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At least 703 records · Page 39
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Crystallographic Snapshots of Pre- and Post-Lanthanide Halide Hydrolysis─Reaction Products Captured by the 4-Amino-1,2,4-triazole Ligand

Reactions of lanthanide(III) chloride salts with 4-amino-1,2,4-triazole (4-NH 2 -1,2,4-Triaz) in azole melts have led to the isolation of both hydrolysis and non-hydrolysis products in the same synthesis with the inclusion of a variety of ligands, anions, and water, allowing us to capture crystallographic snapshots of different forms and intermediate hydrolysis fragments. The structural studies reported here include anhydrous and hydrated nonhydrolyzed complexes which were isolated alongside hydrolysis products giving oxide/hydroxide lanthanide(III) dimers, tetramers, and ultimately hexamers. The compounds isolated include [Nd 2 Cl 6 (μ 2 -4-NH 2 -1,2,4-Triaz) 4 (4-NH 2 -1,2,4-Triaz) 2 ], [Ce 2 Cl 4 (μ 2 -Cl) 2 (μ 2 -4-NH 2 -1,2,4-Triaz) 4 ] n , [Ce 2 (µ 2 -Cl) 4 (µ 2 -OH) 2 (µ 2 -4-NH 2 -1,2,4-Triaz) 2 ] n , [Ln 4 Cl 4 (µ 2 -Cl) 4 (µ 3 -OH) 4 (µ 2 -4-NH 2 -1,2,4-Triaz) 4 ] n •2nH 2 O (Ln = Ce, Nd), and [Ce 6 Cl 6 (µ 6 -O 0.5 )(µ 3 -Cl 0.5 ) 4 (µ 3 -Cl 0.75 ) 3 (µ 3 -OH) 0.75 (µ 2 -4-NH 2 -1,2,4-Triaz) 12 ((OH 2 ) 0.25 ) 2 ] 2 [CeCl 6 ][Cl 9 ]•xH 2 O. In all complexes all lanthanide atoms are pairwise connected via one or more 4-NH2-1,2,4-Triaz ligands and sometimes additional Cl - anions.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2019

Ambient‐Pressure Relithiation of Degraded Li x Ni 0.5 Co 0.2 Mn 0.3 O 2 (0 < x < 1) via Eutectic Solutions for Direct Regeneration of Lithium‐Ion Battery Cathodes

Abstract With the rapid growth of the lithium‐ion battery (LIBs) market, recycling and re‐use of end‐of‐life LIBs to reclaim lithium (Li) and transition metal (TM) resources (e.g., Co, Ni), as well as eliminating pollution from disposal of waste batteries, has become an urgent task. Here, for the first time the ambient‐pressure relithiation of degraded LiNi 0.5 Co 0.2 Mn 0.3 O 2 (NCM523) cathodes via eutectic Li + molten‐salt solutions is successfully demonstrated. Combining such a low‐temperature relithiation process with a well‐designed thermal annealing step, NCM523 cathode particles with significant Li loss (≈40%) and capacity degradation (≈50%) can be successfully regenerated to achieve their original composition and crystal structures, leading to effective recovery of their capacity, cycling stability, and rate capability to the levels of the pristine materials. Advanced characterization tools including atomic resolution electron microscopy imaging and electron energy loss spectroscopy are combined to demonstrate that NCM523's original layered crystal structure is recovered. For the first time, it is shown that layer‐to‐rock salt phase change on the surfaces and subsurfaces of the cathode materials can be reversed if lithium can be incorporated back to the material. The result suggests the great promise of using eutectic Li + molten–salt solutions for ambient‐pressure relithiation to recycle and remanufacture degraded LIB cathode materials.

