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Synthesis of phase-pure and monodisperse iron oxide nanoparticles by thermal decomposition

We present a comprehensive template for the design and synthesis of iron oxide nanoparticles with control over size, size distribution, phase, and resulting properties. Monodisperse superparamagnetic iron oxide nanoparticles were synthesized by thermal decomposition of three different iron containing precursors (iron oleate, iron pentacarbonyl, and iron oxyhydroxide) in organic solvents under a variety of synthetic conditions. We compare the suitability of these three kinetically controlled synthesis protocols, which have in common the use of iron oleate as a starting precursor or reaction intermediate, for producing nanoparticles with specific size and magnetic properties. Monodisperse particles were produced over a tunable range of sizes from approximately 2-30 nm. Reaction parameters such as precursor concentration, addition of surfactant, temperature, ramp rate, and time were adjusted to kinetically control size and size-distribution. In particular, large quantities of excess surfactant (up to 25:1 molar ratio) alter reaction kinetics and result in larger particles with uniform size; however, there is often a trade-off between large particles and a narrow size distribution. Iron oxide phase is also critical for establishing magnetic properties. As an example, we show the importance of obtaining the required iron oxide phase for application to Magnetic Particle Imaging (MPI), and describe how phase purity can be controlled.

Environmental Molecular Sciences Laboratory↗

Co-Operative Resource Allocation: Building an Open Cloud Market Using Shared Infrastructure

In this paper we present DRIVE, a distributed service-based system designed to facilitate an open economic market for federating Cloud providers. Additionally, to address the challenges associated with market ownership and operation we propose the use of a cooperative (co-op) infrastructure in which the services that make up DRIVE are hosted across participants' resources. To prevent malicious behavior we use cryptographic, secure and privacy preserving allocation protocols as a means of establishing trust in the allocation infrastructure. Finally, we investigate through simulation the effect of different strategies, pricing functions, and penalty models on allocation performance and revenue, and show that the overhead of running DRIVE's services on commodity infrastructure is modest.

97 MATHEMATICS AND COMPUTING↗

Development of a Hardware-in-The-Loop Testbed for a Decentralized, Data-Driven Electric Vehicle Charging Control Algorithm

This study presents the design of an electric vehicle (EV)-grid integration (EVGI) hardware test-bed to implement smart EV charging algorithms. Here, the proposed test-bed also allows to create different grid events via flexible integration of other power hardware (e.g., controllable loads and battery energy storage systems) and test their impacts on EV charging. The design uses a real-time digital simulator to realize a complex distribution grid model with primary and secondary networks. A grid simulator physically realizes the selected nodes of the simulated grid to power an actual EV, forming a hardware-in-the-loop (HIL) test setup. The EV-grid integration is demonstrated based on the custom hardware and software implementation of the J1772 charging protocol using dSPACE MicroLabBox, operating as a custom EV Supply Equipment (EVSE). The HIL test-bed features a novel testing platform for accurate implementation and analysis of scalable charging algorithms. To this end, a data-driven, decentralized, model-free charging controller based on the Additive Increase and Multiplicative Decrease (AIMD) algorithm is presented and validated on an EV using the HIL test-bed. We tested the proposed algorithm under various case studies, and presented a comparison study with an existing droop-based, decentralized charging solution. The results showed that the EV successfully performed charging commands generated by the EVSE and regulated its charging power to effectively reduce the system loading caused by high EV penetration.

33 ADVANCED PROPULSION SYSTEMS↗

MO-FG-204-09: High Spatial Resolution and Artifact-Free CT Bone Imaging at Off-Centered Positions: An Application of Model-Based Iterative Reconstruction

