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At least 253 records · Page 14

Evaluation of Detritiation Strategies for Mitigating Tritium Releases

Tritium confinement is performed using different barriers to minimize releases to the environment. Primary confinement is usually performed by process piping and components, secondary confinement typically by inerted gloveboxes connected to a continuously operating tritium stripper system. Some facility designs employ tertiary tritium confinement by using process room confinement with a tritium stripper system activated after an accident to further mitigate tritium releases to the environment. Secondary confinement of some tritium systems such as radiation-hardened or shielded-cell enclosures are not easily achieved using designs for inerted glovebox. These enclosures can be challenging to seal for secondary tritium confinement due to heating, ventilation, and air conditioning (HVAC) needs for temperature control, as well as feedthroughs for equipment and instrumentation, are potential pathways for tritium leaks or loses. Additional tritium leak paths can be created in secondary confinement enclosures due to a Design Basis Accident (DBA) seismic event. These new, larger tritium leak rates from the DBA event are usually not part of the stripper system design basis so all tritium released to the secondary confinement enclosure is assumed released to the environment. Detritiation strategies for shielded enclosures and/or gloveboxes with significant leak rates are necessary to minimize off-site radiological dose consequences. To address this, the relationship between the confinement system leak rate and stripper system (recirculating) flow rate was evaluated to meet prescribed maximum allowable environmental tritium emissions from the event. The simple analysis described assumes a constant leak rate from the confinement system (i.e. shielded enclosure or glovebox) while a recirculating stripper system strips tritium from the system– a competition between tritium release and tritium recovery. At a high level, the resulting expression summarizes the relationship between system leak rate (F L ) and stripper flow rate (F S ) relative to allowable tritium release (Q A ) and initial tritium release (Q 0 ): $\frac{F_L}{F_s}$ ≈ $\frac{Q_A}{Q_0}$. This report derives the relationship between these parameters, examines the impact of finite stripping times followed by purging of the stripped volume. The analysis provides example results for up to 30 gram tritium releases: the maximum tritium inventory of a Hazard Category III (Department of Energy) Nuclear Facility. The detritiation model presented represents a high-level analysis of tritium recovery versus losses for “leaky” confinement enclosures such as shielded cells after large tritium releases. Key parameters for doing the analyses are the system leak rate, stripper flow rate, initial tritium release, and allowable tritium release values. The analyses show a proportional decrease in releases with reduction in initial tritium release but a non-linear increase in tritium recovery with increased stripper flow rate or reduced leak-rate. The analyses also apply to glovebox confinement systems which could have significant increases in leak rates after a DBA. The analysis recognizes but does not include tritium absorption followed by re-emission from the walls of the confinement volume – an analysis which could be pursued in future studies.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

CryoTARPOS Vibration Mitigation System for Layered Experiments

The goal of this project is to implement a system that can eliminate or mitigate vibration so that clear images can be taken without bypassing the cryocooler. By allowing for layer characterization and cryocooler operation at the same time, cooling capacity and thermal stability of the target would be improved, and more layer characterization data could be taken. Increased cooling capacity and thermal stability could allow for layering during occasional off normal conditions that would typically result in a loss of temperature control and NIF operational delays ranging from several hours to several days per month. The increased cooling capacity and thermal stability could also allow for layering of new target platforms that have less cooling margin. Additional layer images could be used for better characterization of defects and non-uniformities in the layer and would reduce the likelihood of layer seed loss, which typically adds ~12 hours per week in layering time. Motion blur from vibration due to off normal activity in the NIF Target Bay could also be mitigated that would usually result in NIF operational delays of several hours every month.

42 ENGINEERING↗

Cooperative Research and Development Agreement between National Energy Technology Laboratory and Korea Institute of Energy Research (KIER) [Abstract]

KIER and NETL will collaborate to study hydrate-based technologies to enhance desalination, gas separation, and hydrocarbon flow through pipelines and wellbores. With optimized selections of hydrate formers and reactors, gas hydrates can be effective and economic mechanisms of separation for solid-water and gas mixtures, and gas hydrate formation or dissociation can be significantly delayed or expedited with suitably selected additives. Comprehensive laboratory studies, including identifying novel hydrate formers or inhibitors to control temperature and pressure requirements and understanding their working mechanism or developing reactor systems for production of large quantities of hydrates, will be performed at both KIER and NETL either parallelly or serially.

