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All sources NASA NTRS DOE OSTI

DOE OSTI2017

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry

Solid sampling and analysis methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), are challenged by matrix effects and calibration difficulties. Matrix-matched standards for external calibration are seldom available and it is difficult to distribute spikes evenly into a solid matrix as internal standards. While isotopic ratios of the same element can be measured to high precision, matrix-dependent effects in the sampling and analysis process frustrate accurate quantification and elemental ratio determinations. Here we introduce a potentially general solid matrix transformation approach entailing chemical reactions in molten ammonium bifluoride (ABF) salt that enables the introduction of spikes as tracers or internal standards. Proof of principle experiments show that the decomposition of uranium ore in sealed PFA fluoropolymer vials at 230 °C yields, after cooling, new solids suitable for direct solid sampling by LA. When spikes are included in the molten salt reaction, subsequent LA-ICP-MS sampling at several spots indicate that the spikes are evenly distributed, and that U-235 tracer dramatically improves reproducibility in U-238 analysis. Precisions improved from 17% relative standard deviation for U-238 signals to 0.1% for the ratio of sample U-238 to spiked U-235, a factor of over two orders of magnitude. These results introduce the concept of solid matrix transformation (SMT) using ABF, and provide proof of principle for a new method of incorporating internal standards into a solid for LA-ICP-MS. This new approach, SMT-LA-ICP-MS, provides opportunities to improve calibration and quantification in solids based analysis. Finally, looking forward, tracer addition to transformed solids opens up LA-based methods to analytical methodologies such as standard addition, isotope dilution, preparation of matrix-matched solid standards, external calibration, and monitoring instrument drift against external calibration standard

47 OTHER INSTRUMENTATION↗

DOE OSTI2016

Anthropogenic plutonium-244 in the environment: Insights into plutonium’s longest-lived isotope

Owing to the rich history of heavy element production in the unique high flux reactors that operated at the Savannah River Site, USA (SRS) decades ago, trace quantities of plutonium with highly unique isotopic characteristics still persist today in the SRS terrestrial environment. Development of an effective sampling, processing, and analysis strategy enables detailed monitoring of the SRS environment, revealing plutonium isotopic compositions, e.g., 244 Pu, that reflect the unique legacy of plutonium production at SRS. This work describes the first long-term investigation of anthropogenic 244 Pu occurrence in the environment. Environmental samples, consisting of collected foot borne debris, were taken at SRS over an eleven year period, from 2003 to 2014. Separation and purification of trace plutonium was carried out followed by three stage thermal ionization mass spectrometry (3STIMS) measurements for plutonium isotopic content and isotopic ratios. Furthermore, significant 244 Pu was measured in all of the years sampled with the highest amount observed in 2003. The 244 Pu content, in femtograms (fg = 10 –15 g) per gram, ranged from 0.31 fg/g to 44 fg/g in years 2006 and 2003 respectively. In all years, the 244 Pu/ 239 Pu atom ratios were significantly higher than global fallout, ranging from 0.003 to 0.698 in years 2014 and 2003 respectively.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2016

SiC/Si{sub 3}N{sub 4} nanotubes from peanut shells

Nanotubes and nanoparticles of SiC and Si{sub 3}N{sub 4} were produced from the thermal treatment of peanut shells in argon and nitrogen atmospheres respectively, at temperatures in excess of 1350°C. Using x-ray diffraction, Raman spectroscopy and transmission electron microscopy analysis, the processed samples in argon atmosphere were shown to consist of 2H and 3C polytypes of SiC nanoparticles and nanotubes. Whereas the samples prepared in nitrogen atmosphere consisted of α-phase of Si{sub 3}N{sub 4}. Nanostructures formed by a single direct reaction provide a sustainable synthesis route for nanostructured SiC and Si{sub 3}N{sub 4}, for potential engineering applications due to their exceptional mechanical and electro-optic properties.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2021

Analysis of Defense Waste Processing Facility Sample: Recycle Collection Tank Sample Batch 4945