Purpose: Although the anatomy of interest should be positioned as close as possible to the isocenter of CT scanners, off-centering may be inevitable during certain exams in clinical practice such as lumbar spine and elbow imaging. Off-centering degrades image sharpness, generates streak artifacts, and sometimes creates blooming artifacts due to truncation. The purpose of this work was to investigate whether the use of model-based image reconstruction (MBIR) can alleviate the negative impacts of off-centering to achieve high quality CT bone imaging. Methods: Both an anthropomorphic phantom and an ex vivo swine elbow sample were scanned at centered and off-centered positions using clinical CT bone scan protocols. The magnitude of off-centering was determined from localizer radiographs. Both FBP and MBIR reconstructions were performed. For FBP, both standard and Bone Plus kernels commonly used in bone imaging were used. Objective assessment of image sharpness, noise standard deviation, and noise nonuniformity were performed. Additionally, we retrospectively analyzed human subject data acquired under off-centered conditions as a validation study. Results: In FBP images of the phantom, off-centering by 10 cm led to a 14% increase in noise (p<1e-3) and a 68% increase in noise nonuniformity (p<0.02). A visible drop in bone sharpness was observed. In contrast, no significant difference in the noise magnitude or the noise nonuniformity between the centered and off-centered MBIR images was found. The image sharpness of off-centered MBIR images outperformed that of FBP images reconstructed with the Bone Plus kernel. In images of the swine elbow off-centered by 20 cm, not only was the noise and spatial resolution performance improved by MBIR, truncation artifacts were also elliminated. The human subject study generated similar results, in which the visibility of the off-centered lumbar spine was significantly improved. Conclusion: High quality CT bone imaging at off-centered positions can be achieved using MBIR. This work was partially supported by an NIH grant R01CA169331 and GE Healthcare. K. Li, D. Gomez-Cardona: Nothing to disclose. G.-H. Chen: Research funded, GE Healthcare; Research funded, Siemens AX. A. Budde, J. Hsieh: Employee, GE Healthcare.

60 APPLIED LIFE SCIENCES↗

WHONDRS Summer 2019 Sampling Campaign: Global River Corridor Surface Water FTICR-MS, NPOC, TN, Anions, Stable Isotopes, Bacterial Abundance, and Dissolved Inorganic Carbon (v8)

The WHONDRS Summer 2019 Sampling (S19S) Campaign collected samples in 97 globally distributed river corridor systems between July and September 2019. Surficial streambed sediments were collected at three locations within each site (upstream, midstream, and downstream). Surface water was collected at the downstream site. This dataset includes a portion of the data types produced from the surface water samples and does not include any results from the sediment. Sediment data can be found at https://data.ess-dive.lbl.gov/view/doi:10.15485/1729719. The S19S campaign was designed with the science community to ask questions associated with links among core/transient metabolomes, microbial metabolism, biogeochemical function, and physical properties of watershed and river corridor systems. This data package was originally published in March 2020. It was updated in October 2020 (v2, new and modified files), July 2021 (v3, new and modified files), January 2023 (v4, new and modified files), February 2023 (v5, new and modified files), August 2023 (v6, new and modified files), July 2025 (v7,new and modified files), and August 2026 (v8, new and modified files). Version 8 includes major restructuring of the files and their formats. See the change history section in readme for more details. In addition to a readme, this data package also includes a file-level metadata (FLMD) file that describes each file and a data dictionary (DD) that describes all column/row headers and variable definitions. This dataset contains (1) readme, (2) data dictionary, (3) file level metadata, (4) sampling protocol, (5) a data checks report, (6) field metadata, (7) international generic sample number (IGSN) mapping file, (8) joint genome institute (JGI) mapping file, and (9) a folder of sample data. The sample data folder contains (1) dissolved organic carbon (DOC, measured as non-purgeable organic carbon, NPOC) and FTICR methods, (2) dissolved inorganic carbon (DIC), (3) stable water isotopes (O and H), (4) specific conductivity, (5) total dissolved nitrogen (TN), (6) anions, (7) flow cytometry bacterial abundance data, (8) laboratory methods, and (9) a folder containing unaligned, peak-picked high resolution characterization of dissolved organic matter from sediment via 12 Tesla Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS) through the Environmental Molecular Sciences Laboratory (EMSL, https://www.pnnl.gov/environmental-molecular-sciences-laboratory), and (12) a folder containing processed FTICR-MS data. All files are .msa, .txt, .spx, .xml, .csv, .pdf, .txt, .html, .jpg, or .jpeg.

