Methods for preparation of low mass chlorine samples for planetary and space science applications
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Tank Waste Characterization: History, Challenges, and Success Stories
The preparation and chemical and radiochemical analysis of Hanford tank waste samples can be performed with standard laboratory equipment and instruments as relatively routine processes that are not particularly challenging. Rather, the main challenges of tank waste characterization are associated with radiological dose and sampling limitations. Accurate, representative and effective sampling techniques are difficult with the waste tanks because they were not designed for routine sampling. There are a finite number of sampling locations for each tank based on riser positioning, depth and the operational functionality of the sampling riser. For example, in one recently emptied SST, there was one riser that was found to have had concrete dumped down it, thereby eliminating that sampling port. Additionally, the waste within the tank; especially true for the saltcake and sludge, is not homogenous. The ability to adequately mix a million-gallon double shell tank (DST) is a concern for data reproducibility. Another real challenge that must be addressed for sampling single shell tanks, is how to dissolve the salt cake waste in a compromised (leaking) SST. These physical constraints mean that uncertainty in the representativeness of samples must be considered when applying analytical results to the bulk contents of the tank. The tank waste is highly radioactive and thus can only be handled initially by facilities that can receive samples into concrete-shielded hot cells with remote operation with an example provided in Figure 1. The shielding protects the worker from the radiological dose while mineral oil windows and remotely operated manipulators enables the samples to be handled. At Hanford, analytical laboratories with these hot cell capabilities are limited to the Pacific Northwest National Laboratory and the main Hanford operations support laboratory, 222-S Laboratory. Because of their highly radioactive nature, samples must be sufficiently diluted to facilitate their analysis outside of a shielded cell. In some cases, this means some accuracy must be compromised to complete the analysis beyond that normally encountered for non-radioactive material.
Waste Characterization, BBI, PHOENIX: Tank Farms: ↗
233 U(n,$\gamma$) measurements at LANSCE [Slides]
A new measurement at LANSCE combined DANCE and NEUANCE at the end of 2020 and 2021. The 233 U material was provided by Oak Ridge National Laboratory (December 2020).Two samples of 10 mg and 20 mg of 233 U have been prepared at LANL by Evelyn M. Bond (December 2020). The experiment was performed in December 2020 and June/July 2021. Data analysis is ongoing to extract capture data knowing fission. LANL is looking forward to delivering the capture/fission ratio from (1-300) keV by the end of the FY2022.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
233 U(n,$\gamma$) measurements at LANSCE [Slides]
A new measurement at LANSCE combined DANCE and NEUANCE at the end of 2020 and 2021. The 233 U material was provided by Oak Ridge National Laboratory (December 2020).Two samples of 10 mg and 20 mg of 233 U have been prepared at LANL by Evelyn M. Bond (December 2020). The experiment was performed in December 2020 and June/July 2021. Data analysis is ongoing to extract capture data knowing fission. LANL is looking forward to delivering the capture/fission ratio from (1-300) keV by the end of the FY2022.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Flash electropolishing for TEM: Reducing FIB‐induced defects in tungsten with protocols for new materials
Focused ion beam (FIB) milling has become the dominant approach for site-specific transmission electron microscopy (TEM) specimen preparation; however, FIB damage remains a critical limitation for reliable microstructural characterisation, particularly in radiation effects studies. Tungsten is especially susceptible to FIB damage due to its high nuclear stopping power, which promotes the formation and strong diffraction contrast of FIB-induced ‘black spot’ defects that are indistinguishable from very fine irradiation-induced loops/defects resulting from low to intermediate temperature neutron irradiation. In this work, flash electropolishing is systematically evaluated as a post-FIB treatment for minimising preparation-induced artefacts for TEM analysis of tungsten-based alloys. Using a range of non-, ion-, and neutron-irradiated tungsten materials, the effectiveness of flash electropolishing has been assessed through direct comparison with conventional FIB and plasma-FIB preparation including low-energy Ga, Ar, Xe ion cleaning. The results demonstrate that flash electropolishing effectively removes FIB-damaged layers and ‘black spot’ defects, thereby enabling reliable observation of irradiation-induced dislocation structures. Key processing parameters governing flash electropolishing quality – including lamella thickness, applied voltage, polishing duration, electrolyte chemistry, and cathode geometry – have been systematically evaluated, and clear criteria were established for determining when flash electropolishing is required to ensure reliable microstructural analysis. This work also provides practical guidance for implementing flash electropolishing as an artefact-controlled specimen-preparation approach for TEM characterisation of FIB-produced specimens. The systematic protocol can be extended to other, non-tungsten materials.
