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

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At least 793 records · Page 44
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

High-speed volumetric imaging of formaldehyde in a lifted turbulent jet flame using an acousto-optic deflector

The development of high-speed volumetric laser-induced fluorescence measurements of formaldehyde (CH 2 O-LIF) using a pulse-burst laser operated at a repetition rate of 100 kHz is presented here. A novel laser scanning system employing an acousto-optic deflector (AOD) enables quasi-4D CH 2 O-LIF imaging at a scan frequency of 10 kHz. The diagnostic capability of time-resolved volumetric imaging is demonstrated in a partially premixed DME/air lifted turbulent jet flame near the flame base. Simultaneous imaging of laser beam profiles is performed to account for the laser pulse energy fluctuation and laser sheet inhomogeneity. With the accurate registration of laser sheet positions, the volumetric reconstruction of CH 2 O-LIF signals is performed within a detection volume of 17.3 × 11.9 × 2.3 mm 3 with an average out-of-plane spatial resolution of 250μm. A surface detection algorithm with adaptive thresholding is used to determine the global maximum intensity gradient by calculating gradient percentiles. The flame topology characteristics are investigated by evaluating the 3D curvatures of CH 2 O surfaces. Curvatures calculated using 2D data systematically underestimate the full 3D curvature due to the lack of out-of-plane information. The inner surfaces near the turbulent fuel jet exhibit higher probabilities of large mean curvature than the outer surfaces. The saddle and cylindrical structures are dominant on both the inner and outer surfaces and the elliptic structures occur with lower probability. The results suggest that the damping of turbulent fluctuations by the temperature increase through the CH 2 O region reduces the curvature, but the local structure topology remains self-similar.

42 ENGINEERING↗
DOE OSTI2024

Predictability of the early summer surface air temperature over Western South Asia

Variability of the Surface Air Temperature (SAT) over the Western South Asia (WSA) region leads to frequent heatwaves during the early summer (May-June) season. The present study uses the European Centre for Medium-Range Weather Forecast’s fifth-generation seasonal prediction system, SEAS5, from 1981 to 2022 based on April initial conditions (1-month lead) to assess the SAT predictability during early summer season. The goal is to evaluate the SEAS5’s ability to predict the El Niño-Southern Oscillation (ENSO) related interannual variability and predictability of the SAT over WSA, which is mediated through upper-level (200-hPa) geopotential height anomalies. This teleconnection leads to anomalously warm surface conditions over the region during the negative ENSO phase, as observed in the reanalysis and SEAS5. We evaluate SEAS5 prediction skill against two observations and three reanalyses datasets. The SEAS5 SAT prediction skill is higher with high spatial resolution observations and reanalysis datasets compared to the ones with low-resolution. Overall, SEAS5 shows reasonable skill in predicting SAT and its variability over the WSA region. Moreover, the predictability of SAT during La Niña is comparable to El Niño years over the WSA region.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Viscoelastic-Mapping of Cellulose Nanofibrils Using Low-Total-Force Contact Resonance Force Microscopy (LTF-CRFM)

Low-total-force contact resonance force microscopy (LTF-CRFM), an atomic force microscopy method, is introduced as a non-destructive means to quantify the local viscoelastic loss tangent (tan..delta..) of supported cellulose nanofibrils (CNFs). The method limits static and dynamic forces during measurement to minimize substrate and geometry effects and to reduce the potential for stress-induced CNF damage. LTF-CRFM uses Brownian motion to achieve the thermally-limited lowest dynamic force, while approaching adhesive pull-off to achieve the low static force. LTF-CRFM measurements were shown to generate analyzable data without evidence of nonlinear artifacts and without damage to the CNF over static forces ranging from 11.6 to 84.6 nN. The measured tan..delta.. of CNFs was 0.015 +/- 0.0094, which is the first reported tan..delta.. measurement of an isolated CNF. Finally, LTF-CRFM successfully mapped tan..delta.. along the length of CNFs to determine that kink defects along the CNF do not impart a local viscoelastic property change at the spatial resolution of the measurement.

