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DOE OSTI2022

Materials Design using an Active Subspace-based Batch Bayesian Optimization Approach

Integrated computational materials engineering (ICME) calls for integrating simulation tools and/or experiments to develop new materials and materials systems. However, implementation of ICME approaches is challenging mainly due to the considerable computational expense of such frameworks and large dimensionality of the design space. Addressing these challenges is thus critical to the success of ICME initiatives. We present here a specific Bayesian optimization framework designed to address these two challenges. In particular, we propose an active subspace batch Bayesian optimization framework. The framework makes use of dimension reduction via the active subspace method and makes use of the ability to query in parallel via the batch Bayesian optimization approach. Here, the integration of these techniques leads to significant efficiency improvements while maintaining accuracy.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Sensitivity Study of Mini-Batch Size on a Long Short-Term Memory Network for In-situ Sensing of Core-to-shell Ratio of Microencapsulated Phase Change Materials

Microencapsulated phase change materials are being studied for applications for thermal energy storage in concentrated solar fields. During fabrication, the thickness of the encapsulation cannot be readily measured for real-time control. Therefore, a machine learning network, specifically a Long Short-Term Memory network, is being developed to estimate the ratio of the shell radius to core radius based on a one second temperature history. The mini-batch size determines how often the algorithm weights are updated during network training, and shuffle indicates whether the training data is shuffled during training. A general factorial design is used to analyze the effects of varying mini-batch size and shuffle, along with the core-to-shell ratio, on the RMSE of the response from the Long Short-Term Memory network. It was found that the network performed better for smaller core to shell ratios (less than 0.6) and had the lowest RMSE when the minibatch size was 128. The minimum RMSE found was 0.00501.

Shannon, Rebecca↗

DOE OSTI2020

Summary Report For The Analysis Of The Sludge Batch 7b (Macrobatch 9) DWPF Pour Stream Glass Sample For Canister S04023 (Rev. 1)

In order to comply with the Defense Waste Processing Facility (DWPF) Waste Form Compliance Plan for Sluldge Batch 7b, Savannah River National Laboratory (SRNL) personnel characterized the Defense Waste Processing Facility (DWPF) pour stream (PS) glass sample collected while filling canister S04023. This report summarizes the results of the compositional analysis for reportable oxides and radionuclides and the normalized Product Consistency Test (PCT) results. The PCT responses indicate that the DWPF produced glass that is significantly more durable than the Environmental Assessment glass.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

SRNL Sludge Batch 10 Qualification SRAT and SME Off-Gas Results

Savannah River National Laboratory (SRNL) completed a small-scale demonstration of the Defense Waste Processing Facility (DWPF) Chemical Process Cell (CPC) utilizing the nitric-glycolic acid (NGA) flowsheet to support Sludge Batch 10 (SB10) qualification. The demonstration utilized a Tank 51 slurry sample washed by SRNL (with added H-canyon material). The purpose of this document is to report the observed off-gas results from the demonstration. With the NGA flowsheet, DWPF has a CPC hydrogen generation limit of 2.4×10 -2 lb/h. The peak observed rate was nearly 90 times less than that limit during SRNL testing.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Chemical Characterization Results for Tank 40 Sludge Batch 10 Waste Acceptance Product Specifications (WAPS) Sample

A 3-L sample (HTF-40-23-24) obtained from Tank 40 following transfer of Tank 51 to achieve the final Sludge Batch 10 processing composition was received by Savannah River National Laboratory (SRNL). SRNL was tasked with characterization of the sample in accordance with requirements for reporting the Waste Acceptance Product Specifications. A representative subsample, approximately 500 mL, was prepared by continuously agitating the 3-L sample via a mixing blade inserted into the bottle. This subsample was then used for the chemical and physical characterization reported here. This characterization includes the following: (1) Supernate and slurry density; (2) Weight percent solids; (3) Mercury Analysis (supernate and slurry); (4) Anions; (5) Total Organic/Inorganic Carbon; (6) Free Hydroxide; (7) Other Base; (8) Elementals; (9) Volatile Organic Analysis and Semi-volatile Organic Analysis; and (10) Fissile Radionuclides and Uranium Enrichment. The results of this physical and chemical characterization of the sample are documented in this report.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Sludge Batch 11 Assembly: Tank 35

