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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Self-supervised and multi-fidelity learning for extended predictive soil spectroscopy

Infrared spectroscopy is a cost-effective, non-destructive, and environmentally benign technology that is increasingly recognized as an important solution for meeting the global demand for soil data. While both near-infrared (NIR) and mid-infrared (MIR) diffuse reflectance spectroscopy enable rapid estimation of soil properties, they present a significant trade-off: NIR offers superior scalability and lower operational costs, whereas MIR provides higher analytical fidelity by capturing fundamental molecular vibrations. In this study, we propose a self-supervised, multi-fidelity learning framework designed to bridge this gap. Our approach leverages large-scale MIR spectral libraries to learn a compact, transferable latent representation, into which NIR spectra are subsequently aligned for downstream prediction. The workflow consists of pretraining a latent model on a large MIR library, adapting the representation using a smaller paired NIR–MIR dataset, and evaluating generalization on an independent external test set. Across a range of chemical and physical soil properties, we found that MIR-derived embeddings improved prediction accuracy relative to baseline models that used raw MIR inputs. Predictions derived from the spectrum conversion (NIR to MIR) task did not match the performance of the original MIR spectra but were similar or superior to predictive performance of NIR-only models, suggesting the unified spectral latent space can effectively leverage the larger and more diverse MIR dataset for prediction of soil properties not well represented in current NIR libraries.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Fast redox switches lead to rapid transformation of goethite in humid tropical soils: A Mössbauer spectroscopy study

Abstract Humid tropical forest soils experience frequent rainfall, which limits oxygen diffusion and creates redox heterogeneity in upland soils. In this study we gauged the effect of short‐term anoxic conditions on Fe mineralogy of relatively Fe‐ and C‐rich surface soils (C/Fe mole ratio ∼5) from a humid tropical forest in Puerto Rico. Soils subjected to 4‐d oxic/anoxic oscillation were characterized by selective chemical extractions, Mössbauer spectroscopy (MBS), and X‐ray diffraction. Chemical extraction data suggested that rapidly switching redox conditions had subtle effects on bulk Fe mineralogy. Mössbauer, on the other hand, indicated that (a) the soil Fe is a mixture of goethites of varying characteristics with minor contributions from ferrihydrite (<5%) and Fe(III)‐organic matter (OM) phases (∼10%), and (b) anoxic conditions rapidly transformed all forms of goethite to relatively stable Fe oxides. Such fast changes in goethite features could be due to rapid depletion and sorption of bio‐released structural Al or sorbed OM onto residual soil components. The rapid temporal changes in MBS parameters and corresponding pore water nominal oxidation state of C values suggest that Fe‐C transformations in these upland tropical soils are complex and intricately coupled. A comprehensive understanding of the fate of Fe, Al, and OM (Fe‐organic moieties) during redox switches and concurrent changes in pore water chemistry is critical for development of robust transport models in humid tropical soils, which are subject to episodic low‐redox events.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Using mid-infrared spectroscopy to estimate soil microbial properties at the continental scale

Understanding microbial community properties is critical to improving the predictions of biogeochemical processes for enhancing soil carbon sequestration. Here, in this observational study, mid-infrared (MIR) spectroscopy and partial least squares regression was used to predict soil microbial and chemical properties from diverse ecosystems across the continental USA. Random calibration and validation demonstrated the prediction potential for soil properties using MIR spectra, with the strongest predictions for microbial respiration, followed by microbial biomass carbon and nitrogen, ß-glucosidase activity, as well as soil chemical properties including organic carbon and total nitrogen. Microbial properties were mainly positively correlated to spectral regions associated with aliphatic C-H groups and C=O stretches of polysaccharides and negatively correlated to quartz and silicate-associated regions. We conclude that MIR spectroscopy can characterize soil microbial functions and be useful for the improvement of continental-scale soil carbon modeling and prediction programs.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2023

Applying NIR and MIR spectroscopy for C and soil property prediction in northern cold-region ecosystems. Which approach works better?