TEM sample preparation↗
Lawrence Livermore National Laboratory Experimental Test Site 300 (Site 300): Site 300 Roadway Improvements - Chem Mag Loop Soil Sampling and Analysis Plan (May 2023)
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 Roadway Improvements Project at the Chem Mag Loop (project). The purpose of the SAP is 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. This SAP follows criteria established in Lawrence Livermore National Laboratory’s (LLNL) Soils Screening and Management Plan (SSMP) (LLNL 2022), which was formalized in accordance with U.S. Environmental Protection Agency (EPA) guidance for developing Data Quality Objectives for environmental data (EPA 2006) and the Multi-Agency Radiation Survey and Site Investigation Manual (MARSSIM) guidance (U.S. NRC, U.S. EPA, U.S. DOE, and U.S. DOD 2000). The scope of this SAP is based on preliminary design information provided to EFA by PMO.
54 ENVIRONMENTAL SCIENCES↗
Sample Preparation Method for Low-Level Total 129 I Measurements by ICP-MS
Trace-level measurements of iodine’s isotopic ( 129 I and 127 I) and chemical species distributions are needed for an accurate understanding of radioiodine migration in the Hanford subsurface. Pacific Northwest National Laboratory (PNNL) previously developed a novel analytical method for iodine characterization that uses ion chromatography (IC) coupled to inductively coupled mass spectrometry (ICP-MS). While the method can measure speciated forms of 129 I at levels below the drinking water standard, an interference from molybdenum (Mo) prevents the assay from quantifying the $\underline{total}$ 129 I concentration in many Hanford sample matrices. In this work, solvent extraction was evaluated as a sample preparation method for eliminating the Mo interference. A series of 10 experiments was conducted in which solutions containing known amounts of iodate or iodide were treated by solvent extraction, and the extracted solutions were analyzed for total iodine concentrations by ICP MS. Several extraction parameters such as reagent concentrations and chemical reaction times were systematically adjusted in attempts to optimize the extraction process. While solvent extraction was shown to be effective at removing Mo, there was a consistent inability to recover more than approximately 75% of the total iodine in most experiments. This would reduce the ability to detect 129 I at levels near the drinking water standard. Additionally, the extraction efficiencies in several experiments were highly variable, suggesting that solvent extraction could add significant uncertainty to radioiodine measurements. We recommend evaluating ion exchange as an alternative sample preparation approach in fiscal year (FY) 2024.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Utah FORGE: Powder X-ray Diffraction Data from Well 16A(78)-32 Core
This dataset from Lawrence Livermore National Laboratory (LLNL) consists of four raw X-ray diffraction (XRD) scans and preliminary results of quantitative XRD analysis. The scanned samples were prepared from four subcores, which came from various depths of the FORGE well 16A(78)-32 core. Desired core lengths were selected from available core photos (on GDR), provided by FORGE personnel, and subcored at LLNL. The XRD scans were collected in May 2023 at LLNL as pre-experimental characterization data for these subcores, which will be used in core-flooding experiments at LLNL and in triaxial direct shear experiments at Los Alamos National Laboratory as part of DOE Project 5-2428. XRD scans are in RAW file format (e.g., FORGE-5477-full.raw) and are suitable for viewing and analysis using open-source quantitative XRD software (e.g., Profex; www.profex-xrd.org ) and/or other proprietary instrument software.