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (now Savannah River Mission Completion (SRMC)), through a Technical Task Request, to characterization the “as-received” Recycle Collection Tank (RCT) Sample identified as sample batch 4945 [Sludge Receipt and Adjustment Tank (SRAT) batch 796)], which was delivered to SRNL Shielded Cells on January 28, 2021. The RCT characterization data will be used as input to the Defense Waste Processing Facility (DWPF) Recycle Diversion Project. This RCT report is the first of three sample characterization reports that will be used for this DWPF Project. The other DWPF reports will involve the characterization of the Off-Gas Condensate Tank (OGCT) and the Slurry Mix Evaporator Condensate Tank (SMECT) samples.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

Analysis of Defense Waste Processing Facility Sample: Recycle Collection Tank Sample Batch 4945

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DOE OSTI2022

Analysis of Defense Waste Processing Facility Sample: Off-Gas Condensate Tank Sample Batch 27862

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (now Savannah River Mission Completion (SRMC)), through a Technical Task Request (X-TTR-H-00107), to characterize the “as-received” Off-Gas Condensate Tank (OGCT) Sample identified as sample batch 27862, which was delivered to SRNL Shielded Cells on April 30, 2021. This OGCT report is the third of three sample characterization reports dealing with this Defense Waste Processing Facility (DWPF) Recycle Diversion Project. The other two recycling stream characterization reports are the Recycle Collection Tank (RCT) and the Slurry Mix Evaporator Condensate Tank (SMECT) sample report.

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DOE OSTI2022

Analysis of Defense Waste Processing Facility Sample: Slurry Mix Evaporator Condensate Tank Sample Batch 4638

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR, now Savannah River Mission Completion (SRMC)), through a Technical Task Request, to characterization the “as-received” Slurry Mix Evaporator Condensate Tank (SMECT) sample identified as sample batch 4638, which was delivered to SRNL Shielded Cells on March 19, 2021. The SMECT characterization data will be used as input to the Defense Waste Processing Facility (DWPF) Recycle Diversion Project. This SMECT report is the second of three sample characterization reports that will be used for this DWPF Project. The other two DWPF characterization reports involve the characterization of the Recycle Collection Tank (RCT) sample and the future Off-Gas Condensate Tank (OGCT) characterization report.

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DOE OSTI2020

GeoMelt{sup R} In-Container Vitrification (ICV){sup TM} for Fukushima Daiichi Water Treatment Secondary Wastes - 20212