03 NATURAL GAS↗

Cooperative Research and Development Agreement between National Energy Technology Laboratory and Raytheon Technologies Corporation [Abstract]

KIER and NETL will collaborate to study hydrate-based technologies to enhance desalination, gas separation, and hydrocarbon flow through pipelines and wellbores. With optimized selections of hydrate formers and reactors, gas hydrates can be effective and economic mechanisms of separation for solid-water and gas mixtures, and gas hydrate formation or dissociation can be significantly delayed or expedited with suitably selected additives. Comprehensive laboratory studies, including identifying novel hydrate formers or inhibitors to control temperature and pressure requirements and understanding their working mechanism or developing reactor systems for production of large quantities of hydrates, will be performed at both KIER and NETL either parallelly or serially.

02 PETROLEUM↗

Low-Cost, Accessible Vaccine Cooler Options

In response to cold chain management requirements for COVID-19 vaccines, Los Alamos National Laboratory has investigated, built, and demonstrated viability for different cryogenic storage options. With ease-of-access and affordability in mind, these cooler units have been built using commercial off-the-shelf (COTS) components. The team was also able to design a testing method for evaluating the performance of the different vaccine cooler options as part of the Technology Evaluation and Demonstration program. The tested cooler units demonstrated compatibility with either dry ice or liquid nitrogen as the cryogen, along with several commercial solvents. This compatibility demonstration would potentially offer sufficient flexibility for temperature control continuity. Next steps are to investigate industry interest in supporting field testing of the cooler units.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Photon Entanglement Spectroscopy and Imaging in Actinide Research

Quantumly entangled particles are capable of affecting the quantum state of their entangled counterpart instantaneously once one particle has changed. Herein, quantumly entangled photons are generated by spontaneous parametric down conversion through a temperature controlled non-linear crystals. This process generates two pairs of photons of lower energy of which the sum of energy equals the energy of the pump photons. These entangled photons can be separated and provide imaging capabilities by using one set of photons for imaging and the other set of photons for detection.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Fiscal Year 2021 Filtration of Hanford Tank 241-AP-107 Supernatant Samples Obtained at Prototypic Tank Level and Filtered at 16 °C

Bench-scale filtration testing of 8.5 liters of supernatant from Hanford waste tank 241-AP-107, chilled to 16 °C, was conducted using a backpulse dead-end filter (BDEF) filtration system equipped with a feed vessel and a Mott inline filter Model 6610 (Media Grade 5) in the hot cells of the Radiochemical Processing Laboratory at Pacific Northwest National Laboratory. This was done to assess the impact of a lower sampling location within the tank as well the lowered filtration temperature on supernatant stability and fouling. The as-received samples were transferred to 1.5-liter poly bottles and held at 16 °C for approximately 1 week prior to filtration. The feed was filtered through the BDEF system at a targeted flux of 0.065 gpm/ft 2 to match the prototypic operation of the TSCR system. During the initial period of filtration, the differential pressure required to effect filtration at 0.065 gpm/ft 2 increased until it reached 2 psid [the Tank Side Cesium Removal (TSCR) action limit] at 26 hours. After this, the filter was backpulsed to dislodge accumulated solids and reduce this pressure differential. An additional eight backpulses were conducted during the initial filtration period; each time, the target pressure was reached sooner than during the previous interval. Volume filtered decreased from 0.9 to 0.03 m 3 /m 2 over the course of 14 processing hours. After the ninth backpulse, the backpulse frequency had become unsustainable, and it was decided to perform an extensive filter cleaning. The filter was cleaned by draining the chilled AP-107 feed into chilled holding containers, introducing 0.1 M NaOH into the feed vessel, and recirculating the NaOH through the system for 20 minutes before allowing the system to soak for 2 hours without temperature control. A measurable decrease in filter resistance during this recirculation indicated that the 0.1 M NaOH was likely dissolving some of the solids that had deposited on the filter. Post cleaning, the filter resistance was effectively restored to initial conditions as the initial transmembrane pressure was restored to original levels. However, resumed processing of the AP-107 feed at 16 °C continued to result in an increased rate of filter resistance. An additional five backpulses were conducted (four during feed processing, one during subsequent cleaning) before the conclusion of the test. Solids concentrated from the backpulse solutions displayed sodium oxalate-type phases, Al-oxides and sodium Al-oxides/carbonates, iron oxides, and Ca-bearing phases (calcite). The scanning electron microscopy analyses also revealed a large distribution of particles, with some particles, notably sodium phosphate dodecahydrate, having diameters close to 0.5 mm.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Development of Enabling Technologies for Chemical Looping Combustion and Chemical Looping with Oxygen Uncoupling (Final Report)