15 GEOTHERMAL ENERGY↗
Toward Automated Plasma Focus Ion Beam Instrument Calibration for Materials Processing [Poster]
To accelerate the transition to autonomous focused ion beam (FIB) microscopy, we require an objective figure of merit (FOM) for assessing calibration. For our purposes, these FOMs related to beam astigmatism, quad, and focus. Intelligent calibration integrated into scripted workflows will enable fully automated sample preparation workflows that produce higher quality samples with less operator time.
97 MATHEMATICS AND COMPUTING↗
Neutron capture of UO 2 targets prepared by spin-coating assisted combustion synthesis
Two uranium dioxide (UO 2 ) targets of (414 ± 23) nm and (1092 ± 93) nm thicknesses were prepared on 6061 aluminum alloy and puratronic grade aluminum backing materials. The targets were deposited with a novel method combining spin coating and solution combustion synthesis (SCS). The target layers consisted of small (3–7 nm) UO 2 grains and uniformly distributed ultra-small (1–3 nm) pores. The prepared targets were tested at the Los Alamos National Laboratory’s LANSCE facility for neutron irradiation damage and suitability for neutron capture experiments. The samples showed no signs of target material loss after the irradiation. However, irradiation caused a significant increase in the grain size (4–10 nm), as well as upward mass diffusion and coalescence of the pores due to the thermal spikes. The magnesium in the aluminum 6061 alloy backing also diffused into the UO 2 layer during neutron irradiation. The structural changes in the target after the irradiation do not affect the data from neutron capture. As a result, the new method can be used more broadly to prepare other actinide targets for nuclear physics experiments.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Robust surfactant-assisted one-pot sample preparation for label-free single-cell and nanoscale proteomics
With advanced mass spectrometry (MS)-based proteomics, genome-scale proteome coverage can be achieved from bulk cells. However, such bulk measurement obscures cell to cell heterogeneity, precluding proteome profiling of single cells and small numbers of cells of interest. To address this issue, in recent 5 years there are a surge of small sample preparation methods developed for robust effective collection and processing of single cells and small numbers of cells for in-depth MS-based proteome profiling. Based on their broad accessibility, they can be categorized into two types: specific device- and standard PCR tube- or multi-well plate-based methods. Herein we describe the detailed protocol of our recently developed, easily adoptable, Surfactant-assisted One-Pot (SOP) sample preparation coupled with MS method termed SOP-MS for label-free single-cell and nanoscale proteomics. SOP-MS capitalizes on the combination of a MS-compatible surfactant, DDM (n-Dodecyl-ß-D-maltoside), and standard low-bind PCR tube or multi-well plate for ‘all-in-one’ one-pot sample preparation without sample transfer. With its robust and convenient features, SOP-MS can be readily implemented in any MS laboratory for single-cell and nanoscale proteomics. With further improvements in MS detection sensitivity and sample throughput, we believe that SOP-MS could open an avenue for single-cell proteomics with broad applicability in the biological and biomedical research.
Single-cell proteomics, nanoscale proteomics, SOP-↗
October 2025 Semiannual Composite Salt Waste Processing Facility Decontaminated Salt Solution Toxicity Characteristic Leaching Procedure Results
The aqueous waste from the Salt Waste Processing Facility is sampled semiannually for transfers to the Saltstone Disposal 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 Processing Facility Decontaminated Salt Solution and Z area premix material for the October 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 51 days cured, the Saltstone sample was collected and shipped to a certified laboratory for analysis using the Toxicity Characteristic Leaching Procedure. The October 2025 Semiannual Cement-Free grout sample met 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.
Hsieh, Madison [Savannah River National Laboratory↗
VitroJet: new features and case studies
Single-particle cryo-electron microscopy has become a widely adopted method in structural biology due to many recent technological advances in microscopes, detectors and image processing. Before being able to inspect a biological sample in an electron microscope, it needs to be deposited in a thin layer on a grid and rapidly frozen. The VitroJet was designed with this aim, as well as avoiding the delicate manual handling and transfer steps that occur during the conventional grid-preparation process. Since its creation, numerous technical developments have resulted in a device that is now widely utilized in multiple laboratories worldwide. It features plasma treatment, low-volume sample deposition through pin printing, optical ice-thickness measurement and cryofixation of pre-clipped Autogrids through jet vitrification. This paper presents recent technical improvements to the VitroJet and the benefits that it brings to the cryo-EM workflow. A wide variety of applications are shown: membrane proteins, nucleosomes, fatty-acid synthase, Tobacco mosaic virus, lipid nanoparticles, tick-borne encephalitis viruses and bacteriophages. These case studies illustrate the advancement of the VitroJet into an instrument that enables accurate control and reproducibility, demonstrating its suitability for time-efficient cryo-EM structure determination.