BIOMASS FUELS↗
DOE OSTI2022

A Square Pulse Thermoreflectance Technique for the Measurement of Thermal Properties

We report on a laser-based square pulse thermoreflectance (SPTR) technique for the measurement of thermal properties for a wide range of materials. SPTR adopts the pump-probe thermoreflectance principle to monitor the evolution of local temperature after square pulse excitation. The technique features a compact setup, high spatial resolution, and fast data collection. By comparing the acquired SPTR signals with a continuum heat transfer model, material thermal properties can be obtained. Taking advantage of various spot sizes and modulation frequencies, SPTR can measure both the thermal diffusivity and thermal conductivity of poorly to moderately conductive materials and the thermal conductivity of conductive materials with satisfactory accuracy, with potential to be applied to more conductive materials. The technique was validated on three materials: fused silica, single crystal CaF2 and single crystal nickel (with conductivities ranging from 1 W·m -1 ·K -1 to 100 W·m -1 ·K -1 ) with typical measurement errors of 5 % to 20 %. The leading sources of error have been identified by Monte Carlo simulations, and the primary limitations of SPTR are discussed. The compact, fiberized platform we describe here will allow instruments based on this methodology to be deployed in complex, multi-analytical environments for the type of high-throughput correlative analyses that are key to materials design and discovery.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2025

Light output and neutron detection efficiency of boron-based neutron scintillator screens for neutron imaging

Recent research has explored the development of boron-based neutron scintillator screens, which potentially offer improved spatial resolution and neutron capture efficiency compared to traditional lithium-based screens. This work builds upon previous efforts to improve boron-based neutron scintillators by assessing a newer generation of boron-based scintillator screens fabricated using different compositions and fabrication approaches compared to previous generations of screens. Some of the test screens exhibit higher light output than previous efforts and higher neutron capture efficiency than lithium-based screens. This paper describes the current state of screen development, measurement results for the most recent generation of screens, and future activities.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗
DOE OSTI2025

SUDA: A SUrface Dust Analyser for Compositional Mapping of the Galilean Moon Europa

Abstract The Surface Dust Analyser (SUDA) is a mass spectrometer onboard the Europa Clipper mission for investigating the surface composition of the Galilean moon Europa. Atmosphereless planetary moons such as the Galilean satellites are wrapped into a ballistic dust exosphere populated by tiny samples from the moon’s surface produced by impacts of fast micrometeoroids. SUDA will measure the composition of such surface ejecta during close flybys of Europa to obtain key chemical signatures for revealing the satellite’s composition such as organic molecules and salts, history, and geological evolution. Because of their ballistic orbits, detected ejecta can be traced back to the surface with a spatial resolution roughly equal to the instantaneous altitude of the spacecraft. SUDA is a Time-Of-Flight (TOF), reflectron-type impact mass spectrometer, optimized for a high mass resolution which only weakly depends on the impact location. The instrument will measure the mass, speed, charge, elemental, molecular, and isotopic composition of impacting grains. The instrument’s small size of$268 ~\mathrm {mm} \times 250 ~\mathrm {mm} \times 171$ 268 mm × 250 mm × 171 $~\mathrm {mm}$ mm , radiation-hard design, and rather large sensitive area of 220 cm 2 matches well the challenging demands of the Clipper mission.

Astronomy & Astrophysics↗
DOE OSTI2022

Fully Integrated Ultra-thin Intraoperative Micro-imager for Cancer Detection Using Upconverting Nanoparticles

