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Container Evaluation: Analysis of the Swagelok Knuckle with Viewport as an Approved Hermetically Sealed Inner Container

This report outlines the results from the water ingress test, helium leak test and additional atmosphere testing for the Swagelok knuckle with viewport container further referred to as the SKV. This container is constructed from a standard union vacuum fitting, 1.33” conflat to 0.5” male VCR, a 1.33” conflat fused silica lensed viewport fitting, and a 0.5 inch VCR cap. The primary intended use of this container is to store Pu metal samples in the vault for a time interval exceeding 40 years. The samples need to be contained in an air free environment to ensure that the material does not oxidize over time. The container viewport is a critical design feature that will help the operators visually inspect and evaluate the state of the metal samples prior to opening the container. These containers are advertised as leak tight, but experimental tests were performed to test the water resistant criteria and the gas leaking criteria set forth by the TA-55 Criticality Safety Program. The results of the water ingress test show that the container is water-tight, with no signs of water penetrating the container within the required guidelines outlined in TA55-AP-522. The preliminary He leak test performed demonstrate that the conflat window port and VCR cap are able to maintain a hermetic seal. Additionally, all containers will be He leak tested independently by the manufacturer prior to shipping to LANL. A third voluntary test was added to assess the container’s ability to hold atmosphere, with successful results indicating the container is able to hold inert atmosphere to prevent lanthanum metal oxidation. It is the conclusion of the authorsthat there is enough evidence through the test conducted and outlined within this document that the proposed container meets the definition of a water-tight container, and it is able to provide a hermetic seal.

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Excerpt from Oxygen Monitor Clean Testing Report Performed in 2010

The Rosemount X-STREAM Series X2GP is a paramagnetic oxygen analyzer with a 0-25% oxygen measurement range. It claims a drift less than 2% of span (0.10% volume oxygen) per week, and a response time of less than 5 seconds (for the analyzer to report 90% of a step change). Our test equipment was set-up such that the same gas was running through each oxygen analyzer at the same time. This allowed Calibration Error, Calibration Drift, and Loss of Power Testing to be run on all monitors at the same time, eliminating any variability between the analyzers from tolerances in the gas cylinder, ambient temperature, ambient pressure, test duration, etc. An APTech pressure regulator was placed on the gas cylinder manifold and a 23 psia Paroscientific pressure transducer measured the regulator’s outlet pressure. This did not give the inlet pressure on any one analyzer but outlet pressure from the manifold before the stream was split. The APTech pressure regulator was used to keep operating conditions consistent. A DWYER rotameter was installed on each oxygen monitor’s outlet piping. With the exception of Variation of Flow Rate Testing, the rotameter was left fully open for all testing. The flow rate through each oxygen monitor was controlled by a Swagelok needle valve that was installed on each analyzer’s inlet piping. Additionally, a filter was installed in the each monitor’s inlet piping to keep particles from the measurement cells and a Swagelok ball valve was installed on each monitor’s outlet piping to isolate each monitor between tests. No pumps were installed. Each of the cylinders used was at a pressure greater than ambient room barometric pressure. This pressure differential was used to move gas through the testing equipment. The flow rate through each analyzer was controlled by the Swagelok needle valve installed on each analyzer’s inlet piping. Finally, for all tests, a Paroscientific Digiquartz Barometer was used to measure ambient room barometric pressure and a Fluke Thermo-hygrometer was used to measure ambient room temperature.

47 OTHER INSTRUMENTATION↗

Analysis of pressure test results of tube fittings for the potential application in cryo systems for helium leak rate reduction

Due to the nature of Helium, it is notoriously difficult to maintain a closed system without experiencing helium inventory loss through leakage in large tubing and piping runs. There are two standard fitting options readily available for piping and tubing assemblies, welded fittings or Swagelok ® . Welding is the best option for leak rate reduction, but more costly than Swagelok ® . A new style of fitting has come to the attention of BNL C-AD Cryo group, and a pressure test and leak rate analysis were performed to evaluate the viability of incorporating this new style fitting into current engineering design of warm helium tubing runs for the purpose of leak rate reduction.

43 PARTICLE ACCELERATORS↗

Metal Bellows Valve Reliability Testing - Copper Stem Tip Testing

SRNL was funded in Mid-Year FY20 by NNSA NA-231 to continue evaluation of alternate valves for use in tritium service to support domestic Mo-99 production. The focus of the effort was to identify valve cycle life as a function of actuator size and stem tip material. Using the minimum size actuator to reliability open and close valves can reduce glovebox size and thus support domestic companies to “come to market” faster in supplying Mo-99 to the US market. This report serves as a continuation to the FY19 report and summarizes the task activities completed in FY20 after authorization to start work was obtained on May 5 th , 2020. Copper stem tips were tested on the Swagelok 1C and 5C actuated metal bellows valves. With ambitions to cycle each set 150,000 times, both 1C and 5C valves were met with high failure rates. The smaller 1C actuated valves required additional closing pressure to form a seal with the Cu stem tips installed however, excessive stem tip deformation may be the root cause of the majority of the valves failing before 500 cycles. The larger 5C actuated valves were cycled 150,000 times but still resulted in 80% failure rate, suspected of metal fatigue in the bellows due to high cycling frequencies.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Realizing high-capacity all-solid-state lithium-sulfur batteries using a low-density inorganic solid-state electrolyte

