Plutonium Packaging
This report is the plutonium packaging portion of the ADPSM plutonium engineering lecture series.
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Technical Basis for Extending Storage Life of DOE-STD-3013 Containers
The U.S. Department of Energy (DOE) Technical Standard for Stabilization, Packaging, and Storage of Plutonium-Bearing Materials, DOE-STD-3013 [USDOE 2018], provides requirements for packaging stabilized metals, alloys, and oxides containing at least 30 weight percent (wt%) plutonium (Pu) plus uranium for storage for up to 50 years. This document provides the technical basis for extending that storage duration to up to 100 years for metals and alloys, and oxides that do not present a corrosion risk to the integrity of the container.
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Destructive Examination Protocol for 3013-Container-Package Storing Plutonium-Bearing Materials
The 3013-container-package consists of a convenience, inner and outer container and is used for long-term storage of plutonium-bearing materials. A destructive examination (DE) protocol has been developed to examine the container package visually and with microscopic aid to find any corrosion conditions that could result in the loss of the integrity of the container package over its lifetime. The DE protocol contains three main steps: initial container examination, helium (He) leak testing, and detailed imaging and analysis of the inner container closure weld region (ICCWR). The ICCWR has been determined to be bounding, defined as exhibiting worst case conditions for stress corrosion cracking (SCC) of the inner container. To assess SCC in the ICCWR, the inner container lid is cut into quarters and the weld and He-leak testing gasket are removed. Then a citric acid wash is performed to remove adherent chlorides from the ICCWR. The wash is then sent for analysis to determine the concentration of chlorides in the ICCWR. While the analysis for chloride concentration is being performed, the quarter sections are further sectioned into 1/8th subsections by cutting each section in half. These subsections are washed using nitric acid to remove corrosion products. Then each subsection is imaged using a Wide Angle 3-D Measurement System (WAMS). After analysis of microscope images for potential SCC, additional imaging can be performed, including subsurface imaging. After review, a determination is made of whether the container integrity may potentially affect the safe storage of the material.
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3013 Baseline Inner Container Report: Description, Imaging, and Analysis
This report presents consolidated findings from three microscopy studies of baseline Bagless Transfer Containers (BTCs), which are the inner containers used in DOE Standard 3013-compliant plutonium storage packages. The studies were conducted by Los Alamos National Laboratory (LANL), Savannah River National Laboratory (SRNL), and DNV, a subcontractor specializing in corrosion science. The baseline BTCs examined had not been exposed to corrosive environments, serving as control samples for comparison with destructively examined (DE) containers. Additionally, the Background section provides an overview of the BTC design, including manufacturing methods, material properties, and container configurations that may influence corrosion behavior. The primary objective of the LANL and SRNL studies was to establish reference characteristics of BTCs to distinguish manufacturing artifacts from corrosion-induced features observed in DE containers. Both laboratories used advanced microscopy techniques, including Wide Area Microscopy (WAMS), Laser Confocal Microscopy (LCM), Scanning Electron Microscopy (SEM), and Focused Ion Beam (FIB), to reveal that most surface anomalies were shallow and attributable to flow-forming processes, not corrosion. Subsurface impurities, identified as non-metallic inclusions, were also observed. DNV’s investigation focused on characterizing the mechanical and chemical properties of the BTC material to support crack growth modeling. Their findings indicate higher hardness and strength but reduced ductility—consistent with flow-formed 304L stainless steel and a higher-than-expected martensite content, in contrast to manufacturer claims. Ongoing and future studies, including Electron Backscatter Diffraction (EBSD), aim to further understand the microstructural factors influencing crack initiation and propagation. The combined studies provide a crucial baseline for distinguishing corrosion effects in DE containers, contributing to the safe and reliable long-term storage of plutonium-bearing materials.
