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DOE OSTI2021

Pulsar-Calibrated Timing Source for Synchronized Sampling

The Global Positioning System (GPS) is critical to the real-time synchronized sampling of phasor measurement units (PMUs). Unfortunately, GPS signals are occasionally unstable due to several factors such as weak satellite signal and GPS spoofing, thereby leaving the PMU with a degraded sampling performance. In this letter, a novel Pulsar-calibrated Timing Source (PTS) is proposed as the alternative timing source for synchronized sampling. Further, the PTS can generate the timing signal with a 1 μs drift error within 91 holdover minutes to ensure continuity of sampling accuracy. Experimental tests are conducted and the results reveal the reliability and accuracy of the PTS for PMU synchronization.

42 ENGINEERING↗

DOE OSTI2023

A Systematic Investigation of the Effects of Standard-Sample Concentration Mismatch during Fe Isotope Measurement by MC-ICP-MS

Advances in multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS) have led to the widespread use of iron (Fe) isotopes to elucidate the (bio)geochemical history of a range of environments. To generate Fe isotope ratio measurements, standard-sample bracketing (SSB) is commonly used to correct for instrumental mass bias inherent to MC-ICP-MS. However, SSB is only accurate when sample and isotope standard Fe concentrations match, in addition to the bulk solution matrix. When the Fe concentrations differ, Fe isotope ratio measurement results may be inaccurate, a phenomenon known as the "self-induced matrix effect." Here, this study systematically characterised the self-induced matrix effect for dry plasma Fe isotope ratio measurements on three MC-ICP-MS instruments and three introduction systems. Our extensive dataset indicates that: (1) the degree of mass bias is consistent regardless of MC-ICP-MS front-end design, (2) the degree of mass bias becomes less reproducible as the concentration difference between the sample and bracketing standard increases, and (3) this applies to both pure Fe solutions and solutions from geological materials. This study reinforces the requirement to match bracketing standard and sample concentrations within 10% and provides a correction method for that fall beyond the recommended concentration range to subsequently allow for proper concentration matching during SSB.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Round Robin Analysis of Uranium Isotopics on Cotton Swipes Measured Using Microextraction-Based Sampling Versus Conventional Bulk Analysis

A comparison of microextraction sampling methods to directly analyze uranium isotopics on cotton swipes was performed concurrently with traditional bulk-processing methods. For the microextraction sampling approach, two different detection platforms were evaluated, a quadrupole-based inductively coupled plasma mass spectrometer (ICP-MS) and the liquid sampling-atmospheric pressure glow discharge (LS-APGD) coupled to an Orbitrap mass spectrometer. Results presented from this innovative sampling approach (i.e., microextraction) are compared with a more traditional approach employed for analysis of cotton-based environmental swipes, namely bulk ashing/digestion, separation, and subsequent analysis by high-precision multi-collector ICP-MS. Overall, the microextraction approach proved to be a reliable and accurate means to determine isotopic ratios of uranium collected on cotton swipes. The ICP-MS-based detection had relative standard deviations of <0.65% for the major isotopic determinations, whereas the LS-APGD-Orbitrap method had relative standard deviations of <3%. The percent relative difference for the 235 U/ 238 U ratios, in comparison to the expected values, was <1% for ICP-MS and <4% for the microplasma-Orbitrap method. Additionally, the microextraction ICP-MS accurately (<2%) and precisely (<5%) determined the minor isotopic compositions (i.e., 234 U/ 238 U and 236 U/ 238 U).

ICP-MS↗

DOE OSTI2020

Chemistry of the thermal water samples of the Camas Prairie area in Idaho, USA

This dataset includes chemistry of geothermal water samples of the Camas Prairie area in Idaho. The samples included in this dataset were collected over the period of 2016-2019. Collection/analysis of new water samples and compilation of existing water chemistry database were conducted for Snake River Play Fairway Project. All chemical analysis of the samples were conducted in the Analytical Laboratory at the Center of Advanced Energy Studies (unless otherwise indicated) in Idaho Falls, Idaho. Isotope analysis were conducted in analytical/isotope measurement labs at Lawrence Berkeley National Laboratory, Utah State University, and University of Utah.