This report summarizes results from the project, “Development of Enabling Technologies for Chemical Looping Combustion and Chemical Looping with Oxygen Uncoupling,” which evaluated several aspects of dual fluidized bed chemical looping combustion and chemical looping with oxygen uncoupling (CLOU). The objective was to provide tools and enabling technologies to help advance fluidized bed chemical looping technology to pilot, demonstration and commercial scale. One focus area is oxygen carriers, which are key to chemical looping combustion. The copper oxygen carrier-coal ash system was systematically evaluated through a combination of thermodynamic modeling and lab-scale experiments, taking into consideration different oxygen carrier support materials and coal types. A method of mapping “safe” and “risk” zones for different combinations was established, and recommendations for target conditions are provided. In addition, a simple solution for limiting negative influence of some coal ashes, namely adding small amounts of calcium to the system, is proposed. In addition, a novel process for recovering and recycling copper from spent oxygen carriers is proposed. A new approach for design and operation of loop seals in a CLOU system was developed, and involves distinct gas injection points and a short horizontal section to help control the fate of the fluidizing gases. For the air-to-fuel reactor loop seal, the upstream side is fluidized with air, ideally input into the side rather than into the bottom, which prevents uncoupling (reduction) of the oxygen carrier before entering the fuel reactor. Also, alternative for separating oxygen carrier particles and gas in circulating fluidized bed-based chemical looping system is proposed. A new reduced reaction scheme for conversion of coal in copper-based CLOU was developed and implemented into CPFD Software’s Barracuda VR package. The resulting model provides higher fidelity than the baseline, especially when it comes to minor reactions that are part of the overall combustion environment. For in-reactor heat extraction, it was determined in this project that the best way to do that in a dual circulating fluidized-bed system is through heat exchange low in the air reactor. The air reactor is the hotter of the two and for a fast-fluidized circulating bed, the lower, more dense section has a higher heat transfer coefficient and offers more consistent particle-wall contact since it doesn’t have the splashing behavior the top of the bed does. It was determined that just the wall surface area in the lower quarter to third of the air reactor is sufficient to control temperatures in both reactors. Finally, consideration was given to a new concept for CLC, which involves a staged fuel reactor with a different type of oxygen carrier in each stage.

01 COAL, LIGNITE, AND PEAT↗

ENG 572 Interim Report

Sandia National Laboratories is a Federally Funded Research and Development Center (FFRDC) founded in 1949 with the mission of developing and testing the non-nuclear components of nuclear weapons. Sandia has since been involved with numerous projects to support the Department of Defense’s (DOE) National Nuclear Security Administration (NNSA). One such set of projects has been implementing over-the-road transportation security enhancements. Under this program, Sandia National Laboratories (SNL) has worked to develop interface compatibility modifications for existing shipping configurations. This summer I will be working with a line of trailers that have been used to transport high asset cargo. These vehicles have successfully traveled millions of miles without any accidents over the course of 15 years. The primary motivation for the work that I will complete this summer is to provide support for existing electronic communication technologies implemented at SNL. As part of an ongoing project to implement modifications to a trailer system, I will focus primarily on the characterization and testing of thermal electric coolers (TEC). Within the scope of the trailer project, these devices provide temperature control for lasers used on optical communication boards (OCB).

42 ENGINEERING↗

Continuous Fiber Bath Treatments at Pilot Scale: A Novel Testbed System

The technical demands on high performance textiles continues to expand, and the research community has answered the call with innovative fiber bath treatments for enhanced properties and sizings for improved composites. However, little translation to greater scale has been demonstrated. To fill this gap, a novel, multifunctional system has been developed to explore polymer fiber treatment methods, the deployment of nanoadditive coatings and other sizings, and smart processing methods at the pilot scale. Continuous tows of fibers can be passed through a temperature-controlled, crossflow bath with an immersion residence time exceeding 2 hours. The modular system is resistant to corrosive solutions, includes additional inline stations for washing and drying after processing, is equipped with a bevy of sensors, pumps, and valves monitored and controlled by a LabView program, and can be fully contained in a standard lab fume hood. This new testbed system, when coupled with high fidelity materials characterization methods, will enable rapid evaluation of new fiber treatment methods at pilot-scale.