Shi, Yang↗
DOE OSTI2022

Time-dependent THMC properties and microstructural evolution of damaged rocks in excavation damage zone

Modeling coupled thermo-hydro-mechanical-chemical (THMC) processes in host rocks near high-level nuclear waste (HLW) repositories at various time scales is an extremely challenging task. The current study integrates experimental, theoretical, and numerical methods in assessing the evolution of excavation damage zone (EDZ) over time and its implication on the long-term migration of hazardous species. Argillite and rock salt and are the focus of this study. The first part of the report presents a novel time-dependent directional microcrack damage theory for generic brittle rocks. It features detailed statistical description of the microcracks within a damaged solid, permitting a direct upscaling of microscale processes such as crack growth kinetics, crack closure/opening, sliding friction to explain the macroscopic creep, nonlinear elasticity, shear dilation, and loading-unloading hysteresis. This provides a basic platform for describing the anisotropic mechanical and transport properties of damaged rocks during excavation and subsequent THMC loadings. The model is validated and numerically implemented to Finite Element (FE) package ABAQUS through the user-defined material (UMAT) interface and have demonstrated great potential in resolving the time-dependent and anisotropic evolution of damage in the EDZ. The second part of the report presents a multi-scale experimental effort in characterizing the thermal, hydraulic, and mechanical properties of Mancos shale and Avery Island salt. For the Mancos shale, triaxial compression tests are performed at different confining pressures and temperatures to probe its thermomechanical properties relevant to HLW repositories. The obtained stress-strain data are interpreted using the proposed directional damage theory. Post-test specimens are subjected to gas permeability tests to reveal the correlation between permeability and the degree of microcracking. At microscale, temperature-controlled nanoindentation tests are performed and found a linear correlation between fracture toughness and elastic modulus from 25°C to 300°C. For Avery Island salt, we have designed and manufactured a novel relative-humidity controlled uniaxial creep device. Long-term creep tests at low stresses (< 5 MPa) are performed at different levels of relative humidity (RH). Besides confirming the much higher creep rates as one would expect through extrapolating the high-stress creep data, the results reveal that the steady-state creep rate of rock salt is strongly dependent on the ambient RH, an aspect that is often neglected in the literature. Both behaviors can be attributed to the pressure-solution creep mechanism which dominates at low stress and high RH levels. The third part of the report explores a set of numerical strategies in modeling the THMC behavior of porous geomaterials. A fully implicit, monolithic FE solution that can flexibly interface with different material models and coupling mechanisms for THMC problems is developed and verified through the ABAQUS user-defined element (UEL) interface. The scheme is used to study the THM response of a hypothetical HLW storage site with reference to an existing in-situ heater test. Strategies for integrating the UEL and the microcrack UMAT are suggested. Another numerical endeavor of this study is to implement a higher-order asymptotic homogenization method to account for the heterogeneous porous structures. The same method is then extended to perform microstructure-informed thermo-mechanical modeling of generalized continua. The above outcomes of this project provide a strong thrust towards enhancing the fundamental understanding and modeling capability of the long-term evolution of host rocks in EDZ, thus helping achieve the design goal of 1-million-year isolation of high-level nuclear wastes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Cesium Batch Contact Equilibrium Testing of Crystalline Silicotitanate (CST) Sieve Cuts in SRS Average Simulant and Examination of CST Samples Aged in Caustic and Simulant in Support of Tank Closure Cesium Removal 1A (TCCR-1A)

Batch contact testing to determine cesium equilibrium loading on Crystalline Silicotitanate ion exchange media in Savannah River Site Average Waste Simulant at 25 °C indicated that smaller diameter particles isolated by sieving pretreated CST media may load slightly higher (<10%) amounts of cesium, though the differences are within analytical uncertainty. In addition, ion exchange media sub-samples stored in 2-4 M NaOH and caustic simulant solutions for ~2.5 years were examined by optical microscopy and the 3 M NaOH sample was also analyzed to determine whether changes in the particle size distribution occurred during storage. No visual indications of particle attrition or agglomeration were observed for any sample. Particle size analysis indicated that a slight decrease occurred in the average particle diameter following contact with 3 M NaOH (541 µm average diameter versus 566 µm for the pretreated CST prior to contact). A small increase (from 0 to <0.5 wt. %) in the number of particles ranging from 271 and 322 µm was also observed for the CST sample contacted with 3 M NaOH relative to a sample of the original pretreated material. However, this small change could be due to sub-sampling differences or analytical uncertainty. It does not appear that small particles are formed to a significant degree during CST caustic contact or that small particles which do form (presumably from attrition of larger particles during pretreatment) load significantly more cesium than the bulk material. Minimal other negative consequences were observed associated with CST extended caustic or simulant contact, except for the tendency for more concentrated salt solutions to form some salt crystals which deposit on the media over time.