15 GEOTHERMAL ENERGY↗

DOE OSTI2022

Temporal Study 2021-2022: Sample-Based Surface Water Chemistry and Organic Matter Characterization across Watersheds in the Yakima River Basin, Washington, USA (v3)

This dataset supports a broader study examining the drivers of temporal variability in sediment respiration rates in the Yakima River Basin. The dataset provides geochemistry and organic matter characterization data generated from samples collected at weekly or bi-weekly intervals at six sites across the Yakima River Basin in Washington, USA. Related sensor data will be published separately and can be used to link sediment respiration rates to biogeochemical processing rates. The data package was originally published in November 2022. It was updated in November 2023 (v2; modified files) and April 2025 (new and modified files). See the change history section in readme for more details. For details on how to navigate data packages generated by this project, see https://data.ess-dive.lbl.gov/portals/PNNLRiverCorridorSFA/About. This dataset is comprised of one main data folder containing (1) file-level metadata; (2) data dictionary; (3) field metadata; (4) dissolved inorganic carbon (DIC), dissolved organic carbon (DOC; reported as non-purgeable organic carbon; NPOC), total nitrogen (TN), total suspended solids (TSS), and ions; (5) averaged values from water chemistry data; (6) surface water sampling protocol; (7) sensor protocol; (8) readme; (9) methods codes; (10) international generic sample number (IGSN) mapping file; and (11) folder of high resolution characterization of organic 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). This folder contains two subfolders, one containing the .xml data files and the other containing instructions for using Formularity (https://omics.pnl.gov/software/formularity) and an R script to process the data based on the user's specific needs. All files are .csv, .pdf, .R, .ref, or .xml. We acknowledge the Yakama Nation as owners and caretakers of the lands where we collected our data. We thank the Confederated Tribes and Bands of the Yakama Nation Tribal Council and Yakama Nation Fisheries for working with us to facilitate sample collection and optimization of data usage according to their values and worldview.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2025

Temporal Study 2022-2024: Sample-Based Surface Water Dissolved Inorganic Carbon, Dissolved Organic Carbon, Total Nitrogen, Stable Isotopes, and Total Suspended Solids from across Multiple Watersheds in the Yakima River Basin, Washington, USA

18-O↗

DOE OSTI2015

Tank 12H residuals sample analysis report

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) to provide sample preparation and analysis of the Tank 12H final characterization samples to determine the residual tank inventory prior to grouting. Eleven Tank 12H floor and mound residual material samples and three cooling coil scrape samples were collected and delivered to SRNL between May and August of 2014.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2015

Analysis of Tank 38H (HTF-38-15-119, 127) Surface, Subsurface and Tank 43H (HTF-43-15-116, 117 and 118) Surface, Feed Pump Suction and Jet Suction Subsurface Supernatant Samples in Support of Enrichment, Corrosion Control and Salt Batch Planning Programs

Compositional feed limits have been established to ensure that a nuclear criticality event for the 2H and 3H Evaporators is not possible. The Enrichment Control Program (ECP) requires feed sampling to determine the equivalent enriched uranium content prior to transfer of waste other than recycle transfers (requires sampling to determine the equivalent enriched uranium at two locations in Tanks 38H and 43H every 26 weeks) The Corrosion Control Program (CCP) establishes concentration and temperature limits for key constituents and periodic sampling and analysis to confirm that waste supernate is within these limits. This report provides the results of analyses on Tanks 38H and 43H surface and subsurface supernatant liquid samples in support of the ECP, the CCP, and the Salt Batch 10 Planning Program.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2016

Sludge batch 9 (SB9) acceptance evaluation. Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tank 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a composition expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2015