Here, developing reliable predictions of soil attributes is necessary to understand northern cold-region climate-soil feedback. Calibration models using near-infrared (NIR) and mid-infrared (MIR) spectroscopy were developed to predict eight commonly measured soil properties for 119 soil samples representing a range of vegetation types, parent materials, and soil types spanning >23° of latitude from southeast Alaska to the Canadian high Arctic. In order to obtain a more accurate prediction, this study compared the performance of linear and non-linear calibration techniques, including lasso regression (Lasso), support vector machine (SVM), random forest (RF) and classic partial least squares (PLS) to predict different soil properties of these soils. Comparing the four models, we noticed that their performance was quite similar for MIR overall, while NIR achieved better results with a PLS model for our dataset. PLS coupled with MIR showed a better performance for soil parameters, such as total organic carbon (TOC), total nitrogen (TN), cation exchange capacity (CEC) and clay (R-squared of 0.9, 0.81, 0.80, and 0.84) when compared with NIR (R-squared of 0.85, 0.72, 0.81 and 0.68). However, using either MIR or NIR spectroscopy, PLS predictions for bulk density (BD) and sand content were not accurate. The variable importance analysis based on the PLS model successfully estimated the relative contribution of wavelengths influencing soil property predictions most. Overall, TOC, TN, CEC and clay mineral predictions are closely related to the occurrence of specific spectral bands in the MIR region. For example, wavelengths at 2978 and 1761 cm -1 for TOC and TN, as well as at 3064 cm -1 for CEC, were selected as the most influential predictor variables. We demonstrated that MIR spectroscopy is a powerful tool for more extensive monitoring in soils of the northern cold climate region; however, NIR could be utilized for rapid estimates when the highest accuracy is not essential.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

Can Agricultural Management Induced Changes in Soil Organic Carbon Be Detected Using Mid-Infrared Spectroscopy?

A major limitation to building credible soil carbon sequestration programs is the cost of measuring soil carbon change. Diffuse reflectance spectroscopy (DRS) is considered a viable low-cost alternative to traditional laboratory analysis of soil organic carbon (SOC). While numerous studies have shown that DRS can produce accurate and precise estimates of SOC across landscapes, whether DRS can detect subtle management induced changes in SOC at a given site has not been resolved. Here, we leverage archived soil samples from seven long-term research trials in the U.S. to test this question using mid infrared (MIR) spectroscopy coupled with the USDA-NRCS Kellogg Soil Survey Laboratory MIR spectral library. Overall, MIR-based estimates of SOC%, with samples scanned on a secondary instrument, were excellent with the root mean square error ranging from 0.10 to 0.33% across the seven sites. In all but two instances, the same statistically significant (p < 0.10) management effect was found using both the lab-based SOC% and MIR estimated SOC% data. Despite some additional uncertainty, primarily in the form of bias, these results suggest that large existing MIR spectral libraries can be operationalized in other laboratories for successful carbon monitoring.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Sulfur x-ray absorption spectroscopy data from bedrock shale, soil, and floodplain sediment from the East River, Colorado watershed

This dataset includes sulfur x-ray absorption near edge spectroscopy (XANES) data collected on solid samples as a part of the Watershed Function Scientific Focus Area (SFA) located in the Upper Colorado River Basin. The data were collected in order to investigate the speciation of sulfur and degree of shale weathering in solid samples across the watershed and their impact on riverine export of sulfate. Solid samples, including shale, hillslope soil, and floodplain sediment samples collected in 2016-2018, were analyzed by bulk XANES. Density fractions of hillslope soil, including a light fraction representing particulate organic matter and a heavy fraction representing minerals are also analyzed by bulk XANES. Micro-focused XANES on a weathered shale sample (PLM6, 2.7 m) was also performed. Sample locations are included in the 'sample meta data.csv' file, and XANES data for each sample type are included in csv files.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2020