Abstract Purpose Intraoperative detection and removal of microscopic residual disease (MRD) remain critical to the outcome of cancer surgeries. Today’s minimally invasive surgical procedures require miniaturization and surgical integration of highly sensitive imagers to seamlessly integrate into the modern clinical workflow. However, current intraoperative imagers remain cumbersome and still heavily dependent on large lenses and rigid filters, precluding further miniaturization and integration into surgical tools. Procedures We have successfully engineered a chip-scale intraoperative micro-imager array—without optical filters or lenses—integrated with lanthanide-based alloyed upconverting nanoparticles (aUCNPs) to achieve tissue imaging using a single micro-chip. This imaging platform is able to leverage the unique optical properties of aUCNPs (long luminescent lifetime, high-efficiency upconversion, no photobleaching) by utilizing a time-resolved imaging method to acquire images using a 36-by-80-pixel, 2.3 mm $$\times$$ × 4.8 mm silicon-based electronic imager micro-chip, that is, less than 100-µm thin. Each pixel incorporates a novel architecture enabling automated background measurement and cancellation. We have validated the performance, spatial resolution, and the background cancellation scheme of the imaging platform, using resolution test targets and mouse prostate tumor sample intratumorally injected with aUCNPs. To demonstrate the ability to image MRD, or tumor margins, we evaluated the imaging platform in visualizing a single-cell thin section of the injected prostate tumor sample. Results Tested on USAF resolution targets, the imager is able to achieve a resolution of 71 µm. We have also demonstrated successful background cancellation, achieving a signal-to-background ratio of 8 when performing ex vivo imaging on aUCNP-injected prostate tumor sample, improved from originally 0.4. The performance of the imaging platform on single-cell layer sections was also evaluated and the sensor achieved a signal-to-background ratio of 4.3 in resolving cell clusters with sizes as low as 200 cells. Conclusion The imaging system proposed here is a scalable chip-scale ultra-thin alternative for bulky conventional intraoperative imagers. Its novel pixel architecture and background correction scheme enable visualization of microscopic-scale residual disease while remaining completely free of lenses and filters, achieving an ultra-miniaturized form factor—critical for intraoperative settings.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

A New Residual Strain Mapping Program Using Energy Dispersive X-Ray Diffraction at the Advanced Photon Source

Here, the ability to non-destructively map the residual strain field inside an engineering component is important for predicting its fatigue life or developing processing methods to prevent failure or enhance performance. In this paper, we describe a new residual strain mapping program at the Advanced Photon Source, Argonne National Laboratory. The new program is based on energy dispersive x-ray diffraction (EDXRD). It is capable of non-destructively penetrating a several- cm thick polycrystalline sample fabricated from engineering alloys using high-energy x-rays and measuring the residual strain field with mm or better spatial resolution and approximately ±1 x 10 -4 strain resolution. A multi-element detector array is employed to measure multiple strain components simultaneously. The residual strain mapping setup is augmented with a high-energy tomography capability, allowing precise alignment of the material volume of interest for residual strain mapping and providing a complementary view of the structure to understand the measured strain field. These measurement capabilities are demonstrated using several strain mapping examples ranging from polycrystalline structural alloys to biological materials. We also provide some guidance for the future users of the program for a successful residual strain mapping experiment. We are expanding the capabilities of the new setup with various in situ capabilities including thermo-mechanical loading.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2025

Eddy covariance towers as sentinels of abnormal radioactive material releases

Ensuring accurate detection and attribution of abnormal releases of radioactive material is critical for protecting human health and safety. Most commonly, such detection is accomplished via active monitoring approaches involving the collection of physical samples. Further, this is labor intensive and limits the temporal and spatial resolution of any detected events to a relatively coarse level. As an alternative first step towards passive monitoring, we developed an approach using eddy flux tower data records to identify signals from a known abnormal release and quantify the extent to which that signal also occurs at other times in the data record. Through two case studies, one of which targeted the Fukushima nuclear disaster and the other targeting an abnormal release event at a radioisotope production facility in Fleurus, Belgium, we tested our approach and identified several potential heretofore unidentified abnormal events that were consistent with atmospheric circulation patterns and/or wind direction from known release sites. Because our approach is relatively simple and is resistant to systematic errors in the observational record, it has broad applicability beyond specific constituents and ecosystem types to identify a wide variety of limited-duration anomalies in flux tower data to ensure human health and industrial safety.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2020

Microscale Observation via High-Speed X-ray Diffraction of Alloy 718 During In Situ Laser Melting

The laser melting process is accompanied by rapid evolution in temperature, phase, structure, and strain because of its high heating and cooling rates. In this study, the evolution of grains within a thin solid plate of Ni alloy 718 during laser processing was probed with in situ high-energy x-ray diffraction experiments. The high temporal and spatial resolution available in the measurement allowed us to study the rapid evolution of the melted region beneath the surface of the sample. The characterization of the evolution of secondary phases, i.e., Laves and carbide, was captured despite the weak diffracted peaks caused by small volume fractions. Thermal history was estimated based on changes in the lattice spacing from the thermal contraction upon cooling. In conclusion, the temporal variation in 2θ with azimuthal direction revealed the evolution in anisotropy of lattice spacing and thus of the mechanical state during laser processing.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Revealing the effect of local stresses on twin growth mechanisms in titanium using synchrotron X-ray diffraction

