THERMAL GRADIENT WITHIN DOE 3013 CONTAINERS DURING STORAGE
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Hensel, S.↗
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Technical Basis for DOE Standard 3013 Equivalency Supporting Reduced Temperature Stabilization of Oxalate-Derived Plutonium Oxide Produced by the HB-Line Facility at Savannah River Site
The HB-Line (HBL) facility at the Savannah River Site (SRS) is designed to produce high-purity plutonium dioxide (PuO 2 ) which is suitable for future use in production of Mixed Oxide (MOX) fuel. The MOX Fuel Fabrication Facility (MFFF) requires PuO 2 feed to be packaged per the U.S. Department of Energy (DOE) Standard 3013 (DOE-STD-3013) to comply with the facility's safety basis. The stabilization conditions imposed by DOE-STD-3013 for PuO 2 (i.e., 950 °C for 2 hours) preclude use of the HBL PuO 2 in direct fuel fabrication and reduce the value of the HBL product as MFFF feedstock. Consequently, HBL initiated a technical evaluation to define acceptable operating conditions for production of high-purity PuO 2 that fulfills the DOE-STD-3013 criteria for safe storage. The purpose of this document is to demonstrate that within the defined operating conditions, the HBL process will be equivalent for meeting the requirements of the DOE-STD-3013 stabilization process for plutonium-bearing materials from the DOE complex. The proposed 3013 equivalency reduces the prescribed stabilization temperature for high-purity PuO 2 from oxalate precipitation processes from 950 °C to 640 °C and places a limit of 60% on the relative humidity (RH) at the lowest material temperature. The equivalency is limited to material produced using the HBL established flow sheet, for example, nitric acid anion exchange and Pu(IV) direct strike oxalate precipitation with stabilization at a minimum temperature of 640 °C for four hours (h). The product purity must meet the MFFF acceptance criteria of 23,600 µg/g Pu (i.e., 2.1 wt %) total impurities and chloride content less than 250 µg/g of Pu. All other stabilization and packaging criteria identified by DOE-STD-3013-2012 or earlier revisions of the standard apply. Based on the evaluation of test data discussed in this document, the expert judgment of the authors supports packaging the HBL product under a 3013 equivalency. Under the defined process conditions and associated material specifications, the high-purity PuO 2 produced in HBL presents no unique safety concerns for packaging or storage in the 3013 required configuration. The PuO 2 produced using the HBL flow sheet conditions will have a higher specific surface area (SSA) than PuO 2 stabilized at 950 °C and, consequently, under identical conditions will adsorb more water from the atmosphere. The greatest challenge to HBL operators will be controlling moisture content below 0.5 wt %. However, even at the 0.5 wt % moisture limit, the maximum acceptable pressure of a stoichiometric mixture of hydrogen and oxygen in the 3013 container is greater than the maximum possible pressure for the HBL PuO 2 product.
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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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Characterization of Representative Materials in Support of Safe, Long Term Storage of Surplus Plutonium in DOE-STD-3013 Containers
The Surveillance and Monitoring Program is a joint Los Alamos National Laboratory/Savannah River Site effort funded by the Department of Energy-Environmental Management to provide the technical basis for the safe, long-term storage (up to 50 years) of over 6 metric tons of plutonium stored in over 5,000 DOE-STD-3013 containers at various facilities around the DOE complex. The majority of this material is plutonium that is surplus to the nuclear weapons program, and much of it is destined for conversion to mixed oxide fuel for use in US nuclear power plants. The form of the plutonium ranges from relatively pure metal and oxide to very impure oxide. The performance of the 3013 containers has been shown to depend on moisture content and on the levels, types and chemical forms of the impurities. The oxide materials that present the greatest challenge to the storage container are those that contain chloride salts. Other common impurities include oxides and other compounds of calcium, magnesium, iron, and nickel. Over the past 15 years the program has collected a large body of experimental data on 54 samples of plutonium, with 53 chosen to represent the broader population of materials in storage. This paper summarizes the characterization data, moisture analysis, particle size, surface area, density, wattage, actinide composition, trace element impurity analysis, and shelf life surveillance data and includes origin and process history information. Limited characterization data on fourteen nonrepresentative samples is also presented.