Savannah River Mission Completion Nuclear Safety and Engineering Integration (SRMC-E) has requested that Savannah River National Laboratory (SRNL) perform Tank 35 characterization analyses in support of Sludge Batch 11 (SB11) assembly. Two Tank 35 samples were delivered to SRNL and composited into a single sample in April 2023. The composite sample was analyzed for the following: density, weight percent solids, chemical composition, radionuclides, supernate corrosion control tests, and x-ray diffraction for burkeite, gibbsite, and boehmite.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Sludge Batch 11 Assembly: Tank 15

Savannah River Mission Completion Nuclear Safety and Engineering Integration (SRMC-E) has requested that Savannah River National Laboratory (SRNL) perform Tank 15 characterization analyses in support of Sludge Batch 11 (SB11) assembly. This report provides important characterization of the slurry in Tank 15 prior to transfer from Tank 15 to Tank 13 (prior to sending to Tank 51) in order to demonstrate that the transfer is "Low Rem" and ensure the sludge concurs with the estimated transfer mass for the SB11 recipe. A total of 3 sets of Tank 15 samples were delivered to SRNL from December 2022 to August 2023. The individual sets of composite samples were analyzed for density, weight percent solids, chemical composition, radionuclides, and/or supernate corrosion control tests.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Sludge Batch 11 Assembly: Tank 26

Savannah River Mission Completion Nuclear Safety and Engineering Integration (SRMC-E) has requested that Savannah River National Laboratory (SRNL) perform Tank 26 characterization analyses in support of Sludge Batch 11 (SB11) assembly. This report provides important characterization of the slurry in Tank 26 prior to transfer from Tank 26 to Tank 51 that confirms the transfer is "Low Rem" and ensures the sludge concurs with the estimated transfer mass for the SB11 recipe. Two Tank 26 samples were delivered to SRNL and composited into a single sample in September 2023. The composite sample was analyzed for the following: density, weight percent solids, chemical composition, radionuclides, supernate corrosion control tests, and x-ray diffraction for burkeite, gibbsite, and boehmite. The slurry was also evaluated for sulfate washing behavior in order to provide knowledge on insoluble sulfate dissolution during Tank 51 sludge washing similar to a previous washing study performed in 2019. The Tank 26 sample results are consistent with and representative of PUREX sludge and the prior usage of Tank 26 as a feed tank for the 1F and 2F Evaporators.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Sludge Batch 11 Assembly: Tank 35

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Sludge Batch 11 Assembly: Tank 26 (Rev.1)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Determination of Reportable Radionuclides for Defense Waste Processing Facility (DWPF) Sludge Batch 10 (Macrobatch 12)

Savannah River National Laboratory (SRNL) was tasked with the radionuclide characterization of the Sludge Batch 10 (SB10) Tank 40 sample (HTF-40-23-24) in accordance with requirements for reporting the Waste Acceptance Product Specifications (WAPS). The Defense Waste Processing Facility (DWPF) is required to report all radionuclides with half-lives greater than ten years and which comprise greater than 0.05% of the total activity inventory for a given waste form at certain specified “index years”. DWPF complies with the requirements by considering the half-life requirement (t1/2 > 10 years) and radionuclides with concentrations greater than 0.01% of the total inventory from the approximate time of production through 1,100 years.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Investigation of the Effect of Injected CO 2 on the Morrow B Sandstone through Laboratory Batch Reaction Experiments: Implications for CO 2 Sequestration in the Farnsworth Unit, Northern Texas, USA