The Japanese government is supporting development work implemented jointly by Veolia subsidiaries Kurion Japan, K.K., Veolia Nuclear Solutions (VNS), Inc., and Veolia Nuclear Solutions Federal Services, LLC for treating radioactive waste generated from Fukushima Daiichi Nuclear Power Station (NPS) water treatment using the GeoMelt{sup TM} In-Container Vitrification (ICV){sup TM} technology. The initial work consisted of glass formulation and engineering-scale testing which was completed in 2018, in the frame of an IRID (International Research Institute for Nuclear Decommissioning) program as part of a project subsidized by Japan's Ministry of Economy, Trade and Industry (METI). The Fukushima Daiichi NPS Mid- and Long-Term Road-map requires investigation of methods to stabilize solid wastes (and to immobilize radioisotopes in the wastes) generated as a result of emergency response and decommissioning activities. Cooling water treatment has resulted in a significant amount of solid and slurry secondary wastes (mostly adsorbents and ion-exchange materials) which will require processing at some point. GeoMelt{sup R} ICV{sup TM} is a joule-heated melter technology which uses a refractory-lined single-use container combining the melter and disposal container. There is no pouring required nor concerns with refractory corrosion which allows the process to accommodate a wide range of waste chemistries and high waste loadings. The testing described here consisted of three engineering-scale melts, each processing between 212 kg and 240 kg of waste simulants, glass formers, and non-radioactive cesium (Cs) and strontium (Sr) tracers. Continuous isokinetic stack sampling of off-gas emissions was performed for each test in order to calculate Cs and Sr retention in the glass wasteform. Single-pass retention of Cs in the final glass wasteform ranged from 91.46 to 99.30%, and single-pass retention of Sr ranged from 99.76 to 100%. Planned particulate recycle will increase these retention levels. Melt 1 processed a mixture of KUR-EH (a zeolite-based ion-exchange material), simulated Advanced Liquid Processing System (ALPS) Carbonate and Iron Slurries, and glass additives. Melt 2 processed a mixture of KUR-EH, KUR-TSG (a titanate-based adsorbent), and glass additives. Melt 3 processed a mixture of KUR-EH, simulated barium sulfate/iron ferrocyanide sludge (AREVA sludge), and glass additives. Waste loadings for these melts ranged from 70 weight percent (wt%) to 82 wt%. Vitrification produces a waste form much denser than the stored water treatment secondary waste wastes, resulting in significant volume reduction. Volume reductions for the three tests ranged from 74 to 79 vol%. Vitrification produces a chemically durable wasteform. Pacific Northwest National Laboratory (PNNL) tested three glass samples from each engineering-scale melt) by the Materials Characterization Center 1 (MCC-1) test, an international standard leach test of the chemical durability of nuclear waste glasses. PNNL also obtained one U.S. reference glass (EA Glass) and two Japan reference glasses P0798) and tested these under the same MCC-1 conditions (90 deg. C, 10 m-1, DIW, and 7, 14, 28-day) as the GeoMelt{sup R} ICV{sup TM} glasses. The GeoMelt{sup R} ICV{sup TM} glasses exhibited lower total normalized releases and 14- to 28-day normalized release rates than the three reference glasses. These results suggest that the GeoMelt{sup R} ICV{sup TM} glasses have durabilities on par with high-level waste glasses under standard test conditions. Post-melt process sampling and analysis indicated no Cs migration into the melter refractory materials and very little deposition of Cs or Sr onto the melter hood or off-gas piping internals. The results of the testing indicated good Cs retention in the glass, high volume reduction and waste loadings, and excellent chemical durability. These factors are important to minimize treatment costs and to protect workers and the environment. (authors)

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DOE OSTI2016

Biological Sampling Variability Study

There are many sources of variability that exist in the sample collection and analysis process. This paper addresses many, but not all, sources of variability. The main focus of this paper was to better understand and estimate variability due to differences between samplers. Variability between days was also studied, as well as random variability within each sampler. Experiments were performed using multiple surface materials (ceramic and stainless steel), multiple contaminant concentrations (10 spores and 100 spores), and with and without the presence of interfering material. All testing was done with sponge sticks using 10-inch by 10-inch coupons. Bacillus atrophaeus was used as the BA surrogate. Spores were deposited using wet deposition. Grime was coated on the coupons which were planned to include the interfering material (Section 3.3). Samples were prepared and analyzed at PNNL using CDC protocol (Section 3.4) and then cultured and counted. Five samplers were trained so that samples were taken using the same protocol. Each sampler randomly sampled eight coupons each day, four coupons with 10 spores deposited and four coupons with 100 spores deposited. Each day consisted of one material being tested. The clean samples (no interfering materials) were run first, followed by the dirty samples (coated with interfering material). There was a significant difference in recovery efficiency between the coupons with 10 spores deposited (mean of 48.9%) and those with 100 spores deposited (mean of 59.8%). There was no general significant difference between the clean and dirty (containing interfering material) coupons or between the two surface materials; however, there was a significant interaction between concentration amount and presence of interfering material. The recovery efficiency was close to the same for coupons with 10 spores deposited, but for the coupons with 100 spores deposited, the recovery efficiency for the dirty samples was significantly larger (65.9% - dirty vs. 53.6% - clean) (see Figure 4.1). Variance component analysis was used to estimate the amount of variability for each source of variability. There wasn’t much difference in variability for dirty and clean samples, as well as between materials, so these results were pooled together. There was a significant difference in amount of concentration deposited, so results were separated for the 10 spore and 100 spore deposited tests. In each case the within sampler variability was the largest with variances of 426.2 for 10 spores and 173.1 for 100 spores. The within sampler variability constitutes the variability between the four samples of similar material, interfering material, and concentration taken by each sampler. The between sampler variance was estimated to be 0 for 10 spores and 1.2 for 100 spores. The between day variance was estimated to be 42.1 for 10 spores and 78.9 for 100 spores. Standard deviations can be calculated in each case by taking the square root of the variance.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2019