Technologies for pre-screening IAEA swipe samples

During the course of International Atomic Energy Agency (IAEA) inspections, many samples are taken for the purpose of verifying the declared facility activities and identifying any possible undeclared activities. One of these sampling techniques is the environmental swipe sample. Due to the large number of samples collected, and the amount of time that is required to analyze them, prioritizing these swipes in the field or upon receipt at the Network of Analytical Laboratories (NWAL) will allow sensitive or mission-critical analyses to be performed sooner. As a result of this study, technologies were placed into one of three categories: recommended, promising, or not recommended. Both neutron activation analysis (NAA) and X-ray fluorescence (XRF) are recommended for further study and possible field deployment. These techniques performed the best in initial trials for pre-screening and prioritizing IAEA swipes. We learned that for NAA more characterization of cold elements (such as calcium and magnesium) would need to be emphasized, and for XRF it may be appropriate to move towards a benchtop XRF versus a handheld XRF due to the increased range of elements available on benchtop equipment. Promising techniques that will require additional research and development include confocal Raman microscopy, fluorescence microscopy, and infrared (IR) microscopy. These techniques showed substantive responses to uranium compounds, but expensive instrumentation upgrades (confocal Raman) or university engagement (fluorescence microscopy) may be necessary to investigate the utility of the techniques completely. Point-and-shoot (handheld) Raman and attenuated total reflectance–infrared (ATR-IR) measurements are not recommended, as they have not shown enough promise to continue investigations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Monitoring, Modeling, and Diagnosis of Alkali-Silica Reaction in Small Concrete Samples

Assessment and management of aging concrete structures in nuclear power plants require a more systematic approach than simple reliance on existing code margins of safety. Structural health monitoring of concrete structures aims to understand the current health condition of a structure based on heterogeneous measurements to produce high-confidence actionable information regarding structural integrity that supports operational and maintenance decisions. This report describes alkali-silica reaction (ASR) degradation mechanisms and factors influencing the ASR. A fully coupled thermo-hydro-mechanical-chemical model developed by Saouma and Perotti by taking into consideration the effects of stress on the reaction kinetics and anisotropic volumetric expansion is presented in this report. This model is implemented in the GRIZZLY code based on the Multiphysics Object Oriented Simulation Environment. The implemented model in the GRIZZLY code is randomly used to initiate ASR in a 2D and 3D lattice to study the percolation aspects of concrete. The percolation aspects help determine the transport properties of the material and therefore the durability and service life of concrete. This report summarizes the effort to develop small-size concrete samples with embedded glass to mimic ASR. The concrete samples were treated in water and sodium hydroxide solution at elevated temperature to study how ingress of sodium ions and hydroxide ions at elevated temperature impacts concrete samples embedded with glass. Thermal camera was used to monitor the changes in the concrete sample and results are summarized.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2016

Analytical results from routine DSSHT and SEHT monthly samples

Strip Effluent Hold Tank (SEHT) and Decontaminated Salt Solution Hold Tank (DSSHT) samples from several of the “microbatches” of Integrated Salt Disposition Project (ISDP) Salt Batch (“Macrobatch”) 8B have been analyzed for 238 Pu, 90 Sr, 137 Cs, cations (Inductively Coupled Plasma Emission Spectroscopy - ICPES), and anions (Ion Chromatography Anions - IC-A). The analytical results from the current microbatch samples are similar to those from previous macrobatch samples. The Cs removal continues to be excellent, with decontamination factors (DF) averaging 22,100 (114% RSD). The bulk chemistry of the DSSHT and SEHT samples does not show any signs of unusual behavior, other than lacking the anticipated degree of dilution that is calculated to occur during Modular Caustic-Side Solvent Extraction Unit (MCU) processing.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2016

Data Validation Package May 2016 Groundwater Sampling at the Bluewater, New Mexico, Disposal Site, September 2016

Groundwater samples were collected from monitoring wells at the Bluewater, New Mexico, Disposal Site to monitor groundwater contaminants as specified in the 1997 Long-Term Surveillance Plan for the DOE Bluewater (UMTRCA Title II) Disposal Site Near Grants, New Mexico (LTSP). Sampling and analyses were conducted as specified in the Sampling and Analysis Plan for U.S. Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated). A duplicate sample was collected from location 16(SG).