36 MATERIALS SCIENCE↗

Technical Guidance on Use of the Linseis Vertical Dilatometer L75

Linseis vertical Dilatometer L75 thermal expansion equipment is a complete system which can be used for measuring change of the absolute length of a sample, determination of the thermal expansion coefficient (CTE), shrinkage, and sintering. The 238 Pu Supply Program is interested in re-establishing the capability to determine CTE and measuring the change of the absolute length of various 237 Np Al/cermet samples during heating. The change in length of the measured sample is recorded using a highly sensitive Linear Variable Differential Transformer (LVDT). The dilatometer is user-friendly and simple to operate which will allow technicians to be trained easily on its use. This equipment was designed to be used specifically for ceramics. It has a highly vacuum tight push rod dilatometer, a high-resolution inductive transducer using innovative and comprehensive temperature controls which provide excellent performance as a measurement system yielding high accuracy, reproducibility, and long-term stability.

07 ISOTOPE AND RADIATION SOURCES↗

Time-dependent THMC properties and microstructural evolution of damaged rocks in excavation damage zone

Modeling coupled thermo-hydro-mechanical-chemical (THMC) processes in host rocks near high-level nuclear waste (HLW) repositories at various time scales is an extremely challenging task. The current study integrates experimental, theoretical, and numerical methods in assessing the evolution of excavation damage zone (EDZ) over time and its implication on the long-term migration of hazardous species. Argillite and rock salt and are the focus of this study. The first part of the report presents a novel time-dependent directional microcrack damage theory for generic brittle rocks. It features detailed statistical description of the microcracks within a damaged solid, permitting a direct upscaling of microscale processes such as crack growth kinetics, crack closure/opening, sliding friction to explain the macroscopic creep, nonlinear elasticity, shear dilation, and loading-unloading hysteresis. This provides a basic platform for describing the anisotropic mechanical and transport properties of damaged rocks during excavation and subsequent THMC loadings. The model is validated and numerically implemented to Finite Element (FE) package ABAQUS through the user-defined material (UMAT) interface and have demonstrated great potential in resolving the time-dependent and anisotropic evolution of damage in the EDZ. The second part of the report presents a multi-scale experimental effort in characterizing the thermal, hydraulic, and mechanical properties of Mancos shale and Avery Island salt. For the Mancos shale, triaxial compression tests are performed at different confining pressures and temperatures to probe its thermomechanical properties relevant to HLW repositories. The obtained stress-strain data are interpreted using the proposed directional damage theory. Post-test specimens are subjected to gas permeability tests to reveal the correlation between permeability and the degree of microcracking. At microscale, temperature-controlled nanoindentation tests are performed and found a linear correlation between fracture toughness and elastic modulus from 25°C to 300°C. For Avery Island salt, we have designed and manufactured a novel relative-humidity controlled uniaxial creep device. Long-term creep tests at low stresses (< 5 MPa) are performed at different levels of relative humidity (RH). Besides confirming the much higher creep rates as one would expect through extrapolating the high-stress creep data, the results reveal that the steady-state creep rate of rock salt is strongly dependent on the ambient RH, an aspect that is often neglected in the literature. Both behaviors can be attributed to the pressure-solution creep mechanism which dominates at low stress and high RH levels. The third part of the report explores a set of numerical strategies in modeling the THMC behavior of porous geomaterials. A fully implicit, monolithic FE solution that can flexibly interface with different material models and coupling mechanisms for THMC problems is developed and verified through the ABAQUS user-defined element (UEL) interface. The scheme is used to study the THM response of a hypothetical HLW storage site with reference to an existing in-situ heater test. Strategies for integrating the UEL and the microcrack UMAT are suggested. Another numerical endeavor of this study is to implement a higher-order asymptotic homogenization method to account for the heterogeneous porous structures. The same method is then extended to perform microstructure-informed thermo-mechanical modeling of generalized continua. The above outcomes of this project provide a strong thrust towards enhancing the fundamental understanding and modeling capability of the long-term evolution of host rocks in EDZ, thus helping achieve the design goal of 1-million-year isolation of high-level nuclear wastes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Modeling of Reactor Design and Optimization for Scale-Up of the Catalyxx Process for Ethanol Conversion to Higher Alcohol Biofuels