Deformation twinning has a significant impact on the evolution of microstructure and mechanical response in hexagonal close packed (hcp) metals. Understanding the physical mechanisms associated with twin nucleation and growth processes is important to enable the broad use of hcp metals. While both nucleation and growth are conditioned by the local stress state, few studies have quantified it in bulk deformed samples. In this study, we reveal the effects of local stresses on twin thickening using in-situ synchrotron experiments with differential aperture X-ray microscopy. High purity Ti is deformed under four-point bending to activate {1012} tensile twins. Further, 3D stress fields with a spatial resolution of 0.5μm are mapped in the vicinity of low and high macroscopic Schmid factor (MSF) twins growing inside a grain. Reconciling this experimental analysis with recent twin growth models reveals that the growth of low MSF twins is limited by the nucleation of twin growth defects in the high-purity Ti sample. While growth-inducing defect nucleation may occur in many places on the interface of the high resolved shear stress (RSS)/MSF twin, the nucleation rate of twinning disconnections for the low MSF twin is high only at the end of the twin near a stress concentration. Once nucleated, these defects easily propagate into lower RSS regions of the grain resulting in twin growth. This work highlights the importance of stress concentrations not only for twin (embryo) nucleation, but also to the growth process of twins, particularly in low MSF twins.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Emergence of complex-regular eutectic patterns in Al–Ge: Observations from correlative nano-imaging

Eutectic solidification exemplifies nonequilibrium pattern formation, making it a well-studied moving boundary problem. Yet the mechanisms behind the formation of complex-regular microstructures – particularly in highly anisotropic systems with a significant volume fraction of a faceted phase – remain poorly understood. Our understanding of such systems is made complicated by the nonlinear interface kinetics and unique growth dynamics characteristic of faceted phases. To address these challenges, we investigate a model Al–Ge eutectic system, where the faceted Ge phase constitutes a substantial volume fraction (~0.35) and where the two solid phases arrange into so-called “fishbone” or “feather” complex-regular patterns. Using synchrotron-based x-ray nano-imaging and nanotomography with high spatial resolution (22 nm per pixel), we capture in real-time the evolution of the solid–liquid interfaces and the resulting three-dimensional microstructures in this faceted/non-faceted eutectic system. By integrating these observations with electron backscattered diffraction, we elucidate the crystallographic biases on the solidification process and the mechanisms driving the formation of such complex-regular microstructures. These findings inform a new growth model for irregular eutectics in (near-)symmetrical phase diagrams, offering insight on advanced microstructural design and processing strategies. More broadly, we demonstrate how interfacial curvature is generated in irregular eutectic alloys and how it depends on the volume fraction of the faceted phase.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Testing of fiber optic based sensors for advanced reactors in the Texas A&M University TRIGA reactor

An Optical Fiber Based Gamma Thermometer has been developed and tested at the Texas A&M University reactor as well as the Ohio State Research Reactor. This sensor technology provides temperature measurement of a thermal mass undergoing gamma heating, from which the gamma flux along the length of the sensor may be calculated. The gamma flux data from an array of OFBGTs could allow the determination of local power density within a nuclear reactor core in three dimensions. The design of the sensor makes use of optical fiber as a truly distributed temperature sensor with a spatial resolution less than 1mm and temperature accuracy of ±1°C. The testing program showed that the system provided the expected temperature data for each location. Overall, this sensor technology shows promise for current Light Water Reactors as well as advanced nuclear reactors by providing an unparalleled level of precision in reactor power measurement.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2024