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Technical Basis for DOE Standard 3013 Equivalency Supporting Reduced Temperature Stabilization of Oxalate-Derived Plutonium Dioxide Produced by the HB-Line Facility at Savannah River Site
This report documents the technical basis for determining that stabilizing highpurity PuO 2 derived from oxalate precipitation at the SRS HB-Line facility at a minimum of 625 °C for at least four hours in an oxidizing atmosphere is equivalent to stabilizing at a minimum of 950 °C for at least two hours as regards meeting the objectives of stabilization defined by DOE-STD-3013 if the material is handled in a way to prevent excessive absorption of water.
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Fire-Induced Pressure Response and Failure Characterization of PCV/SCV/3013 Containers - Phase 3
Several Department of Energy (DOE) facilities have materials stored in robust, welded, stainless - steel containers with presumed fire - induced pressure response behaviors. Lack of test data related to fire exposure requires conservative safety analysis assumptions for container response at these facilities. This conservatism can in turn result in the implementation of challenging operational restrictions with costly nuclear safety controls. To help address this issue for sites that store DOE 3013 stainless - steel containers, a series of ten tests were undertaken at Sandia National Laboratories. The goal of this test series was to obtain the response behavior for various configurations of DOE 3013 containers with various payload compositions when exposed to one of two ASTM fire conditions. Key parameters measured in the test series included identification of failure - specific characteristics such as pressure, temperature, and whether or not a vessel was breached during a test . Numerous failure - specific characteristics were identified from the ten tests. This report describes the implementation and execution of the test series performed to identify these failure - specific characteristics. Discussions on the test configurations, payload compositions, thermal insults, and experimental setups are presented. Test results in terms of pressurization and vessel breach (or no - breach) are presented along with corresponding discussions for each test.
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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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Corrosion Testing of 304L SS 3013 Inner Container and Teardrop Samples
The Department of Energy (DOE) 3013 Standard specifies a minimum of two containers to be used for the storage of plutonium-bearing materials containing at least 30 wt.% plutonium and uranium. Three nested containers are typically used, the outer, inner, and convenience containers, shown in Figure 1. Both the outer and inner containers are sealed with a weld while the innermost convenience container must not be sealed. Lifetime of the containers is expected to be fifty years. The containers are fabricated of austenitic stainless steels (SS) due to their high corrosion resistance. Potential failure mechanisms of the storage containers have been examined by Kolman and Lillard et al.
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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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LANL Response to SRS Requirement G-ESR-G-00035 Item 11 Bed Temperature Requirements, For the Addition of Direct Metal Oxidation Unit 3, Revision 0
Los Alamos National Laboratory has identified a number of plutonium-bearing materials that will be placed in storage in 3013 containers per requirements of DOE-STD-3013-2004, or DOE-STD-3013-2012 when it is implemented in the LANL contract. Before these items can be considered for storage at Savannah River Site, 20 points of agreement, described in Savannah River Site (SRS) document G-ESR-G-00035, Revision 1, must be documented and provided to SRS for review. These agreements include documentation that the requirements of the 3013 Standard are met and the storage facility’s safety envelope is not compromised. Point 11 of the 20 points is the requirement that material be stabilized at 950°C for a minimum of two hours prior to packaging. This report addresses the Point 11 requirement, describing the controls used during stabilization to ensure that the material is properly stabilized using a continuous process (Advanced Recovery and Integrated Extraction System [ARIES] direct metal oxidation [DMO] and recycle oxide calcination). These controls include verification of the furnace controller thermocouple profile and verification of the profiles for the calciner tube hot zone. This report is specific to Direct Metal Oxidation Unit 3 (DMO-3). The point 11 requirements for DMO-2 and muffle furnace oxidation are covered in reference. This report does not replace reference. The process and methodology used in this report are similar to that used for Direct Metal Oxidation Unit 2, or DMO-2, as documented in reference. This report documents the performance for ARIES DMO-3. The temperature on the outside of the calciner tube must be at least 1,032°C. The auger rotation rate set point will be dependent on the pitch of the installed auger. For an auger pitch of 1.297 in/rev the auger set point will be 0.0777 rpm or less, which allows for at least 132 minutes calcination time based on worst case conditions (i.e., lowest possible powder density at the lowest initial powder temperature, and under the least favorable heat transfer conditions, and with the least favorable auger pitch of the currently installed auger.) A new auger design may be used in future modifications of DMO-3 that has an auger pitch of 1.400 ± 0.025 inches which would change the required auger set point to 0.0707 rpm or less.