Iron and Phosphorus Geochemistry in High-Centered and Low-Centered Polygon Soils from the Barrow Environmental Observatory, Utqiagvik, Alaska, 2015

This dataset provides chemical characterization of soil cores obtained in triplicate from center and trough positions of a high-centered polygon and center, ridge, and trough positions of a low-centered polygon in the NGEE Arctic research area within the Barrow Environmental Observatory, Utqiagvik, Alaska. Photographs of the 15 collected cores are provided. Cores were collected to thaw depth in early October 2015 and subsequently divided into subsamples for analysis, which included bulk soil horizons (organic or mineral) and finer scale depth increments (minimum 4 cm thickness per increment). Bulk horizons and depth increments were characterized using sequential chemical extractions for Fe and P and with Fe K-edge x-ray absorption spectroscopy. Additional soil parameters such as loss-on-ignition, gravimetric water content, and carbon and nitrogen concentrations were also quantified for bulk horizons. This dataset includes four csv files, one pdf user guide, and one zip folder of *.jpg photos.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).

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2020

Pilot Test Remediation of a Fractured Bedrock Aquifer at the Maywood Superfund Site, Maywood, New Jersey - 20073

The U.S. Army Corps of Engineers (USACE) and Cabrera Services are conducting a Comprehensive Environmental Response, Compensation and Liability Act (CERCLA) Pilot Test treatment of a fractured bedrock aquifer at the Formerly Utilized Sites Remedial Action Program (FUSRAP) Maywood Superfund Site (FMSS) located in Maywood, New Jersey (NJ), USA. The Maywood Chemical Company Superfund Site in Bergen County, NJ is listed on the United States Environmental Protection Agency (USEPA) Superfund National Priorities List (NPL). The National Superfund Comprehensive Environmental Response, Compensation, and Liability Information System (CERCLIS) identification number is NJD980529762. The Maywood Chemical Company Superfund Site (hereafter referred to as the FMSS) consists of 92 designated properties in the communities of Maywood, Lodi and Rochelle Park, NJ. These are collectively known as FMSS 'Vicinity Properties' and include property owned by the federal government (the Maywood Interim Storage Site, or MISS); the Stepan Company (former location of the Maywood Chemical Works, or MCW); 62 residential properties; three properties owned by the state or federal government; four municipal properties; and 21 commercial properties. The Stepan Company property includes contaminated buildings and three remediated U.S. Nuclear Regulatory Commission (NRC) licensed burial pits; the MISS also includes a contaminated building. Contamination on the FMSS is being addressed under three separate actions coordinated by the lead regulator USEPA Region 2. The USACE is addressing thorium (Th) and other wastes at the site defined as 'FUSRAP waste' in the Soils and Buildings and Groundwater Records of Decision (ROD) for the FMSS. Stepan Company is addressing other chemical wastes (non-FUSRAP waste) at the FMSS. The Groundwater ROD [1] was signed into agreement by USACE Division Commander in June 2012 and USEPA Region 2 Administrator in July 2012 and presents the selected remedial actions for Operable Unit (OU) 2 groundwater at the MISS and adjacent properties. The selected remedial action is removal of non-radiologically contaminated soils on the MISS containing arsenic, lithium, and benzene with concentrations above cleanup levels, and monitored natural attenuation (MNA) of arsenic, lithium, and benzene in groundwater. In situ treatment of arsenic in the overburden aquifer using oxidation reduction (redox) alteration will also be performed if needed to meet the groundwater cleanup levels after the source soil is removed. The need for in situ treatment will be determined during the Groundwater ROD review at least three to four years after the contaminated source soil removal is completed. The third action addressing non-FUSRAP chemical wastes will be the responsibility of the Stepan Company as a primary responsible party in this action. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2020