Development of a Griffin model of the advanced test reactor

In the pursuit of a higher fidelity deterministic simulation capability of the Advanced Test Reactor, it is important to have a fast yet accurate deterministic neutronics model. Here, to achieve this, we employed an advanced two-step method. The first step involves generating homogenized cross sections using OpenMC, a cutting-edge Monte Carlo neutron transport code. OpenMC offers excellent modular capabilities, allowing for easy component integration and flexibility in incorporating new designs into the model. The second step involves deterministic transport calculations, which are performed using Griffin, a reactor physics application based on the Multiphysics Object-Oriented Simulation Environment (MOOSE). To ensure the accurate spatial resolution and assignment of material cross sections, a Cubit-generated mesh for the Advanced Test Reactor is utilized as an intermediate step between the OpenMC and Griffin models; Griffin utilizes the mesh for its finite element solution, while OpenMC material identifications are written to the mesh file to be used in Griffin material assignments. Additionally, a Python-based script converts the cross sections generated by OpenMC into the ISOXML format required by Griffin. Initial comparisons using the Griffin diffusion solver indicated good agreement between the neutron multiplication factors obtained from the standalone OpenMC model and the Griffin model, with differences of less than 10 pcm in the 2D geometry configuration; it was later determined that this agreement was likely due to compensating effect and was more likely on the order of –700 pcm relative to the OpenMC solution. However, in three-dimensional calculations, an unacceptably large error (almost 8,000 pcm) was found in the Griffin solution with the diffusion solver. Subsequent calculations using Griffin’s discrete ordinates solver demonstrated substantially improved agreement, within 116 pcm of the OpenMC solution used to generate the cross sections for Griffin. Building on this capability, future work will seek to perform more detailed validation calculations. The ultimate goal is to evaluate both transient and multiphysics simulations of the reactor.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2020

Dynamic hosting capacity analysis for distributed photovoltaic resources—Framework and case study

Distributed photovoltaic systems can cause adverse distribution system impacts, including voltage violations at customer locations and thermal overload of lines, transformers, and other equipment resulting from high current. The installed capacity at which violations first occur and above which would require system upgrades is called the hosting capacity. Current static methods for determining hosting capacity tend to either consider infrequent worst-case snapshots in time and/or capture coarse time and spatial resolution. Because the duration of violations cannot be captured with these traditional methods, the metric thresholds used in these studies conservatively use the strictest constraints given in operating standards, even though both worse voltage performance and higher overloads may be temporarily acceptable. However, assessing the full details requires accurately capturing time-dependence, voltage-regulating equipment operations, and performance of advanced controls-based mitigation techniques. In this paper, we propose a dynamic distributed photovoltaic hosting capacity methodology to address these issues by conducting power flow analysis for a full year. A key contribution is the formulation of time aware metrics to take these annual results and identify the hosting capacity. Through a case study, we show that this approach can more fully capture grid impacts of distributed photovoltaic than traditional methods and the dynamic hosting capacity was 60%–200% higher than the static hosting capacity in this case study.

14 SOLAR ENERGY↗
DOE OSTI2022

Effect of modeled time horizon on quantifying the need for long-duration storage

Long-Duration Energy Storage (LDES) has gained interest due to its key role in attaining a decarbonized, low-cost, and stable grid driven by variable renewable electricity (VRE). Currently, there is a wide range of LDES technologies being developed to provide electricity with 8+ hours of consecutive discharge. However, current capacity expansion models used in long-term planning processes rarely consider low cost LDES as a candidate technology. If they do, the storage balancing horizon (SBH) of the model usually only considers non-consecutive 1-day periods that do not capture the potential of LDES to shift energy across multiple days or even seasons. Addressing these limitations in existing models, this work explores the ways in which the optimal energy storage changes when increasing the number of consecutive days in the SBH and how these changes will impact planners who are determining the future roles of energy storage. Our analysis uses SWITCH, an open-source capacity expansion model with a high spatial resolution for the entire Western Electricity Coordinating Council (WECC) in a zero-carbon scenario in 2050. We find that the number of consecutive days in the SBH changes both the total selected power and energy capacity of LDES when storage energy and power capacity overnight costs are $\$$13 USD/kWh (or less) and $113 USD/kW, respectively. We also find that the amount of required energy in storage to drive a future VRE-driven WECC grid ranges from 2.5 TWh to 16.0 TWh depending on the length of the SBH. The optimal storage duration (energy to power ratio) we obtain ranges from 10 h to 620 h among all the scenarios. Furthermore, depending on the storage cost assumption, we observe different charge/discharge patterns when varying the length of the SBH. Given our results, we anticipate that as more LDES technologies become commercially available, it will be critical to increase the length of the SBH to fully capture the benefits of LDES assets in long-term planning processes of high VRE-driven grids.