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LANL Response to SRS Requirement G-ESR-G-00035 Item 11 Bed Temperature, Revision 4
Los Alamos National Laboratory has identified a number of plutonium-bearing materials that will be placed in interim storage in 3013 containers per requirements of DOE-STD-3013- 2004, or DOE-STD-3013-2012. Before these items can be considered for storage at Savannah River Site, 20 points of agreement, described in Savannah River Site (SRS) document G-ESR-G-00035, Revision 1, must be documented and provided to SRS for review. These agreements include documentation that the requirements of the 3013 Standard are met and the storage facility’s safety envelope is not compromised. Point 11 of the 20 points is the requirement that material be stabilized at 950°C for a minimum of two hours prior to packaging. This report addresses the Point 11 requirement, describing the controls used during stabilization to ensure that the material is properly stabilized using either a batch (calciner boat) or continuous process (Advanced Recovery and Integrated Extraction System [ARIES] direct metal oxidation unit 2 [DMO-2] and recycle oxide calcination). These controls include verification of the furnace controller thermocouple profile and verification of the profiles for the two thermocouples located in the bed and/or calciner tube hot zone. Revision 4 to this document only modifies the ARIES DMO-2 process controls. Batch processing requirements are unchanged. Changes to the DMO-2 process include use of alternate augers with differing pitch values and reduction of the minimum powder bulk density value. The new DMO-3 unit requirements are covered in a separate document.
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HB-Line Plutonium Oxide Data Collection Strategy
HB-Line and H-Canyon will handle and process plutonium material to produce plutonium oxide for feed to the Mixed Oxide Fuel Fabrication Facility (MFFF). However, the plutonium oxide product will not be transferred to the MFFF directly from HB-Line until it is packaged into a qualified DOE-STD-3013-2012 container. In the interim, HB-Line will load plutonium oxide into an inner, filtered can. The inner can will be placed in a filtered bag, which will be loaded into a filtered outer can. The outer can will be loaded into a certified 9975 with getter assembly in compliance with onsite transportation requirement, for subsequent storage and transfer to the K-Area Complex (KAC). After DOE-STD-3013-2012 container packaging capabilities are established, the product will be returned to HB-Line to be packaged into a qualified DOE-STD-3013-2012 container. To support the transfer of plutonium oxide to KAC and then eventually to MFFF, various material and packaging data will have to be collected and retained. In addition, data from initial HB-Line processing operations will be needed to support future DOE-STD-3013-2012 qualification as amended by the HB-Line DOE Standard equivalency. As production increases, the volume of data to collect will increase. The HB-Line data collected will be in the form of paper copies and electronic media. Paper copy data will, at a minimum, consist of facility procedures, nonconformance reports (NCRs), and DCS print outs. Electronic data will be in the form of Adobe portable document formats (PDFs). Collecting all the required data for each plutonium oxide can will be no small effort for HB-Line, and will become more challenging once the maximum annual oxide production throughput is achieved due to the sheer volume of data to be collected. The majority of the data collected will be in the form of facility procedures, DCS print outs, and laboratory results. To facilitate complete collection of this data, a traveler form will be developed which identifies the required facility procedures, DCS print outs, and laboratory results needed to assemble a final data package for each HB-Line plutonium oxide interim oxide can. The data traveler may identify the specific values (data) required to be extracted from the collected facility procedures and DCS print outs. The data traveler may also identify associated criteria to be checked. Inevitably there will be procedure anomalies during the course of the HB-Line plutonium oxide campaign that will have to be addressed in a timely manner.