Metagenomic Analysis of Three Samples from the MCU Process

Three Modular Caustic-Side Solvent Extraction (CSSX) Unit (MCU) Strip Effluent Feed samples were sent from Savannah River National Laboratory (SRNL) to Microbial Insights (MI), Knoxville, TN, for molecular analysis. The objective of the analysis was to profile and identify dominant members of the microbial community in these samples. More effective control of microbial growth in the MCU depends on the fundamental understanding of the microorganisms responsible for system colonization that leads to biofilm formation and coalescer impairment. This analysis entailed Next-generation sequencing (NGS) of DNA, a collective term for advanced technologies that allow the determination of microbial species present. NGS, also commonly called metagenomics, provides for the identification of microorganisms down to the genus level. Although function, e.g. biofilm formation or corrosion, cannot always be predicted from identification, knowledge of the microorganisms present can offer insight into the potential microbial processes that may influence system function occurring in the MCU. Information on microbial identification can also influence control measures, e.g. operational/maintenance parameters or the choice of biocides to employ. This knowledge can help control undesired microbial activity as conventional cleaning and disinfection regimens may also contribute to inefficient biofilm control and dissemination of microbial resistance to remediation efforts.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2022

Caution on Using Tetrahydrofuran for Processing Crystalline Silica Samples From Engineered Stone for XRD Analysis

Abstract We conducted laboratory experiments to investigate a suspected effect of tetrahydrofuran (THF) on quantifying crystalline silica in samples collected from working with engineered stone when THF is used to process samples prior to the X-ray diffraction (XRD) analysis. Two groups of samples from grinding either engineered stone or granite were simultaneously taken from a laboratory testing system, with one group of samples using THF for processing and another group using muffle furnace for ashing. For each stone type, we also tested four levels of respirable dust loading on the samples by varying the grinding time from 1 to 8 min. Statistical analysis of the experimental results on crystalline silica contents of the two groups of samples showed that the difference between the two methods was not significant (P ≥ 0.05) for the granite at all four levels of respirable dust loading and for the engineered stone at the two levels of respirable dust loading greater than 0.5 mg. However, the crystalline silica content from using THF processing was significantly lower (P = 0.001) than that from using muffle furnace ashing for engineered stone when the respirable dust loading levels were less than 0.5 mg. For the engineered stone dust samples with grinding times of 1 and 2 min, the average respirable dust loading was about 0.19 and 0.34 mg, respectively; while the crystalline silica content from using THF processing was 30.9 and 21.5% lower than that from using muffle furnace ashing, respectively. Since most full-shift samples from field assessments in this industry are expected to have respirable dust loading less than 0.5 mg, muffle furnace or radio frequency plasma ashing should be specified as the preferred sample processing method instead of the THF processing method for quantification of crystalline silica when engineered stone is expected to present to avoid artificially reduced silica content values, which are likely caused by the reactions between THF and the resins in engineered stone.

