0.67 g CO 2 m -2 h -1 or about half of that of the wood chip treatment plots. Wood-derived CO 2 efflux was higher for loam textured soils relative to sands (0.70 and 0.54 g CO 2 m -2 h -1 , respectively; p = 0.045)), for surface relative to buried wood chip treatments (0.92 and 0.39 g CO 2 m -2 h -1 , respectively; p < 0.001), for warmed relative to ambient temperature treatments (0.99 and 0.78 g CO 2 m -2 h -1 , respectively; 0.004), and for natural rot relative to brown and white rots (0.93, 0.82, and 0.78 g CO 2 m -2 h -1 , respectively; p = 0.068). Our first two growing seasons of soil surface CO 2 efflux data show that wood chip location (i.e., surface vs. buried chip application) is very important, with surface chips loosing twice the wood-derived CO 2 . The DOC data support this trend for greater loss of ecosystem C from surface chips. This has strong implications for the importance of root and buried wood for ecosystem C retention. This strong chip location effect on wood-derived C loss was significantly modified by soil texture, soil temperature, decomposer communities, and wood quality as effected by potential future CO 2 and O 3 levels.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2012

Titanium subhydride potassium perchlorate (TiH1.65/KClO4) burn rates from hybrid closed bomb-strand burner experiments.

A hybrid closed bomb-strand burner is used to measure the burning behavior of the titanium subhydride potassium perchlorate pyrotechnic with an equivalent hydrogen concentration of 1.65. This experimental facility allows for simultaneous measurement of the closed bomb pressure rise and pyrotechnic burn rate as detected by electrical break wires over a range of pressures. Strands were formed by pressing the pyrotechnic powders to bulk densities between 60% and 90% theoretical maximum density. The burn rate dependance on initial density and vessel pressure are measured. At all initial strand densities, the burn is observed to transition from conductive to convective burning within the strand. The measured vessel pressure history is further analyzed following the closed bomb analysis methods developed for solid propellants.

36 MATERIALS SCIENCE↗