42 ENGINEERING↗
DOE OSTI2024

Modeling the impact of extreme summer drought on conventional and renewable generation capacity: Methods and a case study on the Eastern U.S. power system

Across recent years, there has been a growing prevalence of extreme weather events throughout the United States, posing significant challenges to the reliable and resilient operation of power systems. Specifically, summer droughts threaten to severely reduce available generation capacity to meet regional electricity demand, potentially leading to power outages. This underscores the importance of accurate resource adequacy (RA) assessment to ensure the reliable operation of the nation’s energy infrastructure. Accurately evaluating the usable capacity of regional generation fleets is a challenging undertaking due to the intricate interactions between power systems and hydro-climatic systems. Here, this paper proposes a systematic and analytical framework to evaluate the impacts of extreme summer drought events on the available capacity of various generating technologies, incorporating both meteorological and hydrologic factors. The framework provides detailed plant-level capacity derating models for hydroelectric, thermoelectric, and renewable power plants, facilitating evaluations with high temporal and spatial resolution. The application of the proposed impact assessment framework to the 2025 generation fleet of the real-world power system within the PJM and SERC regions of the United States yields insightful results. By analyzing the daily usable capacity of 6,055 at-risk generators across the study region, it shows that the summer capacity deration is most significant for hydroelectric and once-through thermal power plants, followed by recirculating thermal power plants and combustion turbines. In the event of the recurrence of the 2007 southeastern summer drought event in the near future, the generation fleet could experience a substantial reduction in available capacity, estimated at approximately 8.5 GW, compared to typical summer conditions. The sensitivity analysis reveals that the usable capacity of the generation fleet would suffer an even more significant decrease under conditions of increasingly severe summer droughts. The proposed approach and the findings of this study provide valuable methodologies and insights, empowering stakeholders to bolster the resilience of power systems against the potentially devastating effects of future extreme drought events.

24 POWER TRANSMISSION AND DISTRIBUTION↗
DOE OSTI2024

Fe Kα XANES, Fe Kβ HERFD XANES and EPMA flank method determinations of the oxidation state of Fe in garnet

The ferric to total iron ratios (Fe 3+ /ΣFe) of garnets can be paired with thermodynamic mineral activity models to quantify the oxygen fugacity of garnet-bearing rocks. However, techniques with a high analytical and spatial resolution are necessary to distinguish differences in garnet Fe 3+ /ΣFe ratios at the percent level and to accurately measure garnets that are zoned or contain inclusions. We acquired conventional Fe Kα and high-resolution energy fluorescence detection (HERFD) Fe Kβ X-ray absorption near edge structure (XANES) spectra and electron microprobe flank method analyses on a suite of 27 peridotitic and eclogitic garnets with Fe 3+ /ΣFe ratios previously determined by Mössbauer spectroscopy to evaluate the precision of each technique. We examined variations in the energy and intensity of three XANES spectral features as a function of Fe 3+ /ΣFe ratios: 1) the intensity ratio of two-post edge features (I-ratio; Fe Kα only); 2) the energy of the Fe edge at 90% normalized intensity (E 0.9 ; Fe Kα only) and 3) the pre-edge centroid energy (Fe Kα and HERFD Fe Kβ). In accordance with previous work, we find the energies of garnet pre-edge centroids are relatively insensitive to Fe 3+ /ΣFe ratios. The I-ratios of peridotitic and eclogitic garnets are offset from each other at low Fe 3+ /ΣFe ratios (≤0.13); I-ratio garnet XANES calibrations are composition-specific. The E 0.9 feature is independent of garnet major element composition in spectra that have been corrected for the effects of self-absorption. We produce two Fe Kα garnet XANES calibrations based on variations in the E0.9 feature; one calibration with all garnet reference materials included (Fe 3+ /ΣFe up to 1.0; “all garnet calibration”) and another calibration specific to garnets with low Fe 3+ /ΣFe ratios (“low ferric calibration”). Fe 3+ /ΣFe ratios calculated from the mean of up to 25 flank method measurements on eight garnet reference materials fall within 4% absolute of a one-to-one correlation with Fe 3+ /ΣFe ratios measured by Mössbauer. The standard error of the mean Fe 3+ /ΣFe ratio calculated from flank method approaches the Mössbauer-determined Fe 3+ /ΣFe ratio within estimated error (3%) after three analyses. Flank method precision is enhanced at higher beam current; however, the precision of the flank method does not approach the precision of XANES under any microprobe analytical condition tested here. Garnet reference materials detailed here are available by request to the Smithsonian Institution.

58 GEOSCIENCES↗