18-O↗

WHONDRS Summer 2019 Sampling Campaign: Global River Corridor Sediment FTICR-MS, Dissolved Organic Carbon, Aerobic Respiration, Elemental Composition, Grain Size, Total Nitrogen and Organic Carbon Content, Bacterial Abundance, and Stable Isotopes (v10)

The WHONDRS Summer 2019 Sampling (S19S) Campaign collected samples in 97 globally distributed river corridor systems between July and September 2019. Surficial streambed sediments were collected at three locations within each site (upstream, midstream, and downstream). Surface water was collected at the downstream site. This dataset includes a portion of the data types produced from the sediment samples and does not include any results from the surface water. Surface water data can be found at https://data.ess-dive.lbl.gov/view/doi:10.15485/1603775. The S19S campaign was designed with the science community to ask questions associated with links among core/transient metabolomes, microbial metabolism, biogeochemical function, and physical properties of watershed and river corridor systems. This data package was originally published in December 2020. It was updated in April 2021 (v2; modified files), May 2022 (v3; new and modified files), November 2022 (v4; new and modified files), January 2023 (v5 and v6; new and modified files), February 2023 (v7; new and modified files), August 2023 (v8; new and modified files), July 2025 (v9; new and modified files), and June 2026 (v10; new and modified files). Version 10 includes major restructuring of the files and their formats. See the change history in the readme for details. In addition to a readme, this data package also includes a file-level metadata (FLMD) file that describes each file and a data dictionary (DD) that describes all column/row headers and variable definitions. This dataset contains (1) readme, (2) data dictionary, (3) file level metadata, (4) sampling protocol, (5) a data checks report, (6) field metadata, (7) international generic sample number (IGSN) mapping file, (8) joint genome institute (JGI) mapping file, (9) a folder of site photos, and (10) a folder of sample data. The sample data folder contains (1) dissolved organic carbon (DOC, measured as non-purgeable organic carbon, NPOC) and FTICR methods; (2) respiration rates and normalized respiration rates calculated from laboratory sediment incubations, (3) X-ray fluorescence (XRF) elemental composition, (4) grain size distribution from the < 2 millimeter fraction of sediment, (5) total organic carbon and total nitrogen content, (6) bacterial abundance flow cytometry data, (7) sediment stable isotopes (C and N), (8) laboratory methods, (9) water and sediment mass and volume used in incubations, (10) a folder with code, inputs, and plots for the respiration rates, (11) a folder containing XRF data, (12) a folder containing unaligned, peak-picked high resolution characterization of dissolved organic matter from sediment via 12 Tesla Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS) through the Environmental Molecular Sciences Laboratory (EMSL; https://www.pnnl.gov/environmental-molecular-sciences-laboratory), (12) and a folder containing processed FTICR-MS data. All files are .msa, .txt, .spx, .xml, .csv, .pdf, .txt, .jpg, or .jpeg.

13C↗

Variation in Biomass Composition Components among Forage, Biomass, Sorghum-Sudangrass, and Sweet Sorghum Types

Alternative biomass sources must be developed if the United States is to meet the goal in the U.S. Energy Security Act of 2007 to derive 30% of its petroleum from renewable sources, and several different biomass crops are currently in development. Sorghum [Sorghum bicolor (L.) Moench] is one such crop that will be an important feedstock source for biofuel production. As composition influences productivity, there exists a need to understand the range in composition observed within the crop. The goal of this research was to assess the range in dietary fiber composition observed within different types of biomass sorghums. A total of 152 sorghum samples were divided into the four end-use types of sorghum: biomass, forage, sorghum-sudangrass, and sweet. These samples were analyzed chemically using dietary fiber analysis performed at the National Renewable Energy Laboratory using published protocols. Significant variation among the groups was detected for glucan and ash. Positive and highly significant correlations were detected between structural carbohydrates in the biomass and sweet sorghums while many of these correlations were negative or not significant in the forage and sorghum-sudangrass types. In addition, a wide range of variation was present within each group indicating that there is potential to manipulate the composition of the crop.