Investigation of Non-Nuclear Plowshare and Vela Uniform Sites - 20447

The Plowshare Program was initiated by the Atomic Energy Commission, a predecessor agency to the US Department of Energy (DOE), to investigate peaceful uses of nuclear devices. 'Vela Uniform,' part of the broader Project Vela, was designed to use nuclear and other explosions to increase the capability of the United States to detect nuclear tests through seismicity. There were underground nuclear tests conducted off the Nevada National Security Site (NNSS) as part of the Plowshare Program (e.g., the Gnome-Coach, New Mexico, Site) and the Vela Uniform Program (e.g., Project Shoal, Nevada, Site) at which the DOE Office of Legacy Management (LM) has been conducting long-term surveillance and maintenance since fiscal year (FY) 2006. There are many additional locations, particularly for the Plowshare Program, that were considered for nuclear tests or used for non-nuclear tests off the NNSS. Some were only named on paper, but at 30 sites, field work such as drilling test wells and conducting tests using conventional explosives was done. A Plowshare nuclear explosion had been proposed at Project Chariot but was canceled in 1962. In 1992, the discovery of soils contaminated with radionuclides from tracer experiments led to a cleanup by the DOE Office of Environmental Management (EM) of the Project Chariot, Alaska, Site, which was completed in 1994. Following the cleanup of the Project Chariot site, EM was concerned that there might be environmental liabilities at other Plowshare or Vela Uniform sites where field investigations were done, even if the nuclear test was never conducted. The EM Program at the Nevada Site Office began examining records and visiting selected locations that were evaluated for Plowshare and Vela Uniform non-nuclear tests. In total, 161 Plowshare and 14 Vela Uniform sites or proposed projects were identified. The Desert Research Institute (DRI) created summaries of the work carried out at these sites and developed a collection of unclassified documents for them. Preliminary investigations had been conducted at these sites by both LM and EM since the early 2000's. In 2016, in preparation for accepting responsibility for the sites, LM started a program to determine if there were any environmental or safety liabilities associated with them. In 2019, LM formally accepted responsibility for these sites off the NNSS where non-nuclear explosive tests were conducted or where underground nuclear tests were proposed as part of the Plowshare and Vela Uniform programs but were never conducted. LM responsibilities will include maintaining institutional knowledge of the sites, responding to public inquiries, and addressing any concerns at each site. To minimize risk associated with site management, LM has archived all historical records compiled by DRI and has performed limited investigations at sites identified by the prior studies as having a higher potential liability. Preserving records related to site operations reduces the risk of doing unnecessary site investigations in the future caused by the loss of institutional knowledge. During the investigations, some maintenance needs were identified and will be addressed by the end of FY 2021. At the end of FY 2021, investigations, maintenance, and archiving activities will be complete. Remnants of test activities found at sites include craters, mud pits, debris, and open boreholes. Open boreholes are being plugged and abandoned in accordance with state regulatory standards. Other issues are being addressed in accordance with land owner requests and preferences as well as state regulations. Archiving activities include the development of project summaries identifying key operational details and current condition to allow site managers to be easily briefed. The LM experience at non-nuclear Plowshare and Vela Uniform sites applies to other programs where there is the potential for liability associated with the non-nuclear aspects of nuclear programs. This may include support activities or early phases of planned nuclear projects. Preserving institutional knowledge enables land managers to adequately address any concerns associated with operations and lowers risk. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2023

Rapid in situ nutrient element distribution in plants and soils using laser-induced breakdown spectroscopy ($\mathrm{LIBS}$)