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The SAVY 4000 Container Storage Program at Los Alamos National Laboratory - 17313
Incidents involving release of nuclear materials stored in containers of convenience such as food pack cans, slip lid taped cans, paint cans, etc. has resulted in the U.S. Defense Nuclear Safety Board concerns over the lack of prescriptive performance requirements for interim storage of nuclear materials. Los Alamos National Laboratory (LANL) has shared in these incidents and in response proactively moved into developing a performance based storage container design, the SAVY-4000{sup R}. The SAVY-4000{sup R} is the first vented general use nuclear material container demonstrated to meet the requirements of DOE M 441.1-1, Nuclear Material Packaging Manual. The SAVY-4000{sup R} is an innovative and creative design demonstrated by the fact that it can be opened and closed in a few seconds without torque wrenches or other tools; has a built-in, fire-rated filter that prevents the build-up of hydrogen gas, yet retains 99.97% of plutonium particulates, and prevents release of material even in a 12 foot drop. Finally, it has been fire then drop tested and will reduce the risk to the public in the event of an earthquake/fire scenario. This will allow major nuclear facilities to credit the container towards source term Material at Risk (MAR) reduction. The container was approved for nuclear material storage in the TA-55 Plutonium Facility on March 15, 2011, and there are currently over 2000 SAVY-4000{sup R} containers available for use within the facility. A Safety Analysis Report was developed to demonstrate Manual 441.1-1 compliance and was approved April, 2014. The first four SAVY-4000{sup R} containers were packaged with plutonium on August 2, 2011. Key aspects of the SAVY-4000{sup R} vented storage container design will be discussed which include design description, qualification and testing, surveillance strategy, and the design life extension program as enhanced by surveillance activities with the intent to extend well beyond the current five year design life. (authors)
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He Leak Testing of 3013 Inner Container Lids
The 3013-container package is used for the long-term storage of plutonium bearing materials at Department of Energy (DOE) sites. The package consists of three nested stainless-steel containers: outer, inner and convenience, which are made of stainless steel. The requirements of the DOE 3013 Standarda, also entail the development of a surveillance program, tasked to ensure structural integrity of the outer container for at least 50 years. The Materials Identification and Surveillance Working Group (MIS-WG) is specified to be responsible for selecting the containers for the surveillance as well as analyzing results. The MIS-WG determined that corrosion is a potential mechanism for container degradation with the most credible type of failure to be stress corrosion cracking (SCC) through wall breach of the inner container closure weld region (ICCWR). A breach of the inner container has the potential of allowing corrosive gases to be released into the safety class outer container.
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Characterization of Stress-Corrosion-Cracking in Plutonium-Bearing Storage Containers
Introduction • The Integrated Surveillance Program, under the Department of Energy, is responsible for the periodic surveillance of storage containers containing plutonium-bearing materials. • The container-packages are designed to isolate the materials for 50 to 100 years with minimal surveillance. • During monitoring, corrosion-pitting and stress-corrosion-cracking (SCC) has been identified in some of the inner-cans near the weld regions. • SCC through wall penetration would result in an undesired increased risk of leakage. • An investigation is in progress to identify and characterize corrosion events to determine the prevalence of corrosion features and the likelihood of a throughwall breach. • Here, we discuss the characterization efforts carried out by Scanning Electron Microscopy (SEM), including 3D-tomography by Focused Ion Beam (FIB) methods.
Perez, Emmanuel E.↗
Comparing elemental measurements at packaging and after storage for signatures of chloride salt radiolysis
Radiolysis of hydrated alkaline earth chloride salts by alpha radiation from plutonium produces the chloride containing gases HCl and Cl 2 . These gases are known to diffuse out of the plutonium-containing material and contribute to corrosion outside of the convenience container. The alkaline earth elements remain with the plutonium-containing material as oxides or hydroxides. The amount of chlorine within the material after storage will be reduced compared to the amount at packaging. The fraction of the alkaline earth elements that are soluble after storage will be reduced compared to the amount at packaging. These signatures may be observable by comparing the chemical analysis measurements made at packaging and after storage. Comparison of measurements on a single Hanford container shows that the chloride does decrease and the alkaline earth elements have reduced solubility in water. Differences seen with other elements make conclusions difficult.