02 PETROLEUM↗

Detecting Process Equipment Failures Using Acoustic Data and Machine Learning

Nuclear power plant (NPP) process equipment such as fans, motors, valves, and pumps generate frequent or continuous noise, and deviations from the normal operational sounds made by this equipment can indicate potential issues. These deviations can be identified via automated acoustic anomaly detection, which involves using acoustic sensors (i.e., microphones) alongside detection algorithms to continuously monitor for changes in acoustic signatures. This task is made challenging by the substantial background noise that exists, such as operators opening and closing doors, manipulating valves, and conversing—in addition to typical plant noises. In collaboration with a nuclear power utility partner, this effort assessed the efficacy of acoustic anomaly detection when using a specific acoustic sensor that compresses data into a fixed set of features that are transferable over a standard Internet of Things communication protocol, thereby improving usability but potentially degrading detection performance. Two methods of performing automated acoustic anomaly detection were evaluated: one-class support vector machine (OC-SVM) and isolation forest (iForest). To enable the use of high-quality acoustic data encompassing both normal and anomalous conditions, the study utilized the publicly available Malfunctioning Industrial Machine Investigation and Inspection dataset, which includes real measured acoustic sensor data for a range of equipment types, model numbers, and signal-to-noise ratios (SNRs), along with a benchmark set of detection results. Using this dataset, the methods were tested and then compared against the benchmark results. The results indicated that although the specific acoustic sensor did not enable as rich a feature set extraction, the proposed methods with the limited feature set performed just as well. This provides solid justification for both the methods and the use of the proposed acoustic sensor.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗

Water Contamination Impacts on Biodiesel Antioxidants and Storage Stability

Biodiesel (fatty acid methyl esters) can oxidize in storage to form acids and gums that negatively impact engine performance and durability. Antioxidant additives are used to increase biodiesel storage stability, and previous studies that evaluated the effectiveness of antioxidants demonstrated that more polar antioxidants tend to be the most effective (provide the largest improvement in stability per unit of antioxidant added). However, polar antioxidants have significant water solubility, and diesel fuel storage tanks are commonly contaminated with water (forming a layer of water under the fuel). This study investigates whether nonpolar antioxidants, which are less effective in dry environments, might be more effective under wet conditions simulating real-world storage. Biodiesel blends treated with polar and nonpolar antioxidants were subjected to accelerated aging using the ASTM D4625 protocol (storage at 43 °C, open to air, for up to 24 weeks) both with and without added water. Fuels treated with polar/higher-effectiveness compounds and stored in contact with water (simulating water in a storage tank) or high humidity showed accelerated loss of stability compared to dry storage. The same fuel treated with a nonpolar antioxidant and stored in the same conditions did not exhibit accelerated stability loss and thus had higher storage stability over the long term despite treatment with an initially less effective additive. Analysis of the fuels during aging showed that this loss of stability was not due to oxidation but rather extraction of the polar antioxidant into the water layer. Antioxidant additives that are incompatible with wet or humid storage conditions were found to cause faster-than-anticipated loss of stability, which was preventable with use of nonpolar additives.

09 BIOMASS FUELS↗

Impacts of Vehicle (In)Security

Nuclear and radioactive material is routinely transported worldwide every day. Since 2010, the complexity of the transport vehicle to support such activities has grown exponentially. Many core functions of a vehicle are now handled by small embedded computer modules with more being added each year to enhance the owner’s experience and convenience. With a system as complex as today’s automobile, the potential for cyber security issues is certain. Hackers have begun exploring this new domain with public information increasingly disseminated. Because vehicles are allowed into and around secure nuclear facilities, the potential for using a vehicle as a new cyber entry point or vector into the facility is now plausible and must be mitigated. In addition, compromising such a vehicle could aide in illicit removal of nuclear material, putting sensitive cargo at risk. Because cyber attacks can now be introduced using vehicles, cyber security, needs to be integrated into an organization’s design basis threat document. Essentially, a vehicle now extends the perimeter for which security professionals are responsible.Electronic Control Units (ECU) responsible for handling all core and ancillary vehicle functions are interconnected using the controller area network (CAN) bus. A typical CAN network in a modern automobile contains 50 or more ECUs. The CAN protocol now supports a wide variety of areas, including automotive, road transportation, rail transportation, industrial automation, power generation, maritime, military vehicles, aviation, and medical devices. In many ways, the nuclear industry is employing the CAN bus protocol or other similar broadcast serial networks. This paper will provide an overview of the current state of automobile and CAN Bus security, as well as an overview of what has been publicly disclosed by many research organizations. It will then present several hypotheses of how vehicle security issues may impact nuclear activities. An initial discussion of how a vehicle can be used as a new threat vector to penetrate secure facilities will be presented. This includes how a modern automobile can be used as the exploitation mechanism for nearby devices such as laptops, cell phones, and wireless access points. Additional discussion will highlight how vehicle security might impact transportation of nuclear material through remote exploitation of a moving vehicle. The final discussion will include what possible implications might be relative to the physical protection systems at nuclear facilities. The audience will also be given details regarding the complexity of attack, thus implying the likelihood of successful exploitation, and information on how such attacks may be mitigated. Emerging security products for automobiles will be discussed and other mitigation methods will be detailed (e.g. disabling vehicle cellular modems). As a result, the audience will have a greater understanding of how to add vehicle security as a part of a comprehensive nuclear security policy.Finally, this paper will highlight the similarities between CAN Bus and other broadcast serial bus networks such as Profibus or DeviceNet, helping educate the reader on how susceptible this type of networking is to nefarious attacks and how it might affect components connected to many different nuclear systems, including control systems, safety systems, emergency systems, and support systems.