Public, Environmental & Occupational Health↗

DOE OSTI2018

Instrumentation for Hanford Direct-Feed Low-Activity Waste Real-Time, In-Line Process Monitoring - 18339

The direct-feed low-activity waste (DFLAW) process will utilize facilities in the Hanford tank farms to stage tank waste feed, a new facility to pretreat the tank waste feed, and facilities in the Hanford Waste Treatment and Immobilization Plant (WTP) to immobilize the low-activity waste (LAW) and disposition effluents from the vitrification process. Process sampling is used extensively throughout the DFLAW process to qualify waste feeds, control the process, and demonstrate compliance with regulatory and contractual commitments. The U.S. Department of Energy's Office of River Protection (ORP) has started a program to evaluate the potential benefits of replacing some sample collection requirements with realtime, in-line monitoring (RTIM). The program will identify, develop, and evaluate technologies that can reduce the number of samples required for WTP operation. Potential benefits of RTIM include elimination of process holds for sample analysis, a reduction in worker exposure to radiation and chemical hazards, decreased secondary waste volume, reducing the cost for sample collection and analysis, an improvement in product quality, and timely indication of process anomalies. In order to incorporate RTIM, the process control strategy for the overall process, as well as each unit operation, was reviewed and revisions to the strategies proposed. The following items were identified for incorporation of RTIM: - Real-time material balance calculations linked to the process control system; - Use of RTIM instruments to validate the material balance for selected analytes; - Anion analysis for determination of selected semi-volatile species (e.g., chlorine, sulfur, and fluorine) in the recycle stream. Based on the proposed process control strategy, a preliminary list of potential analytical equipment was developed. This was followed by a preliminary survey of instrument technologies currently on the market building on surveys performed for ORP, literature reviews, vendor web sites, and subject matter experts from the Savannah River National Laboratory and other U.S. Department of Energy national laboratories. Each technology was evaluated for measurement capability, operations and maintenance requirements, space requirements, and potential for application as process control instrumentation. The instrument technologies were chosen based on the following criteria: - Ability to perform analyses needed; - Potential to be used or adapted for use as process control instruments; - Potential to be adapted to size and operational constraints of standard WTP sample cabinets; - Operational and maintenance requirements. (authors)

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DOE OSTI2013

Extended forward sensitivity analysis of one-dimensional isothermal flow

Sensitivity analysis and uncertainty quantification is an important part of nuclear safety analysis. In this work, forward sensitivity analysis is used to compute solution sensitivities on 1-D fluid flow equations typical of those found in system level codes. Time step sensitivity analysis is included as a method for determining the accumulated error from time discretization. The ability to quantify numerical error arising from the time discretization is a unique and important feature of this method. By knowing the relative sensitivity of time step with other physical parameters, the simulation is allowed to run at optimized time steps without affecting the confidence of the physical parameter sensitivity results. The time step forward sensitivity analysis method can also replace the traditional time step convergence studies that are a key part of code verification with much less computational cost. One well-defined benchmark problem with manufactured solutions is utilized to verify the method; another test isothermal flow problem is used to demonstrate the extended forward sensitivity analysis process. Through these sample problems, the paper shows the feasibility and potential of using the forward sensitivity analysis method to quantify uncertainty in input parameters and time step size for a 1-D system-level thermal-hydraulic safety code. (authors)

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2022

CondiDiag1.0: a flexible online diagnostic tool for conditional sampling and budget analysis in the E3SM atmosphere model (EAM)

Abstract. Numerical models used in weather and climate prediction take into account a comprehensive set of atmospheric processes (i.e., phenomena) such as the resolved and unresolved fluid dynamics, radiative transfer, cloud and aerosol life cycles, and mass or energy exchanges with the Earth's surface. In order to identify model deficiencies and improve predictive skills, it is important to obtain process-level understanding of the interactions between different processes. Conditional sampling and budget analysis are powerful tools for process-oriented model evaluation, but they often require tedious ad hoc coding and large amounts of instantaneous model output, resulting in inefficient use of human and computing resources. This paper presents an online diagnostic tool that addresses this challenge by monitoring model variables in a generic manner as they evolve within the time integration cycle. The tool is convenient to use. It allows users to select sampling conditions and specify monitored variables at run time. Both the evolving values of the model variables and their increments caused by different atmospheric processes can be monitored and archived. Online calculation of vertical integrals is also supported. Multiple sampling conditions can be monitored in a single simulation in combination with unconditional sampling. The paper explains in detail the design and implementation of the tool in the Energy Exascale Earth System Model (E3SM) version 1. The usage is demonstrated through three examples: a global budget analysis of dust aerosol mass concentration, a composite analysis of sea salt emission and its dependency on surface wind speed, and a conditionally sampled relative humidity budget. The tool is expected to be easily portable to closely related atmospheric models that use the same or similar data structures and time integration methods.