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2016

Data Validation Package May 2016 Groundwater Sampling at the Sherwood, Washington, Disposal Site August 2016

The 2001 Long-Term Surveillance Plan (LTSP) for the US. Department of Energy Sherwood Project (UMI'RCA Title II) Reclamation Cell, Wellpinit, Washington, does not require groundwater compliance monitoring at the Sherwood site. However, the LTSP stipulates limited groundwater monitoring for chloride and sulfate (designated indicator parameters) and total dissolved solids (TDS) as a best management practice. Samples were collected from the background well, MW-2B, and the two downgradient wells, MW-4 and MW-10, in accordance with the LTSP. Sampling and analyses were conducted as specified in the Sampling and Analysis Plan for US. Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated). Water levels were measured in all wells prior to sampling and in four piezometers completed in the tailings dam. Time-concentration graphs included in this report indicate that the chloride, sulfate, and TDS concentrations are consistent with historical measurements. The concentrations of chloride and sulfate are well below the State of Washington water quality criteria value of 250 milligrams per liter (mg/L) for both parameters.

2016 Groundwater Sampling Sherwood, Washington↗

DOE OSTI2019

Underground Test Area Annual Sampling Report Nevada National Security Site, Nevada (Revision 1, Calendar Year 2018)

The Sampling Plans (Rev. 0 and Rev. 1) ensure routine sampling that is critical to understanding contaminant transport near and downgradient of the underground nuclear testing areas, and is designed to ensure compliance with the UGTA Activity Quality Assurance Plan and the Federal Facility Agreement and Consent Order. This report presents the analytical data for the 2018 calendar year (CY) (January 1 through December 31, 2018) to ensure that the Sampling Plans’ objectives are achieved. Appendix D presents data from samples collected in 2016 and 2017. These results were not reported in previous reports because they were not available from the specialized laboratories at the time of the publication of the reports.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2017

The Impact of Sampling Medium and Environment on Particle Morphology

Sampling on different substrates is commonly used in laboratory and field studies to investigate the morphology and mixing state of aerosol particles. Our focus was on the transformations that can occur to the collected particles during storage, handling, and analysis. Particle samples were prepared by electrostatic deposition of size-classified sodium chloride, sulfuric acid, and coated soot aerosols on different substrates. The samples were inspected by electron microscopy before and after exposure to various environments. For coated soot, the imaging results were compared against mass-mobility measurements of airborne particles that underwent similar treatments. The extent of sample alteration ranged from negligible to major, depending on the environment, substrate, and particle composition. We discussed the implications of our findings for cases where morphology and the mixing state of particles must be preserved, and cases where particle transformations are desirable.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Multivariate Pointwise Information-Driven Data Sampling and Visualization

With increasing computing capabilities of modern supercomputers, the size of the data generated from the scientific simulations is growing rapidly. As a result, application scientists need effective data summarization techniques that can reduce large-scale multivariate spatiotemporal data sets while preserving the important data properties so that the reduced data can answer domain-specific queries involving multiple variables with sufficient accuracy. While analyzing complex scientific events, domain experts often analyze and visualize two or more variables together to obtain a better understanding of the characteristics of the data features. Therefore, data summarization techniques are required to analyze multi-variable relationships in detail and then perform data reduction such that the important features involving multiple variables are preserved in the reduced data. To achieve this, in this work, we propose a data sub-sampling algorithm for performing statistical data summarization that leverages pointwise information theoretic measures to quantify the statistical association of data points considering multiple variables and generates a sub-sampled data that preserves the statistical association among multi-variables. Using such reduced sampled data, we show that multivariate feature query and analysis can be done effectively. The efficacy of the proposed multivariate association driven sampling algorithm is presented by applying it on several scientific data sets.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2017

Immediate drop on demand technology (I-DOT) coupled with mass spectrometry via an open port sampling interface

Here, the immediate drop on demand technology to a mass spectrometer via the recently introduced open port sampling interface and ESI. A maximum sample analysis throughput of 5 s per sample was demonstrated. Signal reproducibility was 10% or better as demonstrated by the quantitative analysis of propranolol and its stable isotope-labeled internal standard propranolol-d7. The ability of the system to multiply charge and analyze macromolecules was demonstrated using the protein cytochrome c. In conclusion, this immediate drop on demand technology/open port sampling interface/ESI–MS combination allowed for the quantitative analysis of relatively small mass analytes and was used for the identification of macromolecules like proteins.

47 OTHER INSTRUMENTATION↗