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Re-evaluation of Moisture Controls During ARIES Oxide Processing, Packaging and Characterization
DOE-STD-3013 [1] requires limiting the relative humidity (RH) in the glovebox during processing of the oxide product for specific types of plutonium oxides. This requirement is mandated in order to limit corrosion of the stainless steel containers by deliquescence of chloride salts if present in the PuO2. DOE-STD-3013 also specifies the need to limit and monitor internal pressure buildup in the 3013 containers due to the potential for the generation of free H2 and O2 gas from the radiolysis of surfaceadsorbed water. DOE-STD-3013 requires that the oxide sample taken for moisture content verification be representative of the stabilized material in the 3013 container. This is accomplished by either limiting the time between sampling and packaging, or by control of the glovebox relative humidity (%RH). This requirement ensures that the sample is not only representative, but also conservative from the standpoint of moisture content.
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Gas composition observed by destructive examination of 3013 containers
The Department of Energy’s Integrated Surveillance and Monitoring Program implements requirements to measure gas pressure and gas composition during destructive examination of 3013 containers as required by DOE’s 3013 Standard. Gas pressures and gas compositions measured by the Program during destructive examination of 3013 containers from 2007 to 2017 are reported here. The maximum gas pressure within the population of containers that have undergone destructive examination was 299 kPa (43.4 psia) and this container had 0.52 wt% moisture which is higher than the Standard allows. The majority of containers have essentially no gas pressurization. Hydrogen was quantifiable above the measurement uncertainty in less than half (47 out of 114) of the containers that have undergone destructive examination. The amount of hydrogen that is generated within the sealed 3013 containers is always less than the amount predicted by the 3013 Standard’s pressure equation with the maximum observed hydrogen fraction (observed moles of hydrogen/predicted moles of hydrogen) of 0.18. It is recommended that for the purposes of calculating a maximum hydrogen pressure using the 3013 equation, a correction to the amount of hydrogen produced from decomposition of the water be incorporated. The pressure (or moles) of H 2 should be reduced by multiplying by a hydrogen fraction as described in the text. Helium and nitrogen are the other major constituents. Oxygen which is initially present in nearly all of the containers undergoing destructive examination was consumed to low values in all cases. The highest observed oxygen concentration was 1.7%, and in this case the H 2 concentration was essentially zero. Other minor gases observed in some cases included CO 2 with maximum content of 3.5%, CO with maximum content of 0.8%, N 2 O with maximum content of 1.4%, and CH 4 with maximum content of 0.4%.
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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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Summary Report on the Testing of Flow Formed 3013 Outer Containers Manufactured by Dynamic Flowform Inc. as a Supplement to SRS Requirement G-ESR-G000035 Item 7, Container Configuration
The following tests were conducted on containers and storage packages produced from components manufactured by Dynamic Flowform Inc. (DFF). 1) Burst, and 2) Drop. All of the tested containers exhibited burst pressures that were well in excess of the minimum specified design pressure. The tested storage packages remained leak-tight after being dropped from a height of nine meters. Test results demonstrate that the outer containers made from components manufactured by DFF are in compliance with requirements specified in DOE STD 3013 and G-ESR-G-00035. These containers are acceptable for use by LANL for the ARIES Oxide Production (OP) project. This report supplements the information submitted by LANL relative to item 7 previously approved in 2007 to meet the requirements outlined in G-ESR-G-00035. The outer containers, addressed by this report, were produced by DFF using a different manufacturing process than described in drawings and specifications in appendix A of G-ESR-G-00035. LANL is submitting this supplemental item 7 for approval to use the DFF containers for ARIES OP. The DFF containers will be limited to use with ARIES OP material meeting the innocuous definition as outlined in LA-UR-11-04417.
