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At least 19 records

Sample Preparation Laboratory (SPL) Best Practices: CGD as the Primary Acceptance Method

The traditional paradigm applied to the construction of nuclear safety related systems, structures, and components (SSCs), like SPL, involves an owner/licensee hiring an EPC firm with an NQA 1 program to manage the engineering, procurement, and construction of the desired SSC. This traditional approach would have posed significant barriers to the successful completion of the SPL. As a smaller capital project, in the $\$$100–$\$$200 million range, there was concern that employing one of the larger EPC companies would escalate costs and extend the projected schedule beyond what would be feasible for the Department of Energy (DOE). The traditional acceptance method employed for nuclear facilities with credited safety functions requires the use of an EPC firm applying American Society of Mechanical Engineers (ASME) NQA 1 nuclear quality assurance (NQA) to accept safety SSCs. In lieu of this approach, INL elected to apply its own NQA 1 program to hire an EPC firm operating a commercial quality program. This method used commercial grade dedication (CGD) as outlined in NQA 1 which had not been applied at this scale. Use of the commercial supply chain was identified as a key factor to the successful completion of SPL. Favorable conditions enabling the use of CGD included: • INL serving as both the designer and the design authority • Design created by an NQA 1 qualified source • A mature CGD program • Availability of a CGD subject matter expert (SME) • A strong construction management program. This white paper elaborates on the methodology employed in the construction of the SPL, the successes achieved, and best practices implemented.

42 - ENGINEERING↗

Optical vibrational spectroscopic signatures of ammonium diuranate process parameters

Ammonium diuranate (ADU) is commonly encountered in the nuclear fuel cycle; however, previous investigations have shown that ADU is a complex mixture of distinct compounds. Moreover, production parameters are known to heavily influence the composition of the resulting ADU. Here, we examine four samples of ADU prepared at Oak Ridge National Laboratory (ORNL), and one sample of ADU made at Pacific Northwest National Laboratory (PNNL), with the goal of further characterizing and elucidating the effect of processing parameters such as stir rate, strike direction, and temperature on material composition. Process parameters during ADU precipitation at ORNL and PNNL were well documented, and we relate process variables to optical vibrational spectroscopic signatures observed using Raman and infrared (IR) spectroscopy. In addition, powder X-ray diffraction (PXRD) reveals differences in the solid-phase composition of ADU precipitates, but we find that the primary phase is similar to the uranyl oxyhydroxyhydrate mineral metaschoepite. Despite the significant phase contributions of a metaschoepite-like phase, spectroscopic evidence of both nitrate and ammonium are observed for all samples. To gain a more holistic understanding of spectroscopic features of process parameters in ADU, principal component analysis (PCA) is employed and results in observable signatures that relate to the stir rate used during synthesis. These results provide further information about the process-dependence of ADU precipitate composition.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Reproducibility of Radiokrypton in Deep Desert Aquifers: Insights from a Decade of Research

Great technical advances have been achieved since the first atom-trap trace analysis (ATTA) -based radiokrypton application in Egypt, where 1 Myr old groundwater was discovered. Beyond advances in ATTA measurement capabilities, including reduction in sample size, analysis duration, and analytical uncertainty, major progress has been achieved over the past two decades in the sample collection and preparation techniques. These advances paved the expansion of ATTA-based noble gas applications to many other aquifers worldwide, illuminating the nature and flow pattern of deep groundwater systems. While the potential of this new analytical technique for old groundwater dating is well recognized, another important aspect yet to be examined is the reproducibility of radiokrypton in aquifers over time, i.e., how representative is a discrete groundwater sample, collected at a specific time and location, for the natural groundwater system? The likelihood of a negative answer is increased by flow-field disturbance in aquifers following massive groundwater abstraction. Here, in this work, we present repeated 81 Kr sampling and measurements in twenty-one sites over Israel, mostly of deep (up to 1 km) wells tapping confined aquifers in the arid to hyperarid Negev desert. The results demonstrate that radiokrypton measurements are indeed reproducible, even in cases where samples were collected as long as nine years apart and from highly productive (∼1 Mm 3 /yr order) pumping wells. Furthermore, many of the repeated measurements in this study (17 out of the 21 sites) were conducted with different ATTA Instruments in two different laboratories using slightly different sampling, preparation, and analysis techniques, yet with an overall good agreement. The consistency in the ATTA-based 81 Kr-dating results over time highlights the robustness of this state-of-the-art technique as a tool to unravel groundwater flow patterns and encourages further applications to many other yet-to-be-explored deep aquifers.