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DOE OSTI2019

Study on Characterization of Colloidal Silica Grout for Rock Excavation Under Saline Groundwater - 19332

A rock excavation grouting technology has been recently studied as significant technology for reducing the ingress of water into the deep repository. However, it has not been studied for applying to the coastal region, where it is discussed to be a more suitable region for the geological disposal in Japan. The latest material called colloidal silica grout (CSG) is good for sealing narrow fractures but is known to be sensitive to the salinity of groundwater because of its gelling property with salt accelerator. Although the gelling of CSG can be controlled by adding an acidic pH adjuster, the methodology for delivering the appropriate grout is not well established for such conditions of saline groundwater. Therefore, this research project was established to enhance the existing rock grouting technology for deep repositories. Initially, a grouting workshop was held with Nordic authorities in order to understand the state of the art and identify the most significant challenges to developing a generic mixing method for injecting CSG under seawater. Based on laboratory tests, we developed a feasible mixing methodology that prevents the rapid reaction with the salty water, which shows that CSG is not negatively impacted by salty mixing water or submerged by saline water. Combining the latest grouting techniques from Japan and the Nordic countries creates an optimal grouting methodology for use under seawater. Using this hybrid approach, the CSG can find wide-scale use as an agent for grouting narrow rock fractures filled with saline or fossil water in order to decrease the ingress of water in the disposal facilities. The reduction of the water ingress will enhance the safety of the repository, reduce water discharge, and diminish the long-term cost of water treatment. (authors)

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DOE OSTI2019

Molten Salt Reactor Fuel Depletion Tools in SCALE

Molten salt reactor depletion modeling and simulation tools have been implemented into the SCALE suite for reactor analysis and design developed by Oak Ridge National Laboratory. For depletion with material feeds and removals, additional removal and feed rate functionalities are being developed in ORIGEN to account for these flows during depletion. To track separate fuel and waste materials, additional functions and an iterative scheme are being added to the SCALE/TRITON lattice physics tool. The functionality of these tools has been demonstrated in part for previous analyses using external scripts that manage SCALE/TRITON calculations. Direct implementation of these functionalities into SCALE provides for a more ecient, more accurate material accountability methodology that is accessible to external SCALE users with a new input definition. These implementations are being tested for accuracy and to demonstrate their applicability to predefined molten salt reactor use case problems. This work demonstrates the capability of the SCALE modeling and simulation tools for reactor physics and fuel cycle analysis of molten salt reactor concepts.

Betzler, Benjamin↗
DOE OSTI2024

Summary of Gas Generation Behavior Observed in 3013 Surveillance and Monitoring Program Shelf-Life Experiments

Gas generation experiments have been conducted in small- and full-scale test containers at Los Alamos National Laboratory on samples of plutonium oxide material collected from plutonium processes across the DOE complex and tested at the bounding conditions for the Department of Energy 3013 Standard. The gas composition and pressures in the sealed experimental containers were measured over periods of months to years. These experiments have provided results for the formation and consumption of hydrogen and other gases. The conditions supporting the formation of flammable gas mixtures of hydrogen and oxygen in flammable gas mixtures were also determined. Different behaviors were observed between the materials tested based on their compositions, the stabilization performed on the material, and the post stabilization handling of the material. Many of the experiments are still ongoing. This report summarizes the results obtained for the gas generation behavior for high-purity plutonium oxides and salt-bearing impure plutonium oxides in sealed containers.