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Thermal Testing of Waste Packages for a Storage Environment
The Pipe Overpack Container (POC) was developed at Rocky Flats to transport plutonium residues with higher levels of plutonium than standard TRU waste to the Waste Isolation Pilot Plant (WIPP) for disposal. The POC consists of an inner Pipe Container (PC) surrounded by organic fiber dunnage inside of a 7A drum. The PC was design to maintain separation of fissile material and to provide shielding from radiation. The POC has many design features that are similar to Type B packages that do provide protection from engulfing fires. However, it was not specifically designed to prevent release of stored material during a long-duration fire. POCs are now being used to store combustible TRU waste at Department of Energy (DOE) sites (e.g., Waste Isolation Pilot Plant). Radioactive waste storage operators would like to be able to claim some level of protection is provided by the POCs for thermal assaults that could occur within storage facilities when these POCs contain PCs with combustibles. In 1997 Sandia National Laboratories (SNL) conducted a series of tests to determine the degree of protection POCs provide during storage accident events. One of these tests exposed four of the POCs to a 30-minute engulfing pool fire, resulting in one of the 7A drums generating sufficient internal pressure to pop off its lid and expose the top of the PC to the fire environment. However, these tests are not bounding for POC/PC containing combustibles. With the addition of combustible materials in the PC, the possibility exists for generation of higher quantities of gases and much higher pressures inside the PC, which can lead to early rupture of the PC filter and higher radioactive aerosol release fractions. Therefore, a new series of tests was required to determine the temperature response of the exposed PC and determine the amount of material that could be released. DOE contacted SNL in 2015 to discuss the 1997 SNL tests and came to the conclusion that those tests were not bounding for POC/PC containing combustibles Therefore, DOE commission a new set of tests at SNL. Starting in 2015, SNL conducted fire tests to examine whether the contents of the PC would reach a temperature that would result in generation of sufficient gas to cause overpressurization of the PC, and subsequent release of its content. This paper will describe the various test conducted thus far, and present preliminary results from these tests.
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Effect of ionizing radiation on PuO2 and surrogate oxide materials under storage conditions
The stockpile of plutonium separated from used nuclear fuel amounts to many 100s of tonnes. The majority of this plutonium is stored as PuO2 powder packaged in multi-can containers. The conditions during the packaging of reprocessed PuO2 for long term storage are closely controlled to limit water uptake as radiolytic decomposition of any adsorbed water will lead to the formation of both a potentially flammable atmosphere containing molecular hydrogen as well as reactive oxygen species which may be incorporated into the oxide phase. Consequently, the safety case for the long-term storage of PuO2 requires a complete understanding of the fundamental physical, chemical and materials degradation processes occurring at the water-oxide interface inside the storage canisters. This study investigates the effect of ionizing radiation on PuO2 and various surrogate oxides under atmospheres potentially encountered in storage canisters.
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Packaging Plan for Mark-18A Plutonium Oxide
Mark-18A (Mk-18A) targets were irradiated at the Savannah River Site and have been in wet storage at the site since the 1970s. The Mk-18A Target Material Recovery Program has been established to recover the 244 Pu and heavy curium (≥50% 246 Cm and 248 Cm) in the targets at the Savannah River National Laboratory (SRNL) and ship the materials to Oak Ridge National Laboratory’s (ORNL’s) Radiochemical Engineering Development Center for programmatic use. Two products will be recovered from the Mk- 18A targets for shipment from SRNL to ORNL: a plutonium oxide stream and an oxide material that will contain the americium, curium, and lanthanides. This document presents the plan for packaging of the plutonium oxide material for shipment and storage at ORNL.
