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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
NASA NTRS1993

Measuring and distinguishing compositional and maturity properties of lunar soils by remote VIS-NIR spectroscopy

Space weathering on the lunar surface affects the spectra/optical character of an exposed lunar soil in three ways: the reflectance is reduced, absorption band depths are reduced, and a red-sloped continuum is created and increased with exposure. As a result, the spectrum of a lunar soil is dependent upon both the degree of exposure at the lunar surface and the original composition. It is critical to the remote analysis of lunar soils to differentiate between the optical effects of maturity and the effects of composition. In the laboratory, it is possible to determine and consequently distinguish the degree of exposure, or soil maturity, as measured by parameters such as I(sub s)/FeO (e.g., 1; mature defined as I(sub s)/FeO greater than or equal to 60), and the composition, as measured by various chemical and petrographical techniques. Lunar soils returned by the Apollo missions provide important ground truth for developing methods for remotely measuring the maturity and the concentration of Fe-bearing minerals in lunar soil. The ground truth spectral data analyzed are from the John Adams lunar soil spectra collection. Soils collected from or near highland terrains are emphasized in the discussion. The mineralogical makeup of mare soils results in behavior somewhat different from highland soils.

Fischer, Erich M.↗
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↗
NASA NTRS2009

Effect of Space Radiation Processing on Lunar Soil Surface Chemistry: X-Ray Photoelectron Spectroscopy Studies

Current understanding of the chemistry and microstructure of the surfaces of lunar soil grains is dominated by a reference frame derived mainly from electron microscopy observations [e.g. 1,2]. These studies have shown that the outermost 10-100 nm of grain surfaces in mature lunar soil finest fractions have been modified by the combined effects of solar wind exposure, surface deposition of vapors and accretion of impact melt products [1,2]. These processes produce surface-correlated nanophase Feo, host grain amorphization, formation of surface patinas and other complex changes [1,2]. What is less well understood is how these changes are reflected directly at the surface, defined as the outermost 1-5 atomic monolayers, a region not easily chemically characterized by TEM. We are currently employing X-ray Photoelectron Spectroscopy (XPS) to study the surface chemistry of lunar soil samples that have been previously studied by TEM. This work includes modification of the grain surfaces by in situ irradiation with ions at solar wind energies to better understand how irradiated surfaces in lunar grains change their chemistry once exposed to ambient conditions on earth.

Dukes, C.↗
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↗
NASA NTRS1997

Raman Spectroscopy for Mineral Identification and Quantification for in situ Planetary Surface Analysis: A Point Count Method

Quantification of mineral proportions in rocks and soils by Raman spectroscopy on a planetary surface is best done by taking many narrow-beam spectra from different locations on the rock or soil, with each spectrum yielding peaks from only one or two minerals. The proportion of each mineral in the rock or soil can then be determined from the fraction of the spectra that contain its peaks, in analogy with the standard petrographic technique of point counting. The method can also be used for nondestructive laboratory characterization of rock samples. Although Raman peaks for different minerals seldom overlap each other, it is impractical to obtain proportions of constituent minerals by Raman spectroscopy through analysis of peak intensities in a spectrum obtained by broad-beam sensing of a representative area of the target material. That is because the Raman signal strength produced by a mineral in a rock or soil is not related in a simple way through the Raman scattering cross section of that mineral to its proportion in the rock, and the signal-to-noise ratio of a Raman spectrum is poor when a sample is stimulated by a low-power laser beam of broad diameter. Results obtained by the Raman point-count method are demonstrated for a lunar thin section (14161,7062) and a rock fragment (15273,7039). Major minerals (plagioclase and pyroxene), minor minerals (cristobalite and K-feldspar), and accessory minerals (whitlockite, apatite, and baddeleyite) were easily identified. Identification of the rock types, KREEP basalt or melt rock, from the 100-location spectra was straightforward.

Haskin, Larry A.↗
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.

58 GEOSCIENCES↗
DOE OSTI2021

Potassium isotopic fractionation in a humid and an arid soil–plant system in Hawai‘i

Plants play a critical role in the cycling of potassium (K) and the fractionation of its isotopes. However, little is known about K stable isotopic compositions in natural soil–plant systems and possible fractionation during intra-plant transport and root-soil uptake of K. Herein this study focuses on K isotopic fractionation within a humid and an arid soil–plant system sampled on the windward and leeward sides of Kohala Mountain, Hawai‘i. We determined the K isotopic compositions of < 2-mm bulk soil, soil saturation extraction, and selected plant tissues by multi-collector inductively coupled plasma mass spectrometry and X-ray absorption spectroscopy. We studied soils and individual tissue samples such as roots, stems, barks, shoots (a sum of stems and fresh leaves), leaves (fresh and dead), seeds, and flowers of trees and grasses. The results demonstrated that: (i) tissue δ 41 K values ranged from –1.06 ± 0.06 to 1.15 ± 0.09‰; (ii) within the same plant, stems (barks), dead leaves, and reproductive tissues (flowers and seeds) were isotopically lighter compared to fresh leaves, and to a lesser extent, roots; (iii) δ 41 K values of the humid soil (-0.54 ± 0.07 to –0.49 ± 0.06‰) were lower than those of the arid soil (-0.24 ± 0.07 to –0.14 ± 0.06‰); and (iv) soil bioavailable pool δ 41 K (saturation extracts) ranged from –0.63 ± 0.08 to 0.34 ± 0.08‰ and 0.48 ± 0.08 to 0.54 ± 0.10‰ in the humid and arid soils, respectively. From synchrotron-based analysis of K atoms, we identified two major K-bearing phases co-existing as ionic K + and K-pectate association of different fractions. Based on K isotopic and synchrotron data, we conclude that two dominant processes are responsible for plant-mediated K isotopic fractionation, including (1) K redistribution during intra-plant circulation and (2) uptake at the root-soil interface. For intra-plant circulation of K, there is a high affinity of isotopically lighter K to organic complexes as K-pectate, and K-pectate is particularly enriched in roots and fresh leaves. For K uptake at root-soil interface, isotopically lighter K is preferentially taken by roots from soil bioavailable pools following a low-affinity (passive) transport path. Soil K budget in two sites reflects strong source mixing effects with limited plant imprints. This work provides exploratory data on the biogeochemical fractionation of K isotopes in the soil–plant system.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS1991