This report summarizes the results of a collaborative efforts between Oak Ridge National Laboratory (ORNL) and Catalyxx Inc. to investigate scale-up of Catalyxx’s Ethanol upgrading to higher alcohols process. The study was funded by the U.S. Department of Energy (DOE) Bioenergy Technologies Office (BETO) under CRADA (Cooperative Research and Development Agreement) No: NFE-20-08396. The project is part of the Direct Funding Opportunity (DFO) for Computational Science to Enable Bioenergy program which utilized computational toolsets developed by the Consortium for Computational Physics and Chemistry, a multi-laboratory consortium in BETO. The report here summarizes a packed-bed reactor modeling effort spanning the range from lab to industrial scale (from 4 gram to 5-ton catalyst beds), and examining reactor design, process optimization strategies, and suggested design and operating conditions for Catalyxx’s ethanol upgrading plants. The results in this report have been shared in monthly steering meetings and presentations are available in the shared data house owned by Catalyxx. The modeling effort helped to define optimum operation conditions for maximum alcohol selectivity and yield: i.e., temperature control scenarios ranging from adiabatic to isothermal, feed rate, pressure, and inlet H 2 /Ethanol ratio. The modeling results were verified at lab-(4 gram) and pre-pilot (4 kg) scales and has been used to evaluate a 5-ton packed-bed reactor and identify operating conditions to maximize the butanol yield. Special focus was given to understanding mass-transfer effects in the pre-pilot and pilot-scale reactors, over the domain of flow rate, pressure, feed composition, pellet size, shape, porosity, bed voidage, and reactor dimensions (i.e., length/diameter). Modeling was also used to evaluate innovative reactor design concepts such as water removal to improve alcohol selectivity and yield, and a reactor with an additional side inlet to facilitate quenching. These concepts were thoroughly explored, and potential benefits were disclosed. The results in this report are summarized and described qualitatively to protect the IP rights of Catalyxx. The details have been shared with the Catalyxx team in the regular steering meetings. At the end of the project, Catalyxx Inc. announced a successful demonstration of pilot scale operation in Seville, Spain.

02 PETROLEUM↗

Cost-efficient temperature mediation of DPMS synthesis in flow using continuous flow chemistry

An efficient synthesis of diphenylmethylsilanol (DPMS) utilizing continuous flow chemistry was performed using a coil reactor and an ice bath. The inclusion of careful temperature control minimized the exothermic production of an unwanted dimer. Yields of up to 88% were obtained and dimer formation as low as 2.2% was confirmed by NMR. This material will be used in the formulation to make SX358 and its physical and chemical characteristics will be determined using DSC, DMA, TMA, compression set testing and FTIR.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Radiative Cooling Paints: Application on Warehouses and Integration with Phase Change Materials

Despite extensive research on radiative cooling (RC), researchers are still working to understand its best implementation strategy and potential benefits. Understanding this could be an instrumental part of reducing building energy costs and combating climate change. In this work, we introduce two concepts to achieve this goal and broaden the application of RC paints. While building energy simulations for RC are common, most studies focus on single-layer paints in residential settings. Limited research exists on warehouses, and no literature has conducted multi-climate zone analyses or included RC technologies with >90% reflectance. As RC technology advances in efficiency, versatility, and affordability, large-scale simulations across diverse climates are crucial, particularly for warehouses as a passive indoor temperature control solution. Here, a TRNSYS-modeled single-story warehouse assesses the energy impact of BaSO4-based RC paints. Another under-explored RC application is its integration with phase change materials (PCMs), which provide thermal regulation via latent heat storage. Though RC and PCMs have been combined by placing PCMs atop, beneath, or within RC layers, studies focus on either experiments or modeling, with no validation between the two. Here, we develop a simple RC+PCM experimental and modeling setup, placing RC paint atop an aluminum cell filled with a Rubitherm PCM.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

AMMT Round Robin 316H HFIR Irradiation Test Matrix and Readiness for Insertion

The Round Robin 316H HFIR-2 irradiation campaign, conducted under the Advanced Materials and Manufacturing Technologies (AMMT) Program, is designed to evaluate the variability in irradiation response of laser powder bed fusion (LPBF) stainless steel (SS)-316H across multiple national laboratories, powder heats, and processing conditions, with comparison to wrought counterparts. A total of 11 materials are intended for irradiation in the High Flux Isotope Reactor (HFIR), targeting two irradiation temperatures (400°C and 600°C) and one level of irradiation damage (2 dpa). This irradiation campaign utilizes the standardized general tensile (GENTEN) capsule design to accommodate subsized tensile specimens of these materials. Thermal analyses were performed to ensure appropriate temperature control by design and uniformity within the capsules. All the capsules for this irradiation except one have been successfully assembled, welded, and tested and are ready for HFIR insertion. The last capsule requires re-build following a failed weld. All eight capsules are intended to be inserted in HFIR cycle 517, which is scheduled to start September 8, 2026. This report summarizes the design, material selection, and readiness for insertion of the capsules.