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Surveillance and Monitoring Program Full-Scale Experiments to Evaluate the Potential for Corrosion in 3013 Containers
A set of six long-term, full-scale experiments were initiated to determine the type and extent of corrosion that occurs in 3013 containers packaged with chloride-bearing plutonium oxide materials. The materials were exposed to a high relative humidity environment representative of actual packaging conditions for the materials in storage. The materials were sealed in instrumented, inner 3013 containers with corrosion specimens designed to test the corrosiveness of the environment inside the containers under various conditions. This report focuses on initial loading conditions that are used to establish a baseline to show how the conditions change throughout the storage lifetime of the containers.
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Evaluation of the 2018 Version of the Integrated Surveillance Program Database Pressure Equation
The Integrated Surveillance Program (ISP) Database Pressure Equation was developed to determine with reasonable certainty the total maximum pressure of hydrogen and other gases in packaged 3013 containers stored at Savannah River Site (SRS) in support of the destructive evaluation (DE) process. The pressure equation in the Department of Energy (DOE) 3013 Standard, “Standard for Stabilization, Packaging and Storage of Plutonium- Bearing Materials” (DOE-STD-3013-2004) used a bounding assumption that all the water is decomposed to form hydrogen. However, the results of Los Alamos National Laboratory (LANL) shelf-life experiments showed that hydrogen is consumed, and that the maximum pressures would not approach the design pressure of the 3013 container. Therefore, the ISP Database Pressure Equation was revised in 2008 to include terms for the generation of helium and hydrogen as a function of time, as well as the consumption of water and destruction of hydrogen based on shelf-life results. The 2008 ISP Database Pressure Equation provided a more reasonable estimate of the total maximum pressure in packaged 3013 containers than the pressure equation in versions of the 3013 Standard issued prior to 2018.
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Residual Stresses and Other Properties of Teardrops
The Department of Energy’s 3013 Standard for packaging plutonium-bearing materials for storage up to fifty years specifies a minimum of two individually welded, nested containers herein referred to as the 3013 outer and the 3013 inner.1 Stress corrosion cracking (SCC) is a potential failure mechanism for 3013 inner containers.2,3 The bagless transfer container (BTC), a 3013 inner container used by Hanford and Savanna River Site (SRS) made from 304L stainless steel (SS), poses the greatest concern for SCC.4,5 The Surveillance and Monitoring Program (SMP) use stressed metal samples known as teardrops as screening tools in SCC studies to evaluate factors that could result in cracks in the 3013 containers.6,7 This report provides background information on the teardrops used in the Los Alamos National Laboratory (LANL) SMP studies including method of construction, composition and variability. In addition, the report discusses measurements of residual stresses in teardrops and compares the results with residual stresses in BTCs reported previously.4 Factors affecting residual stresses, including teardrop dimensions and surface finish, are also discussed.
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Development and Implementation of a Bag Degradation Predictive Tool at Los Alamos National Laboratory
Nuclear material packaging involves many complex variables derived from the stored material's properties, the storage environment, and the synergistic interaction of said material and its environment on the containment boundary. In the Plutonium Facility (PF-4) at Los Alamos National Laboratory (LANL) the typical containment boundary found, starting from the stored material itself to the outermost containment layer, consists of the material contained within a stainless steel (typically 304) slip-lid (or other equivalent stainless steel packaging layer) wrapped in an sPVC bag-out bag contained within a facility approved outer container stored within the boundaries of an approved facility (i.e., a building designed and approved to store nuclear material). This packaging configuration, though occasionally deviated from in the past, represents the current procedurally enforced, expected containment structure for all interim nuclear material containment outside of an engineered control barrier (e.g., a glovebox). Over the life of containerization research at LANL, packaging engineers have become increasingly concerned with the degradation of the sPVC bag-out bag, which can cause corrosion to the outermost packaging layer as well as possible exposure to alpha contamination if the bag-out bag layer is degraded to the point of containment failure. A bag-out bag degradation predictive tool (BDT) is therefore needed to assess the current and future nuclear material inventory for possible bag degradation in order to continue to ensure safe operations for the facility and its workers to deliver on the vital national security mission of 30 PPY.