59 BASIC BIOLOGICAL SCIENCES↗
Salt mass determination by 22 Na-based radioactive tracer dilution of a highly radioactive molten salt system for pyroprocessing spent oxide nuclear fuels
To demonstrate the feasibility of the 22 Na-based radioactive tracer dilution (RTD) for determining the total salt mass in a 60-kg oxide reduction (OR) system at Idaho National Laboratory (INL) for pyroprocessing spent oxide nuclear fuels, a LiCl- 22 NaCl tracer salt was prepared and spiked to the OR vessel, and salt samples were analyzed by gamma spectroscopy. Due to the high radioactivity (around 10 mCi/g) of the OR salt, mainly from 137 Cs, traditional gamma spectroscopy methods, which typically involve diluted salt samples, was not effective for analyzing the RTD samples. Since the 22 Na tracer radioactivity was very low, undiluted samples were necessary to detect the small amount of 22 Na tracer. Here, despite the high gamma radioactivity of the OR salt, increasing the detector-sample distance from 20 cm to 40 cm during gamma spectroscopy allowed the detection of radioactivity as low as 0.12 µCi/g 22 Na. The preparation of the 22 NaCl-LiCl tracer salt suitable for spiking into the OR salt was successful, and the mass determined by RTD was consistent with that estimated by salt level measurement. Therefore, the 22 Na-based RTD technique for total mass determination of the 60-kg molten salt system for OR is feasible, though more development work, particularly in the improving the uncertainty, is needed .
11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Sample Preparation and Analysis at IMCL - Internship Poster
Poster for the intern poster session on August 7th
11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Technical note: Optimizing the in situ cosmogenic 36 Cl extraction and measurement workflow for geologic applications
Abstract. In situ cosmogenic 36Cl analysis by accelerator mass spectrometry (AMS) is routinely employed to date Quaternary surfaces and assess rates of landscape evolution. However, standard laboratory preparation procedures for 36Cl dating require the addition of large amounts of isotopically enriched chlorine spike solution; these solutions are expensive and increasingly difficult to acquire from commercial sources. In addition, the typical workflow for 36Cl dating involves measuring both 35Cl/37Cl and 36Cl/Cl concurrently on the high-energy (post-accelerator) end of the AMS system, but 35Cl/37Cl determinations using this technique can be complicated by isotope fractionation and system memory during measurement. The traditional workflow also does not provide 36Cl extraction laboratories with the data needed to calculate native Cl concentrations in advance of 36Cl/Cl measurements. In light of these concerns, we present an improved workflow for extracting and measuring chlorine in geologic materials. Our initial step is to characterize 35Cl/37Cl on sample aliquots of up to ∼1 g prepared in Ag(Cl, Br) matrices, which greatly reduces the amount of isotopically enriched spike solution required to measure native Cl content in each sample. To avoid potential issues with isotope fractionation through the accelerator, 35Cl/37Cl is measured on the low-energy, pre-accelerator end of the AMS line. Then, for 36Cl/Cl measurements, we extract Cl as AgCl or Ag(Cl, Br) in analytical batches with a consistent total Cl load across all samples; this step is intended to minimize source memory effects during 36Cl/Cl measurements and allows the preparation of AMS standards that are customized to match known Cl contents in the samples. To assess the efficacy of this extraction and measurement workflow, we compare chlorine isotope ratio measurements on seven geologic samples prepared using standard procedures and the updated workflow. Measurements of 35Cl/37Cl and 36Cl/Cl are consistent between the two workflows, and 35Cl/37Cl values measured using our methods have considerably higher precision than those measured following standard protocols. The chemical preparation and measurement workflow presented here (1) reduces the amount of isotopically enriched chlorine spike used per rock sample by up to 95 %; (2) identifies rocks with high native Cl concentrations, which may be lower priority for 36Cl surface exposure dating, at an early stage of analysis; and (3) allows laboratory users to maintain control over the total chlorine content within and across analytical batches. These methods can be incorporated into existing laboratory and AMS protocols for 36Cl analyses and will increase the accessibility of 36Cl dating for geologic applications.