47 OTHER INSTRUMENTATION↗

Methodology to determine printability criteria of highly concentrated pastes through rheological characterization

Material extrusion is an additive manufacturing technique that enables the creation of reproducible and complex hardware by depositing a viscous, shear-thinning ink onto a substrate in a custom-pattern via extrusion through a syringe. Here, the ability of an ink to be extruded onto a substrate in many layers, and maintain the desired shape is what defines the printability. Printability is often investigated by formulating, printing, and postmortem analysis of final parts in an iterative manner. Investigations of printability through rheological characterization have often been concerned with inks that straddle the line between printable and too thin, leaving out an entire class of inks that are highly-filled pastes, where extrudability is the limiting factor. Highly-filled pastes continue to pose issues for researchers as the effect of filler morphology, size, loading, and packing fraction on the ink rheology and corresponding printability is not understood. While traditional rheological characterizations may be useful for some inks, we show that protocols utilizing steady-shear, or large-amplitude oscillatory shear are difficult and unreliable for highly-filled pastes. Through transient rheology paired with real-time images we show that each traditional protocol produces inhomogeneous deformations that violate the assumptions that underly common rheological definitions. Instead, we demonstrate metrics measured with small-amplitude oscillatory shear that are correlated to the printability of various ink formulations ranging in loading. The rheological measures that accurately predict the printability of the inks are the axial stress measured at small amplitudes, and the critical stress amplitude above which rheological characterizations become impossible. In addition, we estimate the maximum packing fraction for each filler, based on the exponent common to hard sphere models, and show that the printability of each ink can be predicted by the ratio of the packing fraction to the theoretical maximum. We show how small-amplitude oscillatory shear allows users to develop printability criteria for any ink to enhance the workflow in the development of new inks, increase the performance of material extrusion printing, and improve the stability of printed parts, with less wasted time and materials.

36 MATERIALS SCIENCE↗

Intracranial Aneurysms Treated by Flow-Diverting Stents: Long-Term Follow-Up with Contrast-Enhanced Magnetic Resonance Angiography

PurposeLong-term data on aneurysm treatment with flow-diverting stents are still sparse, and follow-up protocols differ widely between institutions. We present long-term results, with a focus on the usefulness of contrast-enhanced MR angiography (ceMRA).Materials and MethodsInterventions and follow-up imaging of patients with aneurysms treated by flow-diverting stents (“Pipeline,” “Silk” and “FRED” models) without additional coiling were analyzed. All MRI scans included dedicated two-phase ceMRA. Aneurysm occlusion rates, size of the aneurysmal sac and complications were evaluated on MRI and digital subtraction angiography (DSA), where available. The ability of ceMRA to depict aneurysm occlusion and stent patency was graded on a three-point scale.ResultsTwenty-five patients with 102 MRI scans were included. The median duration of follow-up was 830 days. Aneurysm occlusion rates were 52% at 3 months (10 of 19 patients), 72% at 6 months (18/25) and 84% overall (21/25). Shrinkage of the aneurysmal sac was found in 19 patients (76%) and in 12 cases to <50% of the original size (48%). CeMRA assessability of aneurysmal occlusion was graded as good in all cases. When compared to DSA (18 cases), ceMRA had a sensitivity of 100% and specificity of 91% regarding aneurysm remnant detection. Assessability of the stent lumen varied and was limited in most cases.ConclusionsFlow-diverter treatment achieves high occlusion rates and can cause major aneurysm shrinkage. CeMRA is highly valuable regarding imaging of the aneurysmal sac. There are limitations regarding the assessability of the stent lumen on ceMRA. Level of Evidence: Level 4, Case Series.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