atom-trap trace analysis↗

October 2024 Semiannual Composite Salt Waste Processing Facility (SWPF) Decontaminated Salt Solution (DSS) Toxicity Characteristic Leaching Procedure (TCLP) Results

The aqueous waste from the Salt Waste Processing Facility (SWPF) is sampled semiannually for transfers to the Saltstone Production Facility (SPF). Salt solution is treated at SPF and disposed of in the Saltstone Disposal Facility (SDF). Per request of customer, X-TTR-Z-00027, Revision 0, one SDF waste form (saltstone) sample was prepared in the Savannah River National Laboratory (SRNL) from the SWPF Decontaminated Salt Solution (DSS) Waste Acceptance Criteria (WAC) sample and Z-area premix material for the October 2024 semiannual Toxicity Characteristic Leaching Procedure (TCLP) sample. The sample contained 60:40 (by weight) of slag and fly ash (referred to as the “Cement-Free grout sample”). Results from the technical report support Task 2: ‘Grout Leaching Analyses’ of the Task Technical Request (TTR) prepared by Savannah River Mission Completion (SRMC). At 64 days cured, a sample of the SDF waste form was collected and shipped to a certified laboratory for analysis using the Toxicity Characteristic Leaching Procedure (TCLP). The October 2024 semiannual Cement-Free grout sample met the South Carolina (SC) Code of Regulations for Hazardous Waste Management Regulations (HWMR) 61-79.261.24 and 61-79.268.48 requirements for a non-hazardous waste form with respect to the Resource Conservation and Recovery Act (RCRA) metals and Underlying Hazardous Constituents (UHCs), and met the SPF WAC that was in effect at the time of the sample collection at SWPF.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

April 2024 Semiannual Composite Salt Waste Processing Facility (SWPF) Decontaminated Salt Solution (DSS) Toxicity Characteristic Leaching Procedure (TCLP) Results

The aqueous waste from the Salt Waste Processing Facility (SWPF) is sampled semiannually for transfers to the Saltstone Production Facility (SPF). Salt solution is treated at SPF and disposed of in the Saltstone Disposal Facility (SDF). Per request of customer, X-TTR-Z-00027, Revision 0, one SDF waste form (saltstone) sample was prepared in the Savannah River National Laboratory (SRNL) from the SWPF Decontaminated Salt Solution (DSS) Waste Acceptance Criteria (WAC) sample and Z-area premix material for the April 2024 semiannual Toxicity Characteristic Leaching Procedure (TCLP) sample. The sample contained 60:40 (by weight) of slag and fly ash (referred to as the “Cement-Free grout sample”). Results from the technical report support Task 2: ‘Grout Leaching Analyses’ of the Task Technical Request (TTR) prepared by Savannah River Mission Completion (SRMC). After at least 28 days cured, a sample of the SDF waste form was collected and shipped to a certified laboratory for analysis using the Toxicity Characteristic Leaching Procedure (TCLP). The April 2024 semiannual Cement-Free grout sample met the South Carolina (SC) Code of Regulations for Hazardous Waste Management Regulations (HWMR) 61-79.261.24 and 61-79.268.48 requirements for a non-hazardous waste form with respect to the Resource Conservation and Recovery Act (RCRA) metals and Underlying Hazardous Constituents (UHCs), and met the SPF WAC that was in effect at the time of the tank sampling.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Advanced Method Optimization with Categorical and Constrained Continuous Parameters

Traditional approaches to analytical method optimization (e.g., univariate and “guess-and-check”) can be time-consuming, costly, and often fail to identify true optima within the parameter space. Previous work defined and implemented a generalized technique for method optimization for continuous method parameters, but a knowledge gap remains for the incorporation of categorical variables into these advanced method optimization schemes. This work presents and validates a generalized optimization approach that incorporates both continuous and categorical variables while also utilizing a multivariate, multiobjective optimization scheme with Karush–Kuhn–Tucker conditions to bound the optimization space to solutions within the physical limitations of the parameter space. Method optimization from a case study using GC–MS for the analysis of 11 analytical standards with objectives to minimize peak width and maximize peak height resulted in a 3 orders of magnitude improvement in the average peak height and a 2 orders of magnitude improvement in the average peak width compared to the least optimal (but reasonable) instrumental parameters utilized in this study. This approach to optimization allows for a customizable method optimization in which users can include both continuous and categorical variables to achieve objectives specific to their analytical goals. This approach significantly reduces the labor and cost associated with traditional method development approaches and can be applied in a variety of scientific fields across a range of laboratory techniques (e.g., instrument method development, sample preparation, and extraction techniques).