58 GEOSCIENCES↗
Residual resistance ratio measurement system for Nb 3 Sn wires extracted from Rutherford cables
Residual resistance ratio (RRR) of superconducting strands is an important parameter for magnet electrical stability. RRR serves as a measure of the low-temperature electrical conductivity of the copper within a conductor that has a copper stabilization matrix. For Nb 3 Sn, due to the need of a reaction heat treatment, the technical requirements for high quality measurements of strands extracted from Rutherford cables are particularly demanding. Quality of wire, cabling deformation, heat treatment temperature, heat treatment atmosphere, sample handling, and measurement methods can all affect the RRR. Therefore, as an integral part of the electrical quality control (QC) of Nb 3 Sn Rutherford cables manufactured at the Lawrence Berkeley National Laboratory, it was prudent that we established a RRR measurement system that can isolate the assessment of cable-fabrication-related impacts from sample preparation and measurement factors. Here we describe a bespoke cryocooler-based measurement system, capable of measuring RRR of over 80 samples in a single cooldown. The samples are mounted on custom-designed printed circuit boards that accommodate the shape of strands extracted from a Rutherford cable without added deformation, which we will show is critical in ensuring that the measurements accurately represent the RRR values of the conductor within the cable. Using this sample mounting solution, we routinely measure the overall RRR of the strand as well as individual intra-strand sections corresponding to both cable edges and cable broad faces with high reproducibility. Such measurements provide valuable information on the variation of RRR along the length of the strands as well as across strand productions and cable runs over time.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
PNNL's Characterization Summary for MP-2 Experiment
Characterization of as-fabricated fuel was performed at Pacific Northwest National Laboratory (PNNL) in accordance with the characterization plan for the fabrication of U 10Mo plate fuel for the U.S. High Performance Research Reactor conversion program’s Fuel Fabrication Pillar (INL 2021). Similar characterization work is also being performed at Idaho National Laboratory to provide a detailed understanding of the as-fabricated foils that would be irradiated in the Mini-Plate 2 (MP 2) experiment. Under the MP 2 characterization plan, foils are studied that have different fabrication parameters (such as rolling condition, rolling thickness reduction, co-rolling with Zr layers). Similar samples from master foils were sent to both the organizations, so that the testing and analysis can be done independently using similar equipment and standardized measurement and analysis procedures. A final, consolidated report will be prepared based on this work and will summarize all the information obtained from the two laboratories. The MP 2 experiment will provide an opportunity to understand the effects of processing conditions on the final fuel microstructure, to compare results obtained independently, and achieve a two-way validation. In Fiscal Year 2022, PNNL received five MP 2 cast (PD STD2) samples to examine the foils’ chemistry and microstructure. For each cast sample, PNNL received samples from three different locations. PNNL also received and characterized 24 U 10Mo foil samples, by sectioning four pieces/specimens from each foil, in accordance with the MP 2 Characterization Plan (INL 2021). These 24 samples consist of four types of foils from BWX Technologies: 0.047 in. thick hot-rolled and annealed samples with Zr layers; 0.025 in. thick cold-rolled and annealed samples with Zr layers; 0.0105 in. thick cold-rolled and annealed samples with Zr layers. Along with these, PNNL also received four plates with Zr layers that were 0.025 in. and 0.0105 in. thick. This report describes the results of PNNL’s MP 2 foil characterization. Microstructure, Mo homogeneity, carbide fraction and morphology, U 10Mo foil thickness, and Zr thickness were evaluated in both the longitudinal and transverse directions for all the foils of the three different thicknesses.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