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Building 151 NNMA Clean Laboratory Project Soil Sampling and Analysis Plan

This Soil Sampling and Analysis Plan (SAP) was prepared by the Environmental Function Area (EFA)/Technical Services Department (TSD) of the Environment, Safety & Health (ES&H) Directorate for the Project Management Office (PMO) for the proposed Building 151 NNMA Clean Laboratory Project (project) located immediately south of Building 154. The purpose of the SAP was to describe the procedures for collection and analysis of environmental samples and evaluation of analytical data (chemical and radiological) to determine management options of excavated soil during project construction in accordance with Lawrence Livermore National Laboratory’s (LLNL) Soils Screening and Management Plan (SSMP) (LLNL, 2022), which is consistent with U.S. Environmental Protection Agency (EPA) guidance for developing Data Quality Objectives for environmental data (EPA, 2006). The SAP was developed in accordance with the SSMP and based on preliminary design information provided to EFA by PMO. In addition to environmental samples, geotechnical samples will be collected by Consolidated Engineering Laboratories (CEL) on behalf of PMO. Geotechnical samples will be collected from a dedicated geotechnical boring location or co-located with environmental samples. Collection of geotechnical samples is determined by CEL and is therefore not discussed in this SAP.

54 ENVIRONMENTAL SCIENCES↗

Traditional Forensic Examinations on Bulk Special Nuclear Material

The Federal Bureau of Investigation (FBI) Laboratory at Quantico, Virginia is responsible for the forensic examination of radiological evidence and evidence contaminated with radioactive materials. Due to these unique hazards and the necessary specialized safety protocols, the FBI has developed a network of Partner Laboratories (PLs) across the United States of America to support conventional forensic examinations of radiological evidence and evidence contaminated with radioactive materials. In support of this, the FBI Laboratory has established the Hazardous Evidence Analysis Team (HEAT), a group of qualified forensic examiners, scientists, technicians, and photographers who can deploy to laboratories outside of the FBI Laboratory at Quantico, VA to perform conventional forensics on evidence containing/contaminated with hazardous materials. One of the FBI’s PLs, the United States Department of Energy’s Los Alamos National Laboratory (LANL), in Los Alamos, New Mexico, has unique facilities, personnel, and procedures to secure, safely handle, and process significant quantities of special nuclear material (SNM). While LANL’s procedures for working with SNM are well established, working with SNM under evidentiary controls is not. Close cooperation between LANL and FBI HEAT is required due to FBI policies on evidence handling, as well as the challenges associated with the exploitation and preservation of conventional forensics (fingerprints, trace evidence, and photography) on SNM evidence.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

Challenges in practical button cell testing for hydrogen production from high temperature electrolysis of water

High temperature electrolysis of water using solid oxide electrochemical cells (SOEC) is a promising technology for hydrogen production with high energy efficiency and may promote decarbonization when coupled with renewable energy sources and excess heat from nuclear reactors. Over the past several decades there have been extensive scientific and engineering studies on cell materials and degradation behaviors that have greatly improved current density, decreased total resistance, and lowered degradation rates. Although the technology is now at a near-commercial level, maintaining consistency in cell testing and minimizing variance in practical testing environments is an often overlooked but crucial topic. To promote high quality data collection, testing procedures and balance of plant component details are extremely important to consider. This work discusses some key factors affecting the reproducibility of practical SOEC testing on the button cell level, namely, current collection layers, cell sealing procedures, the reliability of steam and hydrogen delivery systems, cell testing fixture design, and reduction procedures. To provide a baseline and a level of standardization for the SOEC community, this work also discloses details of the standard operating procedure and techniques adopted for o-SOEC testing at Idaho National Laboratory (INL).