The aim of this study is to develop and test the applicability of a rapid in situ plant chemistry profiling technique to determine elemental composition of small-volume plant and soil samples obtained from a woody bioenergy crop species, Populus trichocarpa. Expanding the research tools available to characterize the nutrient element correlations among plant tissue types and soil depths is a critical need in the path of understanding productivity and adaptation of plants to variations in external abiotic and biotic factors and developing sustainable perennial bioenergy crops that are co-optimized for biomass valorization aboveground and carbon sequestration belowground. Several plant root, stem, and soil samples were tested using laser-induced breakdown spectroscopy (LIBS) to evaluate the presence and distribution of nutrient elements. Samples were tested as collected and after being dried and cross sectioned to evaluate the effectiveness of using LIBS for in situ analysis on plant samples. The collected LIBS spectra show the elemental peaks were the same in both the as collected and prepared samples for roots and stems. Qualitative amounts of elements such as H, C, N, O, Li, Na, Mg, K, Ca, Fe, Al, and Si were able to be identified rapidly in raw samples. Here in this report we demonstrate suitability of LIBS in obtaining rapid, in situ, elemental distribution in plant and soil samples, utilizing only small sample volumes and minimal sample preparation. This demonstration opens up a new rapid phenotyping avenue necessary to fill the asymmetrical knowledge gaps in belowground performance of plant systems.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

Soil Carbon and Nitrogen Elemental Analysis and Middle Infrared Spectroscopy from the Kougarok Fire Complex, Seward Peninsula, Alaska, 2022

In September and October of 2022, soil samples were collected at the Kougarok Fire Complex near mile marker 86 of the Nome-Taylor Highway on the Seward Peninsula of Alaska. This study site was chosen due to its unique fire history, as the Kougarok Fire Complex has experienced multiple wildfires since 1971. As the Arctic warms, the risk of Arctic tundra fires continues to increase due to warmer summer temperatures and higher frequency of lightning. Burned soil carbon or pyrogenic carbon (PyC) is an important component of C cycling after wildfire, and one that is often overlooked in tundra systems where wildfires are historically rare. To better understand PyC signatures and quantify PyC presence in post-regeneration permafrost regions, soils were sampled from soil pits within the 1971, 2002, and 2019 burn sites, as well as two unburned control sites. At each site, three soil pits were dug to the permafrost table. Soil samples were collected with a trowel from the face of each pit at 10 cm increments down to the permafrost table. Thaw depth, maximum vegetation height, vegetation species composition, and O horizon depth were also collected at each soil pit. An HS2 Hydrosense II Handheld Soil Moisture Sensor was used to collect volumetric soil moisture content at each 10 cm sampling increment. This dataset includes one *.csv of middle infrared spectroscopy measurements of soil samples, one *.csv of field observations, one *.csv of carbon and nitrogen analysis of soil samples, and one *.kml of sampling locations.The Next-Generation Ecosystem Experiments: Arctic (NGEE Arctic) was a 15-year research effort (2012-2027) 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).

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Site and endmember spectra of terrestrial vegetation and soils for the Colorado Headwaters Ecological Spectroscopy Study, June-July 2025