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NASA NTRS1977

Thermal storage for electric utilities

Applications of the thermal energy storage (TES) principle (storage of sensible heat or latent heat, or heat storage in reversible chemical reactions) in power systems are evaluated. Load leveling behind the meter, load following at conventional thermal power plants, solar thermal power generation, and waste heat utilization are the principal TES applications considered. Specific TES examples discussed include: storage heaters for electric-resistance space heating, air conditioning TES in the form of chilled water or eutectic salt baths, hot water TES, and trans-seasonal storage in heated water in confined aquifers.

Swet, C. J.↗
DOE OSTI2018

Interactions of Chemical Contaminants to Steel and Concrete Via Spectroscopic and Computational Methods - 18398

There is limited understanding of the scientific interaction of the chemical contaminants to DOE facility materials which can alter the stability of the materials, and in turn, affecting the general safety. In addition, the materials themselves can be considered secondary waste and decontamination is necessary. Therefore, the overall goal of this project is to determine the physiochemical interactions of Hg and Cs to steel and concrete using spectroscopic, adsorption and computational studies. To achieve the overall goal, this proposal has the following objectives: 1) Evaluate the physicochemical interactions of Hg and Cs to steel and concrete using spectroscopic techniques under standard conditions and 2) Evaluate the impact of environmental conditions (temp., salt content, pH, and time) on the physicochemical interactions of Hg and Cs to steel and concrete using spectroscopic techniques. Less labor intensive than traditional wet chemical analyses, spectroscopic methods have the advantage of elucidating both structural and chemical changes at the micro to nano-scale. The potential impacts of the proposed work could lead to cost effective decontamination methods, minimize secondary waste, and reduce worker exposure. (authors)

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DOE OSTI2022

Effect of sucrose on the oxidation-reduction conditions and retention of rhenium during vitrification of low-activity waste

Technetium speciation and solubility during nuclear waste vitrification are affected by oxygen partial pressure in the melt. Thus, reducing agents such as sucrose, which are routinely added to nuclear waste feeds to repress foaming, can significantly affect the volatilization of Tc and increase its retention in glass. Using Re as a surrogate for Tc, we measured the effect of sucrose addition to two low-activity waste melter feeds on the Re retention, oxygen partial pressure, and iron redox as functions of temperature. As expected, Re retention in glass increased as the sucrose content increased. Furthermore, this is attributed to sucrose reaction with nitrates and nitrites in the feed. Destruction of nitrates and nitrites reduces the salt phase fraction and thus likely promotes Re diffusion into the glass-forming melt. In agreement with available literature, we discuss that a modest increase in the sucrose content (compared to current practice) can significantly improve the Tc retention without reducing Fe 2+ to metal.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

Operational Safety and Post-Closure Safety: Investigation of their Interactions by a FEP Analysis - 18040

The consideration of operational safety for a repository for high-level waste is a challenge, since it has to integrate the dimension of long-term safety. The operator has to demonstrate on the one hand the safety of the workers in the mine and of men and environment during operation. On the other hand a proper operation of the mine has to guarantee that the state of the facility at the time of closure will be compatible with the requirements for long-term safety. To achieve this, a pre-closure safety analysis should include (a) a general description of the structures, systems, components, equipment, and process activities during the operational phase, (b) identification and a systematic analysis of naturally occurring and human-induced hazards and (c) identification and documentation of the strong relationships between operational safety and post-closure safety. In a German R and D project, a FEP catalogue for the operational phase was developed based on the national disposal concepts for clay and salt. The FEP catalogue contains analyses of the processes and events that affect the components (features) of the repository system in its entirety. The FEP catalogue was applied to identify hazards for the operational phase and to document the impacts of these FEP (including the identified hazards) on post-closure safety. (authors)