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PDC IC Weld Failure Evaluation and Resolution
During final preparations for start of the PDCF Inner Can (IC) qualification effort, welding was performed on an automated weld system known as the PICN. During the initial weld, using a pedigree canister and plug, a weld defect was observed. The defect resulted in a hole in the sidewall of the canister, and it was observed that the plug sidewall had not been consumed. This was a new type of failure not seen during development and production of legacy Bagless Transfer Cans (FB-Line/Hanford). Therefore, a team was assembled to determine the root cause and to determine if the process could be improved. After several brain storming sessions (MS and T, R and D Engineering, PDC Project), an evaluation matrix was established to direct this effort. The matrix identified numerous activities that could be taken and then prioritized those activities. This effort was limited by both time and resources (the number of canisters and plugs available for testing was limited). A discovery process was initiated to evaluate the Vendor's IC fabrication process relative to legacy processes. There were no significant findings, however, some information regarding forging/anneal processes could not be obtained. Evaluations were conducted to compare mechanical properties of the PDC canisters relative to the legacy canisters. Some differences were identified, but mechanical properties were determined to be consistent with legacy materials. A number of process changes were also evaluated. A heat treatment procedure was established that could reduce the magnetic characteristics to levels similar to the legacy materials. An in-situ arc annealing process was developed that resulted in improved weld characteristics for test articles. Also several tack welds configurations were addressed, it was found that increasing the number of tack welds (and changing the sequence) resulted in decreased can to plug gaps and a more stable weld for test articles. Incorporating all of the process improvements for the actual can welding process, however, did not result in an improved weld geometry. Several possibilities for the lack of positive response exist, some of which are that (1) an insufficient number of test articles were welded under prototypic conditions, (2) the process was not optimized so that significant improvements were observable over the "noise", and (3) the in-situ arc anneal closed the gap down too much so the can was unable to exhaust pressure ahead of the weld. Several operational and mechanical improvements were identified. The weld clamps were changed to a design consistent with those used in the legacy operations. A helium puff operation was eliminated; it is believed that this operation was the cause of the original weld defect. Also, timing of plug mast movement was found to correspond with weld irregularities. The timing of the movement was changed to occur during weld head travel between tacks. In the end a three sequential tack weld process followed by a pulse weld at the same current and travel speed as was used for the legacy processes was suggested for use during the IC qualification effort. Relative to legacy welds, the PDC IC weld demonstrates greater fluctuation in the region of the weld located between tack welds. However, canister weld response (canister to canister) is consistent and with the aid of the optical mapping system (for targeting the cut position) is considered adequate. DR measurements and METs show the PDC IC welds to have sufficient ligament length to ensure adequate canister pressure/impact capacity and to ensure adequate stub function. The PDC welding process has not been optimized as a result of this effort. Differences remain between the legacy BTC welds and the PDC IC weld, but these differences are not sufficient to prevent resumption of the current PDC IC qualification effort. During the PDC IC qualification effort, a total of 17 cans will be welded and a variety of tests/inspections will be performed. The extensive data collected during that qualification effort should be of a sufficient population to determine if additional weld process optimization is necessary prior to production release.
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A summary of volatile impurity measurements and gas generation studies on MISSTD-1, a high-purity plutonium oxide produced by low-temperature calcination of plutonium oxalate
Plutonium dioxide of high specific surface area was subjected to long-term tests of gas generation in sealed containers. The material preparation and the storage conditions were outside the bounds of acceptable parameters defined by DOE-STD-3013-2012 in that the material was stabilized to a lower temperature than required and had higher moisture content than allowed. The data provide useful information for better defining the bounding conditions for safe storage. Net increases in internal pressure and transient increases in H{sub 2} and O{sub 2} were observed, but were well within the bounds of gas compositions previously shown to not threaten integrity of 3013 containers.
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