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Lab touts plutonium storage best practices for Japanese visitors
Engineers from Japan's Oarai Research and Development Center's Plutonium Fuel Research Facility visited TA-55's Plutonium Facility 4 (PF-4) recently to learn best practices from the Laboratory for safely packaging and storing plutonium and other radioactive materials.
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Plutonium-238 Loadout Calorimeter Return To Service
The calorimeter in the transfer area in Building 7920 at the US Department of Energy’s Oak Ridge National Laboratory is used to measure the amount of 238 Pu in the Plutonium Heat Source Oxide. The calorimetry measurement is taken after the oxide is packaged in an ORISC (Oak Ridge Inner Shipping Capsule)/FSO (Fuel Storage Outer) assembly before loading into the Containment Vessel and shipping container. The equipment is used in three specific configurations: zero measurement (nothing in the sample cup), FSO measurement (actual measurement of 238 Pu), and reference calibration measurement (using the reference FSO as a known heat source). System checks were performed in July 2023 in preparation for scheduled material loadout. During these checks, personnel discovered that the reference FSO had experienced an electrical short in the heater cable and was no longer functional. The calorimeter was in the reference calibration measurement configuration at this time. Facility management was notified when the damage was discovered. The data from the Yokogawa recorder were pulled and analyzed for a span of time between September 2022 and July 2023. An unusual spike was found in the sample cup temperature data that started on October 19, 2022, and ended on October 20, 2022. The sample cup reached a temperature of 191.1°C. The maximum allowable temperature for the calorimeter thermopile to reach is 220°C based on the manufacturer statement provided in Appendix B of this report [1]. The calorimeter thermopile and the sample cup thermocouple are physically close to each other; therefore, the data suggest that the calorimeter itself never saw a temperature in excess of 191.1°C. Physical damage present on the cable, tape, and insulation suggests that the temperature reached a higher value in some locations within the sample cup than the data shows. Because of this discrepancy, testing of the calorimeter was required to confirm that the calorimeter is functioning the same as it was before the electrical short. The intent of this report is to assess the functionality of the calorimeter and determine if it is acceptable to use for 238 Pu loadout material measurement. Testing showed that the calorimeter is functionally equivalent to the initial calibration that was performed in the summer of 2021, and thus, the calorimeter was cleared to be used for its intended purposes.
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SAVY-4000 Corrosion Evaluation Plan
Nuclear material packages, with few exceptions, outside of an approved engineered contamination barrier must meet packaging, surveillance, and testing requirements designed to protect workers from airborne contamination per Department of Energy (DOE) Manual 441.1-1, Nuclear Material Packaging. The SAVY-4000 containers were developed at Los Alamos National Laboratory (LANL) in conjunction with Nuclear Filter Technology Inc. (NFT Inc.) as a general purpose vented manually-compliant container system for staging and storage of plutonium for LANL and the DOE complex. The SAVY-4000 containers have a 316L stainless steel containment barrier, which was selected based on its corrosion resistant properties. These containers were approved for use in 2014 with a five-year design life; LANL requested and DOE has approved lifetime extension from 5 to 15 years. The 10-year lifetime extension was proposed as a conservative recommendation based on the corrosion observations for the metal components in surveillance and results from laboratory studies. Extensive accelerated aging studies have been done on the SAVY-4000 O-ring with very little evidence of significant degradation when subjected to aggressive elevated temperature and radiation conditions. Therefore, our current conservative lifetime estimate for the O-ring and the filter is 40 years at 80°C. Additional work is ongoing in a phased approach to further extend the design life of the Manual compliant SAVY-4000 storage container; the limiting component for further life extension is still the 316L containment barrier.
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