This dataset provides site and endmember spectra collected during the 2025 Colorado Headwaters Ecological Spectroscopy Study (CHESS) campaign. The site spectra were collected to help validate airborne hyperspectral data acquired by the National Ecological Observatory Network's aerial observation platform (NEON AOP). Endmember spectra were collected to augment existing spectral libraries with additional samples of bare surfaces and non-photosynthetic vegetation. All measurements were acquired with an Analytical Spectral Devices (ASD) FieldSpec4 Hi-Res NG (Next Generation) spectroradiometer, which records radiance at 1nm (nanometer) intervals from the ultraviolet to the short-wave infrared (350-2500 nm). The dataset includes spectra measured at meadow sites where the CHESS team also collected vegetation samples for trait analyses. The site spectra were collected with the ASD FieldSpec4 palm grip attachment using an 8° field-of-view foreoptic. Site spectra are integrated measurements of the entire surface within the foreoptic’s field of view. For site-level spectra, the sun is the illumination source. A Spectralon panel mounted on a tripod was used for instrument optimization and white reference measurements for all site spectra. Site spectra were acquired within two hours of solar noon and within 48 hours of a NEON AOP overflight. Site spectra are labeled by date, sampling area, and site number according to the naming conventions of the CHESS campaign’s data management plan. The dataset also contains endmember spectra in the following categories: photosynthetic vegetation (PV), non-photosynthetic vegetation (NPV), bare (soil/rock), and flowers. Endmember measurements were acquired using either the contact probe or the leaf clip attachments of the ASD FieldSpec4. In these configurations, the bulb inside the spectrometer provides the light source for the measurements. The spectrometer was optimized and white reference measurements were recorded using the circular white pucks attached to the contact probe and leaf clip. Because they do not rely on solar illumination, contact probe and leaf clip measurements were collected during a broader time frame than the palm grip site spectra. Some endmembers were measured at CHESS meadow sites, while others were collected within the larger sampling area or in nearby locations (e.g. Gothic Townsite) with similar characteristics. Radiance, reflectance, and metadata files are split into three subfolders according to measurement type: proximal/palm grip (prx), contact probe (cp), and leaf clip (lc). Radiance spectra are provided in ASD file format (.asd file extension). All ASD files can be opened using the provided scripts. Metadata is provided in two formats: CSV file format (no geolocation) and GEOJSON file format (includes geolocation for each spectra). The dataset includes a set of pre-processed reflectance spectra as CSV files (yyyymmdd_rfl.csv). The python scripts and jupyter notebook used to calculate reflectance spectra from the ASD radiance data is included here and was previously published at: https://doi.org/10.3334/ORNLDAAC/2446. There is also a folder of JPEG photographs corresponding to selected spectra. We include a protocol document with detailed steps for ASD FieldSpec4 assembly and operations. This data additionally contains a file level metadata (flmd.csv) and data dictionary (dd.csv) file. Geospatial information: Geospatial data for mapping measurement site locations are in the files CHESS_polygons_lai_UTM.geojson, CHESS_polygons_shrub_UTM.geojson, and CHESS_polygons_meadow_UTM.geojson in the companion geospatial package for the 2025 CHESS campaign, ‘CHESS 2025: Location data for field observations and sampling’ (Henderson et al., 2026). CHESS Project Description: The Colorado Headwaters Ecological Spectroscopy Study (CHESS) comprised a multi-week airborne remote sensing and field observation campaign in the Upper Gunnison Basin, Colorado, conducted in June and July of 2025. Airborne remote sensing was conducted by the National Ecological Observatory Network Airborne Observation Platform (NEON AOP), concurrent with a field campaign run by the Rocky Mountain Biological Laboratory (RMBL), the Lawrence Berkeley National Laboratory (LBNL) and SLAC National Accelerator Laboratory Watershed Function Science Focus Area (SFA), and NASA-JPL (Jet Propulsion Laboratory) Earth Surface Mineral Dust Source Investigation (EMIT) program. Between June 10 and July 18, 2025, the NEON AOP flight team collected high-resolution aerial imaging spectroscopy and Light Detection and Ranging (LiDAR) data over three domains: the Upper East River (CRBU), Almont Triangle (ALMO), and the Upper Taylor Basin (UPTA). In coordination with the flights, a field campaign acquired ground-truth observations, including observations of vegetation composition, foliar traits, forest demography, and subsurface properties in 18 core sampling areas within the domains. Additional surface water observations were taken at over 380 point locations. All CHESS campaign datasets can be found within the CHESS ESS-DIVE data portal: https://data.ess-dive.lbl.gov/portals/chess. Funding Acknowledgment: This research was carried out at the Jet Propulsion Laboratory, California Institute of Technology, under a contract with the National Aeronautics and Space Administration (80NM0018D0004) and was funded by EMIT Extended Mission Phase E Science.