58 GEOSCIENCES↗

DOE OSTI2015

Sample registration software for process automation in the Neutron Activation Analysis (NAA) Facility in Malaysia nuclear agency

Neutron Activation Analysis (NAA) had been established in Nuclear Malaysia since 1980s. Most of the procedures established were done manually including sample registration. The samples were recorded manually in a logbook and given ID number. Then all samples, standards, SRM and blank were recorded on the irradiation vial and several forms prior to irradiation. These manual procedures carried out by the NAA laboratory personnel were time consuming and not efficient. Sample registration software is developed as part of IAEA/CRP project on ‘Development of Process Automation in the Neutron Activation Analysis (NAA) Facility in Malaysia Nuclear Agency (RC17399)’. The objective of the project is to create a pc-based data entry software during sample preparation stage. This is an effective method to replace redundant manual data entries that needs to be completed by laboratory personnel. The software developed will automatically generate sample code for each sample in one batch, create printable registration forms for administration purpose, and store selected parameters that will be passed to sample analysis program. The software is developed by using National Instruments Labview 8.6.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Influence of velocity of pressing in RCS processed AA8090 Al-Li alloy

Highlights: • For the first time the Influence of RCS on the properties of AA 8090 has been studied by processing velocity. • It is found that the properties vary according to pressing velocity and number of passes. • Reported significant property improvement achieved through the pressing velocity of 1.5mm/s. - Abstract: The effect of the velocity of pressing on grain refinement in AA8090 Al-Li alloy sheets during repetitive corrugation and straightening (RCS) at 300 °C is studied. V-groove corrugation dies and flattening dies were used at three different pressing velocities of 1.5 mm/s, 2 mm/s and 2.5 mm/s. The specimen temperature was maintained at 300 °C. Grain refinement was significantly influenced by the pressing velocity. The samples processed for 8 passes at a pressing velocity of 1.5 mm/s had an improved microhardness value of 104 HV and an increased tensile strength of 405 MPa which is respectively 39% and 113% more than the corresponding values in the parent material. TEM analysis showed that samples processed at a pressing velocity of 1.5 mm/s had in places a grain size down to 50 nm and the EBSD results revealed that the average grain size was 2 μm, with 86% of the total number of grain boundaries of the high angle type.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Tank 12H Acidic Chemical Cleaning Sample Analysis And Material Balance

A process of Bulk Oxalic Acid (BOA) chemical cleaning was performed for Tank 12H during June and July of 2013 to remove all or a portion of the approximately 4400 gallon sludge heel. Three strikes of oxalic acid (nominally 4 wt% or 2 wt%) were used at 55°C and tank volumes of 96- to 140-thousand gallons. This report details the sample analysis of a scrape sample taken prior to BOA cleaning and dip samples taken during BOA cleaning. It also documents a rudimentary material balance for the Tank 12H cleaning results.

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DOE OSTI2023

Analysis of Defense Waste Processing Facility (DWPF) Condensate Samples and Evaluation of the Glycolate Destruction Process during Nitric-Glycolic flowsheet Transition

Glycolate concentrations were measured by the Savannah River National Laboratory (SRNL) in Slurry Mix Evaporator Condensate Tank (SMECT) and Recycle Collection Tank (RCT) samples retrieved after implementation of the Nitric-Glycolic Acid flowsheet at the Defense Waste Processing Facility (DWPF). No glycolate has been detected in any sample using Ion Chromatography (IC) with a detection limit of 8 mg/L, and no glycolate has been detected using either IC or Proton Nuclear Magnetic Resonance Spectroscopy ( 1 HNMR) after a permanganate strike was performed in the RCT.

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