Amorphous materials↗

OPCW Twining Project Visit by the National Laboratory of Scientific and Technical Police (LNPST) to Lawrence Livermore National Laboratory Forensic Science Center (LLNL)

PURPOSE FOR TRIP Through the Organisation for Prohibition of Chemical Weapons (OPCW) Twinning and Assistance Program, Lawrence Livermore National Laboratory, Forensic Science Center (LLNL) has been paired with Morocco’s National Laboratory of Scientific and Technical Police (LNPST), with the goal of mentoring LNPST to become an OPCW Designated Laboratory. The purpose of this visit was for LLNL staff to mentor staff from LNPST as they participated in hands-on, laboratory-based exercises to analyze proficiency test samples prepared by LLNL. This visit was designed to help LNPST scientists strengthen their skills in OPCW proficiency testing.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

Establishing In-House Titration Capabilities: Part I. Hydroxyl Group Titration through Acetic Anhydride Acetylation

This lessons learned document provides a detailed analysis of the hydroxy termination titration methods employed for determining hydroxyl group content in various chemical samples. The primary focus is on the evaluation of techniques such as ASTM E222 and their practical applications in laboratory settings. Through examination of method selection, sample preparation, and titration execution, key insights have been identified that enhance the accuracy and reliability of results. Notable findings include the advantages of using pressure bottle methods for improved heating uniformity and reduced solvent loss, as well as the challenges associated with endpoint detection in dark-colored solutions. Recommendations for alternative sampling and titration techniques are proposed to address these challenges. This document serves as a valuable resource for enhancing the effectiveness and efficiency of hydroxy termination titration methods in chemical analysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A New Method for Polishing Laminated Dissimilar Metals

Here, this paper presents a novel method for preparing metallographic samples of laminated dissimilar metals, specifically a layered structure of zirconium (Zr), vanadium (V), and tungsten (W), which pose a challenge due to their differing crystal structures and hardness levels. The work was motivated by the need to develop a cladding for tungsten targets in spallation neutron sources, where a zirconium face is applied over an interlayer of either vanadium or titanium to prevent the formation of brittle intermetallic compounds such as ZrW 2 . Traditional polishing techniques prove inadequate because each constituent metal requires a different polishing approach based on its unique material properties. The methodology outlined includes a sequential process involving conductive epoxy mounting, successive grinding and polishing with specific abrasives, and a final chemical-mechanical polish using a colloidal silica-based solution. Optical microscopy confirmed that this multi-step process successfully produced scratch-free surfaces and minimized surface relief across the different metal interfaces. Although developed for refractory metals, this approach shows promise for other layered structures comprised of transition metals, offering a meticulous yet effective technique for high-quality metallographic sample preparation.

Newberry, Daniel [Oak Ridge National Laboratory (O↗

April 2025 Semiannual Composite Salt Waste Processing Facility (SWPF) Decontaminated Salt Solution (DSS) Toxicity Characteristic Leaching Procedure (TCLP) Results

The aqueous waste from the Salt Waste Processing Facility is sampled semiannually for transfers to the Saltstone Production Facility. Salt solution is treated at the Saltstone Production Facility and disposed of in the Saltstone Disposal Facility. Per request of customer, X-TTR-Z-00027, Revision 0, one Saltstone Disposal Facility waste form was prepared at Savannah River National Laboratory using the Salt Waste Processing Facility Decontaminated Salt Solution and Z-area premix material for the April 2025 semiannual Toxicity Characteristic Leaching Procedure sample. The sample contained 60:40 (by weight) of slag and fly ash (referred to as the “Cement-Free grout sample”). Results from the technical report support Task 2: ‘Grout Leaching Analyses’ of the Task Technical Request prepared by Savannah River Mission Completion. At 43 days cured, the Saltstone sample was collected and shipped to a certified laboratory for analysis using the Toxicity Characteristic Leaching Procedure. The April 2025 semiannual Cement-Free grout sample met the South Carolina Code of Regulations for Hazardous Waste Management Regulations 61-79.261.24 and 61-79.268.48 requirements for a non-hazardous waste form with respect to the Resource Conservation and Recovery Act metals and Underlying Hazardous Constituents, and met the Saltstone Production Facility Waste Acceptance Criteria that was in effect at the time of the sample collection at the Salt Waste Processing Facility.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Interlaboratory comparison of secondary ion mass spectrometry analysis results from the 7th international technical nuclear forensics working group collaborative material exercise