About one million tons of CO 2 have been injected into the Farnsworth unit to date. The target reservoir for CO 2 injection is the Morrow B Sandstone, which is primarily made of quartz with lesser amounts of albite, calcite, chlorite, and clay minerals. The impact of CO 2 injection on the mineralogy, porosity, and pore water composition of the Morrow B Sandstone is a major concern. Although numerical modeling studies suggest that porosity changes will be minimal, significant alterations to mineralogy and pore water composition are expected. Given the implications for CO 2 storage effectiveness and risk assessment, it is crucial to verify the accuracy of theoretical model predictions through laboratory experiments. To this end, batch reaction experiments were conducted to model conditions near an injection well in the Morrow B Sandstone and at locations further away, where the CO 2 has been diluted by formation water. The laboratory experiments involved submerging thin sections of both coarse- and fine-grained facies of the Morrow B Sandstone in formation water samples with varying levels of CO 2 . The experiments were conducted at the reservoir temperature of 75 °C. Two experimental runs were conducted, one lasting for 61 days and the other for 72 days. The initial fluid composition used in the second run was the same as in the first. The mineralogy changes in the thin sections were analyzed using SEM and the Tescan Integrated Mineral Analyzer (TIMA), while changes in the composition of the formation water were determined using ICP-AES. During each experiment, a thin layer of white fine-grained particles consisting mainly of dolomite and silica formed on the surface of the thin sections, leading to significant reductions in Ca, Mg, and Sr in the formation water. This outcome is consistent with numerical model predictions that dolomite would be the primary mineral that would react with injected CO 2 and that silica would be oversaturated in the formation water. Changes in mineral abundance in the thin sections themselves were much less systematic than in the theoretical modeling experiments, perhaps reflecting heterogeneities in the mineral grain size surface area to volume ratios and mineral distributions in the thin sections not considered in the numerical models.

58 GEOSCIENCES↗

DOE OSTI2025

Kinetic Investigation by Batch Processing of Film Growth during the Electrodeposition of Titanium from Ethaline

Titanium electrodeposition as a technological advance has been out of reach due to the poor film quality obtained when using previously developed methods. This study shows that the electrodeposition of Ti is possible and feasible from the deep eutectic solvent ethaline. Moreover, this study shows through batch analysis that this deposition has temperature-dependent aspects that alter the film deposition kinetics upon modest heating. This ultraviolet–visible spectroscopic study is highlighting the more facile reduction of Ti 4+ to Ti 3+ and then to Ti 2+ at elevated temperatures. Understanding the underlying kinetics of electrodeposition opens up new venues for the application of this important metal.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Batch and column studies of radium, actinium, thorium and protactinium on CL resin in nitric acid, hydrochloric acid and hydrofluoric acid

CL resin (TrisKem International) was characterized for separations of radium, actinium, thorium and protactinium. Batch studies are presented for radium, actinium and thorium in HCl and HNO3 as well as for radium, thorium and protactinium in HF. The uptake of thorium from dilute HNO3 (≤ 10 -4 M) and dilute HCl (≤ 10 -4 M) was found to be very high (D w > 100 in HNO 3 and > 1000 in HCl). Kinetics studies on thorium were performed in HCl and HNO 3 to determine suitably for column separations. Six column separation studies are presented including the separation of trace thorium from radium and actinium in dilute HCl and HNO 3 , the separation of radium from 1 mg 232 Th in dilute HCl, the separation of thorium and radium in the presence of HCl and excess Cl-, the separation of radium, protactinium and thorium by retention of protactinium and the separation of protactinium and thorium by retention of thorium.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Fed-batch production of deuterated protein in Escherichia coli for neutron scattering experimentation

Neutron scattering is a powerful technique for determining the structure and dynamics of biological materials in a variety of environmental conditions. A distinguishing property of the neutron is its sensitivity to detecting hydrogen and distinguishing it from its isotope deuterium. This enables unique types of experiments that take advantage of this differential sensitivity called isotopic contrast variation. Using this approach, the chemistry of the system is not changed, but the visibility of individual sample components can be tuned by varying the deuterium content of the system under investigation. Deuterated proteins are commonly produced in bacterial systems that are adapted to growth in D2O minimal media. To maximize the yield of deuterium-labeled protein and efficiently utilize D2O and occasionally the deuterated substrate, fed-batch processes are routinely used to maximize biomass production without compromising cell viability. A step-by-step procedure will be described along with a case study of the production of deuterated green fluorescent protein. Limitations of the process will also be discussed.

Weiss, Kevin L.↗

DOE OSTI2024

Long-term effects of cycle time and volume exchange ratio on poly(3-hydroxybutyrate-co-3-hydroxyvalerate) production from food waste digestate by Haloferax mediterranei cultivated in sequencing batch reactors for 450 days

Food waste digestate was fed into a sequencing batch reactor (SBR) for Haloferax mediterranei (HM) to produce poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV). This SBR was operated uninterruptedly for 450 days to test its stability, during which the cycle time and volume exchange ratio were varied to understand their impacts on the PHBV fermentation performance under ranged organic loading rates (OLR). Results showed that 1) PHBV productivity was proportional to OLR of food waste digestate; 2) substrate and product inhibitions were two limiting factors constraining substrate utilization and PHBV yields; 3) PHBV titer was dependent on the hydraulic retention time of the SBR while a volume exchange ratio lower than 0.5 is unfavorable due to the product inhibitor accumulation. Furthermore, this study for the first time demonstrated that the long-term stability of food waste-fed PHBV production by HM and revealed that inhibition effects could be barriers in SBR limiting the full-scale application of the technology.