08 HYDROGEN↗

Development of Chemical Procedures for Isotope Harvesting: Separation of Trace Hafnium from Tungsten

The separation of trace hafnium from bulk tungsten alloys is of interest for isotope harvesting at the National Superconducting Cyclotron Laboratory and the Facility for Rare Ion Beams because 172 Hf, the parent of 172 Lu, accumulates in tungsten alloy beam blockers at these facilities. In this work, a procedure for the separation of trace hafnium from a bulk tungsten alloy (454 g) was established using tracer isotopes ( 175 Hf, 88 Zr, 173 Lu, and 88 Y). Here, the procedure employed dissolution in an HF–HNO 3 solution followed by a calcium fluoride precipitation, and then extraction chromatography was used for more selective separation steps. Two stages of column separations using LN resin (HDEHP based) and TRU resin (CMPO based) were performed. Gamma-ray spectroscopy and mass spectrometry were used to analyze the final hafnium sample and follow the steps in the chemical processing. Furthermore, the final recovery of hafnium was high (90 ± 8)%, and the mass of tungsten and other transition metals was reduced to near background levels (as determined by ICP-MS of the blank acid solutions). Zirconium follows hafnium quantitatively in this procedure; there was no detectable 173 Lu in the final hafnium sample.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Microbial Biomass in Soils Receiving Varying Levels of Organic Inputs - A Data Compilation

This dataset contains soil microbial biomass data compiled from published laboratory studies and field manipulations of organic inputs to soils. Each study included at least three levels of a given type of organic input applied to a given type of soil. Studies were selected from the literature that had experimentally manipulated organic input rates to soils using unburned, non-synthetic material (e.g. plant litters, manures, and composts). Fifty-five (55) studies, conducted from 1997 to October 2019, were chosen and compiled into a dataset with 358 observations from 96 combinations of a given organic material applied to a given soil in agricultural systems, laboratory incubations, forests, or grasslands. • Studies were selected when biomass measurements used the chloroform fumigation-extraction procedure followed by carbon analysis, or, in two instances, studies estimated microbial biomass using phospholipid fatty acid analysis. • Studies that used fewer than three input rates or characterized microbial biomass via substrate induced respiration were excluded. • The temporal and spatial aspects of the laboratory and field studies were not essential to the analyses (Craig et al., 2021) and were not included with the measurement data. These data were used to assess the relationship between organic input amounts and microbial biomass. Complete reference citations are provided if additional information is needed. The compiled data are provided in two .csv files: (1) soil treatments and microbial biomass data and (2) literature citations. The “Study” field is the cross reference between files. Also provided is the R code for reproducing the results in the related publication.

54 ENVIRONMENTAL SCIENCES↗

Practical procedures for sensor quality assessment

Sensors are increasingly deployed for process monitoring and control. These produce on-line measurements at a high frequency, in parallel with low-frequency laboratory measurements. Compared to laboratory practices, sensor data quality assessment and control practices are far less structured at most utilities. This leads to inaccurate sensor data with unknown uncertainty factors.This chapter shows how to establish standard operating procedures (SOPs) to support sensor data quality assessment and control and subsequent maintenance actions by producing relevant sensor metadata. Furthermore, SOPs are provided for the most commonly used wastewater quality sensors, inspired by utility and academic best practices. This chapter builds on definitions provided in Chapter 3 and provides additional definitions specifically related to sensors maintenance. Chapter 6 complements the methods in this chapter, which are based on reference measurements, with data-analytical techniques.

Alferes, Janelcy↗

Cosmogenic 10 Be in pyroxene: laboratory progress, production rate systematics, and application of the 10 Be– 3 He nuclide pair in the Antarctic Dry Valleys