2018 NEON and 2025 CHESS Campaigns↗
DOE OSTI2022

High manganese redox variability and manganate predominance in temperate soil profiles as determined by X-ray absorption spectroscopy

Manganese speciation is a key to understanding the fate of contaminants, nutrients, and organic matter in soils. To date, quantification of Mn species in bulk soils has been performed mainly by sequential extraction methods and rarely supported by spectroscopic analysis. In order to obtain quantitative information on the Mn species inventory of soils, we investigated 46 soil horizons (<2-mm fraction, 45.1–2,280 mg/kg Mn) of nine typical Central European soils (Cambisols, Chernozems, Luvisols, Podzol, Stagnosol) by chemical Mn analyses and Mn K-edge X-ray absorption spectroscopy, and related speciation results to major soil properties. Amounts of Mn 2+ , Mn 3+ , and Mn 4+ and the average oxidation state of Mn were evaluated by linear combination fitting (LCF) of X-ray absorption near edge structure (XANES) spectra. Additionally, we used extended X-ray absorption fine structure (EXAFS) spectroscopy to identify and quantify major Mn species. For this, EXAFS spectra of 20 organic and mineral soil samples from five soils (Cambisols, Chernozem, Luvisol) were analyzed by LCF and shell fitting. XANES analyses revealed a high Mn redox variability in organic surface layers, with Mn 2+ being most abundant (≤100%, $\overline{x}$ = 54%), followed by Mn 3+ (≤80%, $\overline{x}$ = 32%) and Mn 4+ (≤55%, $\overline{x}$ = 14%). Mineral soil horizons contained significantly less Mn 2+ (≤56%, $\overline{x}$ = 23%), about equal quantities of Mn 3+ (≤68%, $\overline{x}$ = 31%), and were enriched in Mn 4+ (≤89%, $\overline{x}$ = 46%). EXAFS analyses implied the presence of six major Mn species groups: manganates, organically complexed Mn, Mn(III) oxyhydroxides, silicate-bound Mn, Mn oxides without tunnel- or layer structure, and physisorbed Mn. In litter horizons, Mn was mainly present in organic complexes (58–91%, $\overline{x}$ = 78%) and as physisorbed Mn (≤15%), but individual horizons also comprised manganates, Mn(III) oxyhydroxides, and silicate-bound Mn. Manganates, likely mixtures of phyllomanganates with hexagonal layer symmetry and tectomanganates, dominated in all mineral soil horizons (37–94%, $\overline{x}$ = 67%). Correlation analysis showed that manganates dissolve completely during dithionite-citrate and acid ammonium oxalate extractions, and suggested that Mn 4+ -rich manganates preferentially form under less acidic soil conditions, partly by oxidation of organically complexed Mn(II), and that they are enriched in the soil clay fraction. Mineral soil horizons also contained minor quantities of organically complexed Mn (≤39%, $\overline{x}$ = 11%), silicate-bound Mn (≤30%, $\overline{x}$ = 8%), Mn(III) oxyhydroxides (≤37%, $\overline{x}$ = 7%), Mn oxides without tunnel- or layer structure (≤18%, $\overline{x}$ = 5%), and physisorbed Mn (≤14%, $\overline{x}$ <1%). The detection of Mn(III) oxyhydroxides such as feitknechtite (β-MnOOH) or groutite (α-MnOOH) as well as the spinel hausmannite (Mn 3 O 4 ) in acidic soils is remarkable, since their formation is normally linked to neutral or alkaline pH conditions. Minor contributions of silicate-bound Mn indicate the release of Mn from primary minerals already at early stages of soil formation, and low concentrations of physisorbed Mn suggest that exchangeable Mn is rapidly converted into manganates in oxic soils. In conclusion, the predominance of manganates in mineral soils has far-reaching implications for the functioning of soils and biogeochemical element cycles, as these minerals play an important role in metal binding, plant nutrition, and redox-related processes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Capillary absorption spectroscopy for high temporal resolution measurements of stable carbon isotopes in soil and plant-based systems