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DOE OSTI2022

Characterization of Tank 9h Salt Dissolution Batch 2C In Support of Tank Closure Cesium Removal (TCCR) 1A Batch 2 Preparations

Savannah River Mission Completion (SRMC) is currently preparing the second batch of material to be processed through the Tank Closure Cesium Removal (TCCR) 1A system. The feed for TCCR 1A consists of dissolved saltcake from Tank 9H. The third batch of salt to make up processing Batch 2 (Batch 2C) has recently been dissolved in Tank 9H and transferred to Tank 10H where it was composited with the first part of the batch (Batches 2A and 2B) in preparation for processing through the TCCR 1A unit. Savannah River National Laboratory (SRNL) received samples from the recent batch (2C) of dissolved salt for characterization.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Time Dependence of Methane Generation Rates from Saltstone

This report documents the tests performed to address the requirements listed in the Technical Request, which resulted in a Task Technical & Quality Assurance Plan (TTQAP) and a Run Plan to obtain the required information. The research expands previous scoping work to better understand methane generation in the Saltstone Disposal Facility (SDF). That scoping work demonstrated that methane is produced when sulfide-containing material is added to methylmercury (MeHg), which is found in the SDF Tank 50 feed waste. When Tank 50 waste is combined with grout premix solids dry feed ingredients of cement, slag cement, and fly ash, sulfides are released from the slag cement component of the premix. The prior testing results showed that while the concentration of total mercury was not affected in the pH 14 waste, the MeHg likely reacted with the sulfide contained in the slag. The scoping tests were performed in sealed reactors and thus, methane generation was not measured continuously; rather, it was measured after one hour and after 24 hours. After 24 hours, a large percentage of the MeHg was converted to methane, but after 1 hour only a small percentage of methane was released. It is noteworthy that the methane generation rate (MGR) was greater at the one-hour measurement. The data compiled from the scoping work needed to be expanded to better understand the generation of methane released from grout mixed with Tank 50 waste. This expanded study developed a more extensive knowledge of how and when methane is generated to inform the Documented Safety Analysis (DSA) of the SDF. As such, employing 8 sealed reactors, the methane generation time periods were extended to 2, 4, 6, 18, 30, 48, 72, and 96 hours (4 days). Results are documented herein to determine the capacity for MeHg, contained within Tank 50 salt solution (T50SS) simulant, to produce methane when mixed with saltstone dry feed ingredients, i.e., individual components (cement, slag, and fly ash) or a combination of those components.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2020

Characterization and CST Batch Contact Equilibrium Testing of Modified Tank 9H Process Supernate Samples in Support of TCCR