Here, we present cosmogenic- 10 Be and cosmogenic- 3 He data from Ferrar dolerite pyroxenes in surficial rock samples and a bedrock core from the McMurdo Dry Valleys, Antarctica, with the goal of refining the laboratory methods for extracting beryllium from pyroxene, further estimating the 10 Be production rate in pyroxene and demonstrating the applicability of 10 Be– 3 He in mafic rock. The ability to routinely measure cosmogenic 10 Be in pyroxene will open new opportunities for quantifying exposure durations and Earth surface processes in mafic rocks. We describe scalable laboratory methods for isolating beryllium from pyroxene, which include a simple hydrofluoric acid leaching procedure for removing meteoric 10 Be and the addition of a pH 8 precipitation step to reduce the cation load prior to ion exchange chromatography. 10 Be measurements in pyroxene from the surface samples have apparent 3 He exposure ages of 1–6 Myr. We estimate a spallation production rate for 10 Be in pyroxene, referenced to 3 He, of 3.6 ± 0.2 atoms g –1 yr –1 . 10 Be and 3 He measurements in the bedrock core yield initial estimates for parameters associated with 10 Be and 3 He production by negative-muon capture ($f_{10}^{*}$ = 0.00183 and $f_{3}^{*}f_{C}f_{D}$ = 0.00337). Next, we demonstrate that the 10 Be– 3 He pair in pyroxene can be used to simultaneously resolve erosion rates and exposure ages, finding that the measured cosmogenic-nuclide concentrations in our surface samples are best explained by 2–8 Myr of exposure at erosion rates of 0–35 cm Myr –1 . Finally, given the low 10 Be in our laboratory blanks (average of 5.7 × 10 3 atoms), the reported measurement precision, and our estimated production rate, it should be possible to measure 2 g samples with 10 Be concentrations of 6 × 10 4 and 1.5 × 10 4 atoms g –1 with 5 % and 15 % uncertainty, respectively. With this level of precision, Last Glacial Maximum to Late Holocene surfaces can now be dated with 10 Be in pyroxene. Application of 10 Be in pyroxene, alone or in combination with 3 He, will expand possibilities for investigating glacial histories and landscape change in mafic rock.

58 GEOSCIENCES↗

Towards Energy–Efficient Direct Air Capture with Photochemically–Driven CO 2 Release and Solvent Regeneration

The intensive energy demands associated with solvent regeneration and CO 2 release in current direct air capture (DAC) technologies makes their deployment at the massive scales (GtCO 2 /year) required to positively impact the climate economically unfeasible. This challenge underscores the critical need to develop new DAC processes with significantly reduced energy costs. Recently, we developed a new approach to photochemically drive efficient release of CO 2 through an intermolecular proton transfer reaction by exploiting the unique properties of an indazole metastable-state photoacid (mPAH), opening a new avenue towards energy efficient on-demand CO 2 release and solvent regeneration using abundant solar energy instead of heat. In this Concept Article, we will describe the principle of our photochemically-driven CO 2 release approach for solvent-based DAC systems, discuss the essential prerequisites and conditions to realize this cyclable CO 2 release chemistry under ambient conditions. We outline the key findings of our approach, discuss the latest developments from other research laboratories, detail approaches used to monitor DAC systems in situ, and highlight experimental procedures for validating its feasibility. Finally, we conclude with a summary and outlook into the immediate challenges that must be addressed in order to fully exploit this novel photochemically-driven approach to DAC solvent regeneration.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Simultaneous determination of electrical conductivity and thickness of nonmagnetic metallic foils using two-sided multifrequency eddy current techniques

Here, in this paper, we describe a simple method for performing multifrequency eddy current characterization of free-standing uniform-thickness metallic foils using a forked inductive coil arrangement. The method involves measuring the mutual inductance between two coils when a foil is present between the coils, and when it is not present; the ratio of these mutual inductances is compared with an analytical solution, and foil conductivity, thickness, and sheet resistance are simultaneously estimated using numerical inversion and least-squares fitting. This method was used to characterize 34 non-ferrous metallic samples with thicknesses between 50 and 640 μm and with conductivities between 0.8 × 10 7 and 5.8 × 10 7 S/m. The estimated thicknesses from eddy current characterization agreed well with those measured using confocal optical techniques; the two approaches agreed to within 1 μm for samples that were thinner than 200 μm, and to within 0.5% for samples that had a thickness of 200 μm or greater. The estimated conductivities from eddy current characterization were in close agreement with expected values, given knowledge of the materials used. A particular strength of this approach is that the instrumentation needed is broadly available in research and development laboratories and the associated fixturing is easy to manufacture and assemble. A calibration procedure is described that can be used to reduce errors from geometric uncertainties. This calibration requires a sample that has only a known conductivity or thickness; both do not need to be known. The method described herein is likely extensible to conductivities and thickness well outside the ranges measured as part of this work.