36 MATERIALS SCIENCE↗

Hydrated Metal and Metal-Nitrate Complexes in Water: Full Lanthanide(III) Series plus Miscellaneous Metal Ions

This is a dataset of hydrated metal complexes and metal–nitrate hydrated complexes intended for public use, reproducibility, and downstream structural analysis. A key feature is coverage across the full lanthanide(III) series (La–Lu), enabling systematic comparisons of coordination motifs and bonding trends across the entire lanthanide sequence. In addition to the lanthanides, the dataset also includes other metal ions such as UO2(VI), Fe(II), and Fe(III). The dataset provides optimized geometries for hydrated and nitrate-containing hydrated complexes, together with representative ab initio molecular dynamics (AIMD) trajectories saved in standard XYZ formats. The accompanying NWChem input decks enable reproduction of the reported calculations and provide a starting point for extending the simulations to related coordination environments. Computationally, DFT calculations employ the B3LYP functional with DFT-D3BJ dispersion corrections and a COSMO continuum solvent model (dielectric constant 78.4) to represent solvation beyond the explicitly treated first hydration shell. AIMD simulations are performed with the NWChem qmd module at 298 K, integrating nuclear motion with the velocity-Verlet algorithm and controlling temperature using a Nosé–Hoover thermostat. Trajectories are approximately 4.8 ps in length and are used primarily to assess short-time stability of candidate coordination motifs, including (for lanthanides) differences between 8- versus 9-water coordination and comparisons between nitrate-bound and nitrate-free hydrated complexes.

Dinpajooh, Mohammadhasan [Pacific Northwest Nation↗

Synchrotron-based techniques for characterizing STCH water-splitting materials

Understanding the role of oxygen vacancy–induced atomic and electronic structural changes to complex metal oxides during water-splitting processes is paramount to advancing the field of solar thermochemical hydrogen production (STCH). The formulation and confirmation of a mechanism for these types of chemical reactions necessitate a multifaceted experimental approach, featuring advanced structural characterization methods. Synchrotron X-ray techniques are essential to the rapidly advancing field of STCH in part due to properties such as high brilliance, high coherence, and variable energy that provide sensitivity, resolution, and rapid data acquisition times required for the characterization of complex metal oxides during water-splitting cycles. X-ray diffraction (XRD) is commonly used for determining the structures and phase purity of new materials synthesized by solid-state techniques and monitoring the structural integrity of oxides during water-splitting processes (e.g., oxygen vacancy–induced lattice expansion). X-ray absorption spectroscopy (XAS) is an element-specific technique and is sensitive to local atomic and electronic changes encountered around metal coordination centers during redox. While in operando measurements are desirable, the experimental conditions required for such measurements (high temperatures, controlled oxygen partial pressures, and H 2 O) practically necessitate in situ measurements that do not meet all operating conditions or ex situ measurements. Here, we highlight the application of synchrotron X-ray scattering and spectroscopic techniques using both in situ and ex situ measurements, emphasizing the advantages and limitations of each method as they relate to water-splitting processes. The best practices are discussed for preparing quenched states of reduction and performing synchrotron measurements, which focus on XRD and XAS at soft (e.g., oxygen K-edge, transition metal L-edges, and lanthanide M-edges) and hard (e.g., transition metal K-edges and lanthanide L-edges) X-ray energies. The X-ray absorption spectra of these complex oxides are a convolution of multiple contributions with accurate interpretation being contingent on computational methods. The state-of-the-art methods are discussed that enable peak positions and intensities to be related to material electronic and structural properties. Through careful experimental design, these studies can elucidate complex structure–property relationships as they pertain to nonstoichiometric water splitting. A survey of modern approaches for the evaluation of water-splitting materials at synchrotron sources under various experimental conditions is provided, and available software for data analysis is discussed.

08 HYDROGEN↗