The Tank Closure Cesium Removal (TCCR) system uses ion exchange columns filled with crystalline silicotitanate (CST) media to process radioactive waste solutions for the removal of ¹³⁷Cs. TCCR currently focuses on dissolving Savannah River Site (SRS) radioactive tank waste (primarily sodium saltcake solids) within Tank 10H followed by at-tank ion exchange column treatment. Two supernate batches from Tank 10H have been processed through the TCCR unit and processing of a third batch is expected soon. After processing of this supernate batch, plans are to replace the CST columns and process dissolved salt solution from Tank 9H through Tank 10H and then through the new CST columns installed in the TCCR unit. The new columns are expected to contain either a media similar to an archived CST batch (IE-911) or the R9120-B CST media used in the current TCCR columns (the two materials are fundamentally the same; just different specifications, product names, and preconditioning steps). Samples of Tank 9H dissolved saltcake were received at the Savannah River National Laboratory (SRNL) and characterized. The Tank 9H supernate contained a high sodium concentration (~9.6 M Na⁺) and will require dilution to near 6 M [Na⁺] prior to processing through the TCCR unit. The cesium concentration in Tank 9H is currently significantly higher than was observed with Tank 10H. Three dilutions of the Tank 9H supernate were conducted to mimic possible dilutions that could be conducted in the tank farm prior to TCCR processing using inhibited water, sodium hydroxide, and sodium nitrate solutions. Dilution #1 was prepared by diluting the Tank 9H supernate by a factor of 1.6 with inhibited water, Dilution #2 was prepared by diluting the Tank 9H supernate by a factor of 3.7 with a mixed sodium hydroxide/sodium nitrate diluent, and Dilution #3 was prepared by also diluting by a factor of 3.7 but with sodium hydroxide only. All three dilutions have similar Na⁺ concentrations (~6 M), but Dilutions #2 and #3 contain significantly less cesium. Major and key minor components of the diluted Tank 9H supernate samples are provided in Table ES-1. Batch contact equilibrium tests were conducted with the Tank 9H dilutions and the two different CST media batches being considered for use in the new TCCR columns. Results are summarized in Table ES-2 and compared to ZAM model predictions. The highest cesium distribution coefficient and percent removal were observed with Dilution #3. IE-911 CST (an archived CST media batch) was more effective at removing cesium than the more recently prepared R9120-B CST media, though both media samples removed >88% of the cesium and the differences may not be statistically different considering the overall uncertainty. Based on the results, maximum cesium loadings were calculated for each CST media type and Tank 9H dilution. In general, maximum cesium loadings from dilutions of this supernate batch are quite high (approaching 0.1 mmol total Cs⁺/g CST for Dilution #1). The highest calculated maximum ¹³⁷Cs loading for the Tank 9H dilutions using the ZAM model with input of the tank compositions and batch contact results was 207 Ci/kg CST (Dilution #1 with IE-911 CST). In all cases, higher maximum cesium loading values were predicted for IE-911 CST versus R9120-B, although the differences varied considerably between the dilutions. The maximum loading value for IE-911 CST with Tank 9H Dilution #1 was only 7% higher than the maximum loading for R9120-B. The maximum loading value for IE-911 CST with Dilution #3 was 24% higher than the maximum loading for R9120-B. Dilution #2 was intermediate between these values. Note that these maximum loading values are the theoretical calculated values, and actual operating conditions will cause differences. A CST binder dilution (correction) factor near 0.7 (relative to pure powder CST) was required for each batch contact test with IE-911 engineered CST using the three Tank 9H dilutions. Correction factors calculated for R9120-B CST ranged from 0.56 to 0.66 for the three dilutions. Following the batch contact tests, the CST samples were isolated from the Tank 9H solution, washed, dried, and digested in acid following established procedures. The analysis results are provided in Table ES-3. Total cesium loading values determined by CST digestion were similar to the calculated loading values based on solution analysis (Table ES-2) for all samples. In addition, the CST was observed to load calcium (R9120-B sample only), iron, strontium, lead, uranium, and plutonium after contact with the waste supernate, as has been observed previously.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

Investigation of Tank 241-AW-104 Composite Floating Layer

Seven grab samples and one field blank were taken June 2, 2017. A visible layer with brown solids was observed floating on the top of two surface tank waste samples (4AW-17-02 and 4AW 17 02DUP). The floating layers were collected, composited, and submitted for chemical analyses and solid phase characterization in order to understand the composition of the floating layer. Tributyl phosphate and tridecane were higher in the floating layer than in the aqueous phase. Density in the floating layer was slightly lower than the mean density of all grab samples. Sodium nitrate and sodium carbonate were major components with a trace of gibbsite and very small size agglomerates were present in the solids of the floating layer. The supernate consisted of organics, soluble salt, and particulates. These agglomerates include uranium extruded from the supernate by the floating organics.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

Study on the Extraction of Aluminum From Aluminum Dross Using Alkali Roasting and Subsequent Synthesis of Mesoporous γ-Alumina