47 OTHER INSTRUMENTATION↗

Canister Centerline Cooling Experiments for DPF5-336 Reference Material Made with ERV3b Salt Simulant

This report provides experimental details and results on the elemental distributions (compositions), crystalline/amorphous phase distribution, and microstructures for DPF5-336 reference materials made with ERV3b salt that were subjected to the canister centerline cooling (CCC) heat treatment process. To fabricate these materials, ammonium dihydrogen phosphate was mixed with ERV3b salt simulant and a dechlorination procedure was run in the generation-2 dechlorinator at the Pacific Northwest National Laboratory up to 600°C in an alumina crucible. After the dechlorination process, the product was removed from the crucible, lightly crushed, loaded into a new alumina crucible, Fe 2 O 3 was added, and this was vitrified at 1100°C for 1 hour and quenched. The quenched material was mostly amorphous but showed some small diffraction peaks attributed to Li 3 Fe 2 (PO 4 ) 3 . This quenched material was ground to a fine particle size in a milling chamber, and this was subjected to the CCC cooling profile in duplicate within alumina and fused quartz crucibles. The CCC experiment is designed to simulate the slowest cooling profile (the vertical centerline) of a 0.61-m diameter canister where the slower cooling profile often results in the production of a variety of different crystalline phases upon formation of which result in a residual glass of unknown composition and properties. The information gleaned from these types of experiments will lead to improved composition-property predictions for materials with similar compositions. The results of the alumina and fused quartz experiments show different microstructures but similar diffraction patterns providing evidence of similar crystalline phases being present in each sample. Both samples had monazite [i.e., (Ce,Nd)PO 4 ] and mixtures of phases containing P, Fe, and alkali metal elements. This report completes the milestone M4FT-23PN030104042 with details provided in Appendix B.

36 MATERIALS SCIENCE↗

Site 200 #1400 Block Area New Trailers Project, Soil Sampling and Analysis Plan/Quality Assurance Plan

Lawrence Livermore National Laboratory's (LLNL) Project Management Office (PMO) is proposing to install a series of modular trailers and install associated underground utilities in the 1400 Block at the Livermore Site. This Sampling and Analysis Plan (SAP) outlines the processes and procedures to collect environmental and geotechnical soil samples from the project area and to send the samples to the appropriate laboratory or laboratories for analysis or testing. The resulting environmental laboratory data will determine whether excavated soils can be reused on the project, or which type of landfill or landfills the soils may be sent for disposal. This SAP has been prepared and is organized to be consistent with LLNL's Soils Screening and Management Plan (SSMP) (LLNL, 2019), as well as the U.S. Environmental Protection Agency's (EPA) Data Quality Objectives programs (EPA, 2006).

54 ENVIRONMENTAL SCIENCES↗

Demonstration of Algorithm for Sensor Placement Optimization using Simulation Data

This deliverable reports FY26 progress in advancing a neural-network-based Green’s-function framework for reconstructing neutron-flux distributions from ex-core measurements and for translating reconstruction requirements into a practical detector-layout strategy. Building on the FY25 formulation, the present work had two main objectives: (1) refine and re-evaluate the reconstruction methodology on an updated Purdue University Reactor Number One (PUR-1) model, and (2) develop a systematic, Green’s-function-guided procedure for boundary detector placement.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

An interlaboratory comparison of mid-infrared spectra acquisition: Instruments and procedures matter