Spectroscopy and reactivity of mineral analogs of the Martian soil

To answer the question of why life occurred on Earth but not on Mars requires a study of the geochemical and physical aspects of the Martian soil. Some of the best Mars analog mineral models of the soil have been prepared and justified according to known constraints of chemical composition, reflectance spectroscopy, and chemical reactivity. Detailed laboratory reflectance spectra in the ultraviolet, visible, and near infrared (.30 to 2.5 microns) and the infrared (2.5 to 25 microns) regions have been obtained for the pure candidate minerals and some analog mixtures and compared to Mars reflectance spectra. Modeling of the reflectance spectra from optical constraints determined for the analog minerals has begun and will be interpreted in terms of the effects of particle size variation, component mixing, and soil packing upon remotely sensed reflectance spectra. This has implications not only for Mars, but for other planets and planetoids. The ratio of Fe(II)/Fe(III) in the Martian soil analog materials on spectral reflectance in the visible range has begun, and the results will be evaluated according to conformity with the visible Mars reflectance spectrum. Some initial LR and GEX data have been collected for the mineral samples and their mixtures, which can be compared with the Viking data and interpreted in terms of the redox (Fe(II)/Fe(III) environment.

Banin, A.↗
NASA NTRS1993

Reflectance and Mossbauer spectroscopy of ferrihydrite-montmorillonite assemblages as Mars soil analog materials

Spectroscopic analyses show that Fe(3+)-doped smectites prepared in the laboratory exhibit important similarities to the soils on Mars. Ferrihydrite has been identified as the interlayer ferric component in Fe(3+)-doped smectites by a low quadrupole splitting and magnetic field strength of approximately 48 tesla in Mossbauer spectra measured at 4.2 K, as well as a crystal field transition at 0.92 micrometer. Ferrihydrite in these smectites explains features in the visible-near infrared region that resemble the energies and band strengths of features in reflectance spectra observed for several bright regions on Mars. Clay silicates have met resistance in the past as Mars soil analogs because terrestrial clay silicates exhibit prominent hydrous spectral features at 1.4, 1.9, and 2.2 micrometers; and these are observed weakly, if at all, in reflectance spectra of Mars. However, several mechanisms can weaken or compress these features, including desiccation under low-humidity conditions. The hydration properties of the interlayer cations also effect band strengths, such that a ferrihydrite-bearing smectite in the Martian environment would exhibit a 1.9 micrometers H2O absorption that is even weaker than the 2.2 micrometers structural OH absorption. Mixing experiments demonstrate that infrared spectral features of clays can be significantly suppressed and that the reflectance can be significantly darkened by mixing with only a few percent of a strongly absorbing opaque material. Therefore, the absolute reflectance of a soil on Mars may be disproportionately sensitive to a minor component. For this reason, the shape and position of spectral features and the chemical composition of potential analogs are of utmost importance in assessing the composition of the soil on Mars. Given the remarkable similarity between visible-infrared reflectance spectra of soils in bright regions on Mars and Fe(3+)-doped montmorillonites, coupled with recent observations of smectites in SNC meteorites and a weak 2.2 micrometers absorption in some Mars soils, ferrihydrite-bearing smectites warrant serious consideration as a Mars soil analog.

NASA Discipline Exobiology↗
NASA NTRS1978

Research on lunar materials

Abstracts of 14 research reports relating to investigations of lunar samples are presented. The principal topics covered include: (1) optical properties of surface and core samples; (2) chemical composition of the surface layers of lunar grains: Auger electron spectroscopy of lunar soil and ground rock samples; (3) high frequency electrical properties of lunar soil and rock samples and their relevance for the interpretation of lunar radar observations; (4) the electrostatic dust transport process; (5) secondary electron emission characteristics of lunar soil samples and their relevance to the dust transportation process; (6) grain size distribution in surface soil and core samples; and (7) the optical and chemical effects of simulated solar wind (2keV proton and a particle radiation) on lunar material.

Gold, T.↗
NASA NTRS2009

Micro Electron MicroProbe and Sample Analyzer

A proposed, low-power, backpack-sized instrument, denoted the micro electron microprobe and sample analyzer (MEMSA), would serve as a means of rapidly performing high-resolution microscopy and energy-dispersive x-ray spectroscopy (EDX) of soil, dust, and rock particles in the field. The MEMSA would be similar to an environmental scanning electron microscope (ESEM) but would be much smaller and designed specifically for field use in studying effects of geological alteration at the micrometer scale. Like an ESEM, the MEMSA could be used to examine uncoated, electrically nonconductive specimens. In addition to the difference in size, other significant differences between the MEMSA and an ESEM lie in the mode of scanning and the nature of the electron source.

Manohara, Harish↗