This study presents a process for recovering aluminum from aluminum dross (an industrial waste product) via an alkali roasting process and using it to synthesize mesoporous γ-alumina. The results show that the inherent chlorides in dross (KCl and NaCl) reduce Al extraction efficiency and should be removed first by water leaching. Use of salt-free dross increases the Al extraction rate (from 85 to 96 pct) within 90 minutes alkali roasting at 923 K (650 °C). In addition, an ammonium bicarbonate byproduct can be obtained from water leaching due to the hydrolysis of AlN, which can be used as a precipitating agent in the boehmite sol preparation. Synthesis of mesoporous γ-alumina was carried out by the sol-gel method with EO{sub 20}PO{sub 70}EO{sub 20} (P123) as a template. The prepared mesoporous γ-alumina was characterized as having a disordered mesostructure with a high pore volume of 1.02 cm{sup 3}/g and surface area of 312 m{sup 2}/g. Thus, we achieved highly efficient utilization of aluminum dross and yielded products with high added value. Mesoporous γ-alumina has potential applications in environmental remediation and catalysis.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Cradle-to-Grave: Assessment Methods for Hazardous Waste Management

The Resource Conservation and Recovery Act (RCRA) was passed to set up a framework for the proper management of waste. The 40CFR260-273 regulation established the regulatory framework to handle solid and hazardous waste, from the point of generation to its disposal; or cradle-to-grave management. Per these regulations, a hazardous waste generator is responsible for its waste from initial generation through its ultimate disposal and beyond. Nothing will relinquish a generator of this responsibility. There is no expiration date or time limit, and hiring a someone else to transport and dispose of waste does not transfer responsibility. If an incident occurs at any point during the life cycle of a waste, the generator can be held liable. The first step to compliance with RCRA is proper characterization of the waste. Waste may either be listed specifically or may show a characteristic as defined in the regulation: Is my waste hazardous? Why is it Hazardous? What should I do as a generator? Plan chemical use: - Create a chemical inventory for your research project. - Use existing chemicals if available instead of ordering new ones. - Brainstorm methods that will help to reduce toxicity and minimize waste. Waste Inventory: - Label all waste bottles with: ID no., What is it, Whose is it, Hazards, and Date. - Add waste containers into the inventory log. - Initiate/complete the container sheet to describe the waste. Satellite Areas: - Store waste in containers compatible with the waste with lids on tight. - Store waste containers properly and segregate them according to their specific hazards. - Use secondary containment for liquids. Store acids and bases separately; apart from cyanides or sulfides. Acids should never be put into steel containers. Water-reactive, strong acids such as organic acid halides, organic acid anhydrides, inorganic acid anhydrides, and strong acidic salts must be kept apart from both alkalis and water. Oxidizing agents must be kept apart from reducing agents and organic compounds. Water-reactive agents must be stored apart from water, aqueous solutions, and acids. Air-reactive materials must be packed in containers that are sealed off from the atmosphere. Explosive and shock-sensitive materials present risks that require special handling.

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DOE OSTI2022

Leveraging Multiple Raman Excitation Wavelength Systems for Process Monitoring of Nuclear Waste Streams

Processing nuclear waste from sites such as Hanford is a significant environmental cleanup need while being a significant logistical challenge. Integration of process monitoring tools, that can provide in situ and real-time feedback about the process, can significantly alleviate needs to collect grab samples for process control and product characterization. Raman spectroscopy paired with chemometric analysis is one process monitoring tool that can provide chemical composition information on a large number of chemical targets in nuclear waste streams. However, methods to improve limits of detection as well as drop uncertainty in quantification are needed. Optimizing instrument specifications can achieve this, here this is demonstrated by comparing limits of detection for key analytes when using Raman systems with 671 nm, 532 nm, and 405 nm excitation wavelengths. Generally, limits of detection decease (allowing the measurement of lower salt concentrations) with decreasing wavelength. Similarly, data collection times and averaging were optimized. Finally, multiple chemometric modeling approaches were leveraged, including multiblock methods that combined data from all three Raman systems to simultaneously quantify targets with improved sensitivity.

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