09 BIOMASS FUELS↗

DOE OSTI2024

Coupled feldspar dissolution and secondary mineral precipitation in batch systems: 6. Labradorite dissolution, calcite growth, and clay precipitation at 60 °C and pH 8.2–8.4

Here, we conducted experiments on concurrent labradorite dissolution, calcite precipitation, and clay precipitation in batch reactor systems and tracked reaction processes using multiple isotope tracers. Labradorite was chosen for its role as a major and reactive component in basalt; the experiments thus directly impact our understanding of CO 2 storage in basalt aquifers and enhanced rock weathering. We doped initial solutions with 29 Si, 43 Ca, and Ca 13 CO 3 (s). Experiments were conducted at 60 °C and pH ~ 8.3 for up to 840 h, with isotope ratios in the experimental aqueous solutions measured using MC-ICP-MS. Unidirectional rates of labradorite dissolution near equilibrium were approximately two orders of magnitude slower than far-from-equilibrium rates reported in the literature. Calcite growth occurred near equilibrium and the rates were limited by the labradorite dissolution rates. In the steady state phase, the interplay of these three heterogeneous reactions—labradorite dissolution, calcite growth, and clay precipitation—results in a coupled system that approaches a near-equilibrium state. The system does not reach true equilibrium because labradorite continues to dissolve, albeit at a much slower rate near equilibrium. The overall reaction can be approximated as, Na 0.4 Ca 0.6 Al 1.6 Si 2.4 O 8 + 0.6HCO 3 - + 1·.7H 2 O + 0.4H + → 0.4Na + + 0.6CaCO 3(s) + 0.5Al 2 Si 2 O 5 (OH) 4(s) + 0.6Al(OH) 4 - + 1.4SiO 2 o (aq). The experimental results show that using short-term far-from-equilibrium rate constants would lead to an overestimation of feldspar weathering rates at the Earth’s surface (e.g., basalt weathering and enhanced rock weathering) and CO 2 mineralization in basalt aquifers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Influence of aluminum source and Ni/Al ratio in a batch stirred tank reactor on the structure, morphology, and electrochemical performance of Ni-rich NMA cathodes

Here, the structural, morphological, and electrochemical performance of Ni-rich LiNi 0.9 Mn 0.05 Al 0.05 O 2 (955NMA) and LiNi 0.85 Mn 0.05 Al 0.1 O 2 (85,510) cathodes strongly depends on the properties of their hydroxide precursors. Ni-Mn-Al hydroxide precursors were synthesized through controlled co-precipitation in a batch stirred tank reactor, where pH, reaction time, metal-ion feed rate, aluminum source, and aluminum concentration were systematically varied to tailor particle morphology, phase composition, and dopant distribution. Two aluminum sources, aluminum nitrate and sodium aluminate produced two distinct hydroxide precursors NMA(OH) 2 -1 and NMA(OH) 2 -2, which were lithiated to form LiNMA1 (Li 0.992 [Ni 0.905 Mn 0.049 Al 0.046 ]O 2 ) and LiNMA2 (Li 0.990 [Ni 0.850 Mn 0.047 Al 0.103 ]O 2 ). Structural and compositional analyses revealed that aluminum incorporation and phase formation in Ni–Mn–Al hydroxides are governed by local supersaturation and interfacial growth kinetics. Rapid dilute aluminum addition produced aluminum-free β-phase hydroxides, intermediate conditions generated mixed α/β phases, whereas slow concentrated dosing enabled uniform aluminum incorporation and stabilization of the β-phase structure. LiNMA1 delivers a high initial discharge capacity of 223 mAhg −1 but significant capacity fading with 67% retention after 100 cycles, associated with structural instability. In contrast, LiNMA2 delivers a lower initial capacity 172 mAhg −1 yet excellent cycling stability 91% retention, attributed to improved TM–O framework stability and reduced cation disorder.

Capacity↗