A new apparatus for the concurrent measurement of friction and permeability evolution in fault gouge

Here we introduce a new miniature double direct shear (mini-DDS) apparatus, housed within a standard-triaxial (TEMCO) pressure vessel, capable of concurrently measuring the evolution of frictional strength, stability, healing and along-fault permeability under in situ conditions of stress and temperature. The apparatus accommodates gouge samples (25 mm × 32 mm) and intact rock samples with confining and shear stresses and pore pressures up to ~26 MPa. Permeability may be measured with applied flow rates ranging from 1.67 × 10 -11 to 3.6 × 10 -6 m 3 /s to a flow accuracy of 0.5% representing a lower bound of permeability >2.2 × 10 -18 m 2 . Sliding velocities are in the range 0.1 μm/s to 0.67 cm/s with a frame stiffness of 0.067 kN/μm. We describe protocols and procedures for calibration and experiments and note the potential of the apparatus for both rapid and extended-duration measurements of friction-permeability evolution and healing. The apparatus returns measurements of friction and stability of reference materials of F110 quartz consistent with the literature while additionally allowing the concurrent measurement of permeability. Permeability of F110 quartz evolves in slide-hold-slide (SHS) experiments with increases during holds and decreases during subsequent slides. These observations are consistent with grain crushing and resultant wear products that reduce that permeability by clogging during slides with unclogging of the major fluid channels occurring during shearing.

58 GEOSCIENCES↗

Parallel transmit excitation at 1.5 T based on the minimization of a driving function for device heating

Purpose: To provide a rapid method to reduce the radiofrequency (RF) E-field coupling and consequent heating in long conductors in an interventional MRI (iMRI) setup. Methods: A driving function for device heating (W) was defined as the integration of the E-field along the direction of the wire and calculated through a quasistatic approximation. Based on this function, the phases of four independently controlled transmit channels were dynamically changed in a 1.5 T MRI scanner. During the different excitation configurations, the RF induced heating in a nitinol wire immersed in a saline phantom was measured by fiber-optic temperature sensing. Additionally, a minimization of W as a function of phase and amplitude values of the different channels and constrained by the homogeneity of the RF excitation field (B{sub 1}) over a region of interest was proposed and its results tested on the benchtop. To analyze the validity of the proposed method, using a model of the array and phantom setup tested in the scanner, RF fields and SAR maps were calculated through finite-difference time-domain (FDTD) simulations. In addition to phantom experiments, RF induced heating of an active guidewire inserted in a swine was also evaluated. Results: In the phantom experiment, heating at the tip of the device was reduced by 92% when replacing the body coil by an optimized parallel transmit excitation with same nominal flip angle. In the benchtop, up to 90% heating reduction was measured when implementing the constrained minimization algorithm with the additional degree of freedom given by independent amplitude control. The computation of the optimum phase and amplitude values was executed in just 12 s using a standard CPU. The results of the FDTD simulations showed similar trend of the local SAR at the tip of the wire and measured temperature as well as to a quadratic function of W, confirming the validity of the quasistatic approach for the presented problem at 64 MHz. Imaging and heating reduction of the guidewire were successfully performed in vivo with the proposed hardware and phase control. Conclusions: Phantom and in vivo data demonstrated that additional degrees of freedom in a parallel transmission system can be used to control RF induced heating in long conductors. A novel constrained optimization approach to reduce device heating was also presented that can be run in just few seconds and therefore could be added to an iMRI protocol to improve RF safety.

60 APPLIED LIFE SCIENCES↗

A tailored fast thioacidolysis method incorporating multi-reaction monitoring mode of GC-MS for higher sensitivity on lignin monomer quantification

Abstract Thioacidolysis is widely used for lignin structural characterization by cleaving β-aryl ethers to release syringyl (S), guaiacyl (G), and p -hydroxyphenyl (H) monomers followed by GC analysis. However, the traditional thioacidolysis method requires tedious extraction steps with chlorinated solvent underlying harmful to health, limiting its efficiency and application. Herein, an improved thioacidolysis method with high sensitivity for the quantitation of lignin-derived monomers was developed. The improved protocol used a quick, streamlined procedure to recover the monomeric products using ethyl acetate as extracting solvent and MS detector in multi-reaction monitoring mode to enhance its ability to detect extremely low concentration (0.1 ppb with signal-to-noise higher than 2) of monomeric products. Additionally, a fast GC program was established to speed up the GC quantitation. Several representative lignocellulose samples, including gymnosperm, angiosperm, and poaceae, were used to test this tailored method. The results demonstrated that the ratios of lignin monomer compositions determined by this method were consistent with that of traditional procedure despite the slightly higher monomer yields measured. More importantly, this method uses non-chlorinated solvent for microscale extraction and requires no evaporation step for workup, which is a green and efficient way for the quantification of lignin monomer compositions.