Diffuse reflectance spectroscopy has been extensively employed to deliver timely and cost-effective predictions of a number of soil properties. However, although several soil spectral laboratories have been established worldwide, the distinct characteristics of instruments and operations still hamper further integration and interoperability across mid-infrared (MIR) soil spectral libraries. In this study, we conducted a large-scale ring trial experiment to understand the lab-to-lab variability of multiple MIR instruments. By developing a systematic evaluation of different mathematical treatments with modeling algorithms, including regular preprocessing and spectral standardization, we quantified and evaluated instruments' dissimilarity and how this impacts internal and shared model performance. We found that all instruments delivered good predictions when calibrated internally using the same instruments' characteristics and standard operating procedures by solely relying on regular spectral preprocessing that accounts for light scattering and multiplicative/additive effects, e.g., using standard normal variate (SNV). When performing model transfer from a large public library (the USDA NSSCKSSL MIR library) to secondary instruments, good performance was also achieved by regular preprocessing (e. g., SNV) if both instruments shared the same manufacturer. However, significant differences between the KSSL MIR library and contrasting ring trial instruments responses were evident and confirmed by a semi-unsupervised spectral clustering. For heavily contrasting setups, spectral standardization was necessary before transferring prediction models. Non-linear model types like Cubist and memory-based learning delivered more precise estimates because they seemed to be less sensitive to spectral variations than global partial least square regression. In summary, the results from this study can assist new laboratories in building spectroscopy capacity utilizing existing MIR spectral libraries and support the recent global efforts to make soil spectroscopy universally accessible with centralized or shared operating procedures.

58 GEOSCIENCES↗

Optimizing the use of pressurized bladders for the assembly of HL-LHC MQXFB magnets

The use of pressurized bladders for stress control of superconducting magnets was firstly proposed at Lawrence Berkeley National Laboratory in the early 2000s. Since then, the so-called ‘bladders and keys’ procedure has become one of the reference techniques for the assembly of high-field accelerator magnets and demonstrators. Exploiting the advantages of this method is today of critical importance for Nb$_{3}$Sn-based accelerator magnets, whose production requires the preservation of tight stress targets in the superconducting coils to limit the effects of the strain sensitivity and brittleness of the conductor. The present manuscript reports on the results of an experimental campaign focused on the optimization of the ‘bladders and keys’ assembly process in the MQXFB quadrupoles. These 7.2 m long magnets shall be among the first Nb$_{3}$Sn cryomagnets to be installed in a particle accelerator as a part of the High Luminosity upgrade of the LHC. One of the main practical implications of the bladders technique, especially important when applied to long magnets like MQXFB, is that to insert the loading keys, the opening of a certain clearance in the support structure is required. The procedure used so far for MQXF magnets involved an overstress in the coils during bladder inflation. The work presented here shows that such an overshoot can be eliminated thanks to additional bladders properly positioned in the structure. This optimized method was validated in a short model magnet and in a full-length mechanical model, becoming the new baseline for the series production at CERN. Furthermore, the results are supported by numerical predictions using finite element models.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Procedure for locating oil and gas wells in the Appalachian Basin

Locating undocumented (or poorly documented) oil and gas wells for environmental assessment is often difficult. Remnant features that confirm the presence of a well (intact casing/wellhead, well bore, etc.) are typically less than a meter in size and often are obscured from direct observation on the ground or from the air (by dense vegetation, for example). To efficiently find such features, it is useful to first systematically compile publicly available digital data at progressively smaller scales prior to embarking on field campaigns. Further, the information presented here describes the procedure developed and used by the U.S. Department of Energy's National Energy Technology Laboratory to locate potential oil and gas well sites for follow-up field verification and characterization. Digital data are first compiled from national and state resources such as well location/production databases, historical topographic maps, historical aerial photographs, and LiDAR data. Although each data set is likely to be incomplete or inaccurate to some extent, combining the data resources using geographic information system technology can generate potential well site targets with a higher degree of confidence, which improves the efficiency of fieldwork activities. This workflow was developed in the Appalachian Basin region, and although certain aspects may be unique, the general process would be applicable to locating undocumented wells in other regions.