A review and interlaboratory comparison of secondary ion mass spectrometry (SIMS) data obtained by laboratories participating in the International Technical Nuclear Forensics Working Group (ITWG) 7th Collaborative Material Exercise (CMX-7) has been conducted. The analyzed materials were two uranium compounds in powder form and two pieces of uranium metal. The instruments used in this comparison were a small-geometry (SG) SIMS, CAMECA IMS 7f from the Research Centre Rez, and a large-geometry (LG) SIMS, CAMECA IMS 1280 from Los Alamos National Laboratory. Despite the differences in instruments and analytical procedures, e.g., sample preparation, SIMS setups, and data post-processing, there was good agreement for the 234 U/ 238 U, 235 U/ 238 U, and 236 U/ 238 U ratios in the analyzed materials. The main difference was in the precision, which was, as expected, higher for the LG-SIMS. In addition, a comparison between the laboratories was also made for the image processing algorithms applied to raw data acquired in automated particle measurement (APM) mode. In conclusion, the result of this comparison has led to identification of best practices for setting up parameters of the APM software.

and nuclear chemistry↗

A new capability facilitating nuclear materials research: the Activated Materials Laboratory at the Advanced Photon Source

The Activated Materials Laboratory (AML), located in the Long Beamline Building (LBB) of the Advanced Photon Source (APS) of Argonne National Laboratory (ANL), serves as a centralized radiological facility for preparing radioactive samples for APS beamline experiments. The AML is equipped to receive shipments, handle open-form radioactive materials, encapsulate samples, and transport samples to-and-from beamline end-stations. The AML works closely with users and the APS radiological safety committee to make sure the safe conduct of experiments.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Characterization of Tank 9H Annulus Sample in Support of Residual Material Inventory Determinations

The Savannah River National Laboratory (SRNL) was requested by Savannah River Mission Completion (SRMC) to provide sample preparation and characterization of the Tank 9H annulus sample in support of Residual Material Inventory Determinations. One Tank 9H sample in three vials [HTF-9-25-13, HTF-9-25-14 and HTF-9-25-15], with each vial containing approximately 200 mL of the Tank 9H annulus salt solution, were delivered to the SRNL Shielded Cells for sample preparation and characterizations in February 2025. The density of the “as-received” solution contained in each of the three Tank 9H annulus sample vials were determined followed by a solid-liquid separation on each one using 0.45-micron Nalgene® nylon filter membranes. The resulting filtrates were combined to form the Tank 9H annulus sample with a total volume of about 600 mL. The combined wet solid fractions, about a total of 4.8 grams of salt material, remaining on the filter membranes were air-dried in the Shielded Cells for 72 hours. The total weight of the air-dried solids was 2.1 grams. These air-dried solids were washed with deionized water (DI water) at a phase ratio of 60 mL DI water/gram of solids to recover insoluble solids, if any. No visible or measurable quantity of insoluble solids were recovered after DI water washing of the air-dried solids because the air-dried solids completely dissolved in the DI water. The solid fraction-wash water was not combined with the 600 mL of the filtrate solution, and the resulting solution was not screened or analyzed for radionuclides. Aliquot sample volumes of the undiluted Tank 9H annulus sample were sent to the SRNL analytical services groups for radionuclides, elementals, anions and total mercury analysis by various methods including radiochemical separations/counting methods, inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) and special preparations. All sample analyses were performed in triplicate. This report presents the analytical characterization results for the Tank 9H annulus sample. The results are also reported where analytical methods yielded additional analytes, other than those requested by SRMC. In the characterization of the Tank 9H annulus sample, the detection limits for all the analytes, as specified in the Technical Task Request (TTR) and Task Technical and Quality Assurance Plan (TTQAP), were met.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Characterization of Tank 15H Sample in Support of Preliminary Cease Waste Removal and Closure Mode Determination

The Savannah River National Laboratory (SRNL) was requested by Savannah River Mission Completion (SRMC) to provide sample preparation and analysis of Tank 15H characterization samples. These samples follow an interest in exploring avenues to condense the extensive sampling of the Tank Closure process. One such pathway would be to collect a sample during an earlier waste removal campaign for analysis to determine comparability to the later residual tank inventory determined through Residual Material sampling and characterization prior to grouting. Six Tank 15H samples (HTF-15-24-9, HTF- HTF-15-24-10, HTF-15-24-11, HTF-15-24-12, HTF15-24-13, and HTF-15-24-14) were delivered to SRNL in May of 2024. These six Tank 15H samples were taken as close as possible to the solids layer of the Tank 15H. These six Tank 15H samples were combined to form one composite sample for characterization due to the lack of sufficient solids fraction.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

FY 2024 Multidimensional Data Correlation Platform Data Management Infrastructure Progress: Materials Laboratory

This report provides an inventory of the equipment available at the ORNL Manufacturing Demonstration Facility (MDF) for sample preparation and material characterization, including both destructive and non-destructive techniques that generate critical data to support the development of the Multi-Dimensional Data Correlation (MDDC) framework. The success of the MDDC framework depends heavily on the quality and completeness of the data it can access. Therefore, it is essential to establish a comprehensive inventory of the technologies available to the Advanced Materials and Manufacturing Technologies (AMMT) multi-laboratory team. This starts by gathering information about the types of data they produce, the data collection and transfer protocols used, file formats, and data storage requirements for experiments. This information is then carefully evaluated to create the operations and trackables elements of the Damara Tern platform, which is the foundation of the MDDC framework.