Forestry↗

Preparation of Aluminum Oxide Films Under Water Exposure – Preliminary Report on 1100 Series Alloys

This report describes laboratory experiments performed to produce oxyhydroxide (oxide) films on aluminum 1100 series alloy substrates at various water/temperature conditions. The aluminum alloys selected in this program are types used on aluminum-clad research reactor fuel, and the water/temperature conditions are selected to produce film structures that would be prototypic to those formed on the fuel as a result of reactor exposure and post-discharge water and/or dry storage exposure. The experimental set-up and results to characterize the oxide morphology, thickness, structure, and chemical composition are reported. The results from this work will be compared to oxide characterizations of fuel cladding alloys that have been exposed to actual reactor and post-discharge service conditions. The aim is to develop a laboratory protocol to produce specimens for further studies for response under drying and radiation conditions. The work in this report is interim results and preliminary information prepared under Task 6, Milestone 6.1 in TTQAP SRNL-RP-2018-00610 as part of the action plan described in Ref. [1]. Additional experimental milestones are in progress and will be reported upon completion.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Advancing Insights into Electrochemical Pre‐Treatments of Supported Nanoparticle Electrocatalysts by Combining a Design of Experiments Strategy with In Situ Characterization

Activation, break-in, and/or pre-treatment protocols are generally applied to energy conversion devices before regular operation to reach stable performance. There remains much to understand about the relationships among physical properties, performance, and electrochemical pre-treatments. Here, a design-of-experiments (DoE) strategy is employed to address this gap by demonstrating the influence of five pre-treatment parameters for carbon-supported Pt-nanoparticle catalysts on the electrocatalytic oxygen reduction reaction (ORR). A subset of pre-treatments, developed using a central composite design, are tested in a flow cell combined with an inductively-coupled plasma mass spectrometer (on-line ICP-MS). The DoE-based approach facilitates comprehensive insights from two orders of magnitude fewer experiments than a conventional grid search. The coupled on-line ICP-MS setup enables effective catalysis and real-time catalyst dissolution data. Leveraging insights from DoE for on-line ICP-MS and additional characterization, a model is built between the degradation of a multi-dimensional supported Pt surface, its performance, and applied electrochemical parameters. These investigations identify surface modifications, such as oxidation, and subsequent restructuring of Pt during pre-treatment as a primary cause of performance deterioration during ORR. By combining DoE with advanced characterization techniques, a powerful approach is demonstrated to gain a mechanistic understanding of pre-treatment protocols that can be broadly adapted to various reaction chemistries.

Platinum↗

A Uniform Practice for Conceptualizing and Communicating Food‐Energy‐Water Nexus Studies

There is growing interest in nexus research: energy‐water, energy‐water‐land, and more recently food‐energy‐water. Motivating this movement is the recognition that the dynamics and feedbacks that constitute these nexuses have been overlooked in the past but are critical to the planning and management of these interacting elements. Formal reviews have identified gaps in current studies. In this commentary, we highlight additional oversights that are hindering integration of findings in nexus studies, notably usage of imprecise terminology to describe analyses, a failure to close the loop by linking production with corresponding waste streams, and exclusion of dynamics linking diverse constituent elements. Equally lacking from current nexus studies is a consistent protocol for communicating the conceptual basis of our studies. To fill this gap, we draw on diverse perspectives and fields to propose a comprehensive and systematic framework that can guide the model conceptualization phase of nexus studies. We also present a standardized documentation practice (similar to one utilized by the agent‐based modeling community) to facilitate communication of nexus studies. These initiatives can improve our ability to account for and communicate the nuanced, food‐energy‐water nexus interactions in a consistent manner, which is necessary to better inform risk analysis and avoid decisions with unintended consequences and hidden costs to society.

54 ENVIRONMENTAL SCIENCES↗