Capillary Absorption Spectroscopy (CAS) is a relatively new analytical technique for performing stable isotope analysis. Here, we demonstrate the utility of CAS by recording and quantifying variation in 13C in controlled and biologically relevant applications. We calibrated CAS system response to increased 13CO2, with an observed ~4‰ increase in measured Δ13C for each 0.03 ppm shift in 13CO2 concentration. We leveraged this calibration to quantify rates of biogeochemical processes using a 13C tracer. For example, we monitored microbial respiration of 13C-glucose within an agricultural soil at 10 s quantification intervals and results demonstrated 8.6% ± 0.4 of added glucose was converted to 13CO2 within 1.5 h of incubation. We expanded the demonstration by adapting a rhizobox to permit continuous monitoring of 13CO2 in a soil (as distinct from plant) headspace to track the timing and quantify respiration rates of fresh plant photosynthate and observed a 3.5 h delay between plant exposure to a13CO2 tracer and the first signs of respiration by soil biota. These experiments highlight CAS is effective in producing high temporal resolution quantification of 13CO2 and demonstrate potential applications.

13CO2↗
DOE OSTI2026

Effects of 9.5 years warming on SOC concentration and composition in bulk soil and density fractions

Original data of whole-soil warming experiment after 9.5 years at Blodgett Forest Research Station. The Blodgett Forest is a mixed coniferous temperate forest with Mediterranean climate. The annual air temperature is 12.5℃ and the annual precipitation is 1774 mm yr-1- The soil is mesic ultic Alfisol of granitic origin, equivalent to Dystric Cambisol according to The World Reference Base for Soil Resources (WRB) system. The soil is warmed down to 1 m at + 4℃ by vertically installed heating cables. At the time of soil sampling on 1 May 2023, the whole-soil warming experiment had been running for approximately 9.5 years, from January 2014 to May 2023. The dataset includes: - Bulk_EA: C, N content, δ13C, and CN ratio of bulk soil; - Density_fractionation: organic carbon concentration, δ13C, and C/N ratio of free light fraction (fLF), occluded ligh fraction (oLF), and heavy fraction (HF); - PCA_DRIFT_AUC: original data of area under the curve (AUC) values of eight carbon bond types integrated on diffuse reflectance infrared fourier transform spectroscopy for each soil sample and soil fraction, which are consequently used for principal component analysis (PCA); - DRIFTS_stability_index: the calculation of aliphatic C–H (3000–2800 cm-1) to aromatic C=C (1670–1600 cm-1) ratios for each bulk soil sample and soil fraction. All data are provided in CSV format and can be viewed using Microsoft Excel.

Climate change↗
DOE OSTI2023

An interlaboratory comparison of mid-infrared spectra acquisition: Instruments and procedures matter

Diffuse reflectance spectroscopy has been extensively employed to deliver timely and cost-effective predictions of a number of soil properties. However, although several soil spectral laboratories have been established worldwide, the distinct characteristics of instruments and operations still hamper further integration and interoperability across mid-infrared (MIR) soil spectral libraries. In this study, we conducted a large-scale ring trial experiment to understand the lab-to-lab variability of multiple MIR instruments. By developing a systematic evaluation of different mathematical treatments with modeling algorithms, including regular preprocessing and spectral standardization, we quantified and evaluated instruments' dissimilarity and how this impacts internal and shared model performance. We found that all instruments delivered good predictions when calibrated internally using the same instruments' characteristics and standard operating procedures by solely relying on regular spectral preprocessing that accounts for light scattering and multiplicative/additive effects, e.g., using standard normal variate (SNV). When performing model transfer from a large public library (the USDA NSSCKSSL MIR library) to secondary instruments, good performance was also achieved by regular preprocessing (e. g., SNV) if both instruments shared the same manufacturer. However, significant differences between the KSSL MIR library and contrasting ring trial instruments responses were evident and confirmed by a semi-unsupervised spectral clustering. For heavily contrasting setups, spectral standardization was necessary before transferring prediction models. Non-linear model types like Cubist and memory-based learning delivered more precise estimates because they seemed to be less sensitive to spectral variations than global partial least square regression. In summary, the results from this study can assist new laboratories in building spectroscopy capacity utilizing existing MIR spectral libraries and support the recent global efforts to make soil spectroscopy universally accessible with centralized or shared operating procedures.

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