36 MATERIALS SCIENCE↗

Compositional Homogeneity in Rapidly Solidified 316L stainless steel produced by laser powder-bed fusion processing

The segregation of alloying elements in rapidly solidified 316L stainless steel produced using additive manufacturing technologies is widely reported throughout literature. The microstructure of thin walls manufactured from 316L stainless steel using laser powder bed fusion are examined for the presence of alloy segregation, i.e. the rejection of solutes to grain boundaries. Metallographic methods including mechanical polishing and chemical etching are used to prepare samples for microanalysis m

Jankowski, Alan F. [Sandia National Laboratories (↗

Simultaneous Determination of Halogens and Metals in Waste Plastic Pyrolysis Oil by Inductively Coupled Plasma Mass Spectrometry

A major barrier to integrating pyrolysis-derived oil into conventional refinery technology is the presence of impurities, particularly halogens and metals, that can deactivate catalysts. This study presents a novel, cost-effective approach for the simultaneous analysis of a subset of halogens, metals, nonmetals, and metalloids in complex, industrially relevant distilled pyrolysis oil samples, this was previously achievable only through multiple techniques. Excellent results were obtained using a widely accessible inductively coupled plasma mass spectrometry (ICP-MS) method with helium gas mode and standard laboratory consumables, enabling high-throughput analysis and efficient evaluation of adsorbent performance. Sample preparation is straightforward, requiring only dilution in a compatible matrix, and provides accurate and precise quantification, with 75%–137% spike recovery for Be, Ti, V, Cr, Fe, Ni, Co, Cu, As, Se, Mo, Cd, Sb, Tl, and Pb, and 62%–65% spike recovery for Cl and 109%–133% spike recovery for Br. Additionally, an enhanced version of the method using ICP-MS/MS and hydrogen gas is described, which has higher accuracy with 69%–112% spike recovery for Be, B, Ti, V, Fe, Co, Ni, Cu, As, Se, Mo, Cd, Sb, Tl, and Pb, with 85%–102% spike recovery for Cl and 63%–93% spike recovery for Br. Helium mode detection limits for industrially relevant elements (V, Fe, Ni, Cu, As, and Pb) are less than 1.7 µg/kg, and less than 0.2 mg/kg for Br and Cl. Furthermore, this methodology facilitates rapid systematic evaluation of adsorption capacities of materials under time-on-stream conditions and supports robust comparisons across diverse operating environments.

Lazarcik, James [University of Wisconsin-Madison, ↗

Creep suppression and fatigue in bio-based composites manufactured via conventional and large format additive manufacturing processes

The emergence of novel extrusion-based additive manufacturing (AM) processes has prompted the development of new thermoplastic composite feedstocks, and broadening sustainability initiatives have driven the development of bio-based and recyclable material for AM feedstocks. Poly(lactic acid) (PLA) with wood flour (WF) is one composite system that has been demonstrated in numerous AM applications, as well as traditional processing methods (i.e., compression and injection molding); however, there has been a need to understand how the variation in processing methodology impacts the material performance of these bio-based feedstocks from a fundamental perspective, with particular emphasis on creep for an extended application use-life. Herein, PLA/WF is explored as a feedstock material for large format additive manufacturing (LFAM) and the performance of additively manufactured materials is compared to those produced via more traditional processing methods. It is also demonstrated that the addition of WF decreases the material’s coefficient of thermal expansion (CTE) while increasing its Young’s modulus, susceptibility to water uptake, and creep fatigue resistance. Essentially, the addition of 20 wt% WF results in a 92 % decrease in rubbery regime CTE while simultaneously resulting in a 14 % increase in modulus, 190 % increase in water uptake, and a 31 % decrease in residual strain after cyclic creep tests. The processing method was also found to play a large role in the final part performance, with the printed material increasing the crystallinity by 183 % and 214 % compared to its compression and injection molded counterparts. Furthermore, the porosity of printed samples increased by two orders of magnitude compared to samples prepared via traditional processing methods.

36 MATERIALS SCIENCE↗