54 ENVIRONMENTAL SCIENCES↗

HP in Cybersecurity: CyOTE

The U.S. Department of Energy’s (DOE) Office of Cybersecurity, Energy Security, and Emergency Response (CESER), through the Cybersecurity for the Operational Technology Environment (CyOTE) Program, worked with energy sector asset owners and operators (AOOs), partners, and Idaho National Laboratory (INL) to develop capabilities for AOOs to independently detect adversarial tactics, techniques, and procedures (TTPs) within their operational technology (OT) environments. Unlike the approach taken with commercial security solutions, CyOTE seeks to tie anomalies in cyber operations to a cyber-attack. By stringing together multiple techniques in the OT environment, AOOs can identify attack campaigns with ever decreasing impacts. The CyOTE methodology applies fundamental concepts of perception and comprehension to a universe of knowns and unknowns increasingly disaggregated into observables, anomalies, and triggering events. MITRE’s ATT&CK® Framework for Industrial Control Systems (ICS) is used as a common lexicon to identify a set of triggering events related to three Use Cases – Alarm Logs, Human-Machine Interface (HMI), and Remote Logins – which together account for 87 percent of the techniques commonly used by adversaries. The CyOTE methodology is also appropriate for OT-related anomalies perceived outside the three Use Cases, such as through the energy system itself.

99 GENERAL AND MISCELLANEOUS↗

CyOTE ASSET OWNER ENGAGEMENT – SIDE CHANNEL POWER ANALYSIS PROTOTYPE

The U.S. Department of Energy’s (DOE) Office of Cybersecurity, Energy Security, and Emergency Response (CESER), through the Cybersecurity for the Operational Technology Environment (CyOTE) Program, worked with energy sector asset owners and operators (AOOs), partners, and Idaho National Laboratory (INL) to develop capabilities for AOOs to independently identify adversarial tactics, techniques, and procedures (TTPs) within their operational technology (OT) environments. The CyOTE methodology seeks to identify adversarial techniques within an AOO OT environment that could result in physical disruptions to energy flow or damage to equipment. CyOTE provides a general roadmap for AOOs, starting from a triggering event, or the point in time and space they perceive an anomalous event or condition meriting investigation, and culminating when the AOO has sufficient confidence to make a business risk decision on the appropriate resolution. This paper outlines the results of one such engagement with the New York Power Authority (NYPA), where the CyOTE program partnered with an AOO to develop a design specification for a power side channel detector to identify anomalous changes to device load. It describes the goal of developing this capability, the development process, the challenges the technical teams faced and the future steps an AOO will need to take to install and use this detector in its OT environment.

99 GENERAL AND MISCELLANEOUS↗

Creating Hydride Rim Structures in Zircaloy 4 Cladding Tubes to Mimic High Burnup

During their long service in commercial light water reactors, zirconium alloy cladding tubes are subject to oxidation and subsequent hydrogen pickup which can degrade the materials mechanical properties [1]. These degradations can lead to premature cladding ruptures during reactor power transients [2] as well as negatively impact the claddings post quench ductility following high temperature steam oxidation in thermal hydraulic transients [3]. Hydrogen has low solid solubility in zirconium and usually precipitates as brittle zirconium hydride platelets in the cladding metal matrix. Due to temperature driven diffusion (Soret effect) and the grain texture of stress relieved zirconium metal tubes, these hydrides precipitate with a circumferential orientation near the outer surface of the cladding tubes forming a hydride rim which can serve as a site for crack initiation during circumferential ‘hoop’ loading of the cladding [4rim formation][5]. In order to better understand the effect of hydride rims on the fracture behavior of stress relieved zirconium alloy cladding tubes a procedure to produce these rim-like structures is being developed at Idaho National Laboratory (INL).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