Abstract Lithium-sulfur all-solid-state batteries using inorganic solid-state electrolytes are considered promising electrochemical energy storage technologies. However, developing positive electrodes with high sulfur content, adequate sulfur utilization, and high mass loading is challenging. Here, to address these concerns, we propose using a liquid-phase-synthesized Li 3 PS 4 -2LiBH 4 glass-ceramic solid electrolyte with a low density (1.491 g cm −3 ), small primary particle size (~500 nm) and bulk ionic conductivity of 6.0 mS cm −1 at 25 °C for fabricating lithium-sulfur all-solid-state batteries. When tested in a Swagelok cell configuration with a Li-In negative electrode and a 60 wt% S positive electrode applying an average stack pressure of ~55 MPa, the all-solid-state battery delivered a high discharge capacity of about 1144.6 mAh g −1 at 167.5 mA g −1 and 60 °C. We further demonstrate that the use of the low-density solid electrolyte increases the electrolyte volume ratio in the cathode, reduces inactive bulky sulfur, and improves the content uniformity of the sulfur-based positive electrode, thus providing sufficient ion conduction pathways for battery performance improvement.

25 ENERGY STORAGE↗

Aqueous electrolyte solutions with anion-bridged secondary solvation sheaths for highly efficient zinc metal batteries

Aqueous zinc metal batteries are low-cost electrochemical devices suitable for safe grid energy storage. However, water decomposition and Zn dendrite formation detrimentally affect their coulombic efficiency. Conventional aqueous electrolyte solutions, with a concentration around 1 M, are cost-effective and exhibit high bulk ionic conductivity but cannot form a stable solid electrolyte interphase. Water-in-salt and aqueous-organic hybrid electrolyte solutions can form robust solid electrolyte interphases, but they are not kinetically efficient and cost-effective. Here, to circumvent these issues, we design variously concentrated aqueous electrolyte solutions using several salts with different donor numbers to extend anion coordination into the secondary solvation sheath. We show that salt-derived anions with donor number > 18 enter the Zn2+ first solvation sheath, and ensure a strong binding energy between the Zn2+(H2O)5-anion nanometric clusters and water molecules in the secondary solvation sheath. In particular, 2 M aqueous electrolyte solutions containing fluorinated anions exhibit bulk ionic conductivities of 26-35 mS cm−1 at 25 °C and form a ZnF2-rich solid electrolyte interphase. When tested in Zn||NaV3O8·1.5H2O Swagelok cells, the best-performing electrolyte solution enables an average coulombic efficiency of 99.99% for 1,000 cycles at 1.5 mA cm−2, corresponding to an initial specific energy of 130 Wh kg−1 (based on the combined weight of the positive and negative electrodes).

25 ENERGY STORAGE↗

Hydriding, Oxidation, and Ductility Evaluation of Cr-Coated Zircaloy-4 Tubing

Accident-tolerant fuel concepts have been developed recently in diverse research programs. Recent research has shown clear advantages of Cr-coated Zr cladding over bare cladding tubes regarding oxidation behavior under the design basis loss-of-coolant accident condition. However, limited data are available about the hydriding behavior of the Cr coating. For that purpose, Cr-coated Zricaloy-4 tubes were tested to investigate the effects of hydriding, oxidation, and postquench ductility behavior on coated Zr cladding. A high-power impulse magnetron sputtering (HiPIMS) process was used to produce a high-density coating on the Zircaloy-4 tube surface. Coated and uncoated Zircaloy-4 tube specimens underwent one-sided hydriding in a tube furnace filled with pure hydrogen gas at 425 °C. The tubing specimen ends were sealed with Swagelok plugs before the hydriding runs. For uncoated specimens, H analysis of the hydrided specimens indicated that the H content increased as the test time and initial pressure increased. However, almost no change was observed for the coated specimens that were hydrided under the same test conditions. After one-sided hydriding, the hydrided coated and uncoated specimens were exposed to steam at high temperatures for two-sided oxidation studies to simulate accident conditions. The coated specimens showed a slower oxidation: oxygen pickup was 50% lower than the uncoated specimens tested under the same conditions. Ring compression testing was performed to evaluate the embrittlement behavior of the Cr-coated specimens after hydriding and oxidation. The results indicated that the HiPIMS coating provides excellent protection from hydriding and oxidation at high temperatures.

36 MATERIALS SCIENCE↗

Erosion-Corrosion Detection in Carbon Steel Pipe Loops using SRNLs Thickness and Mass Loss Measurement Coupons - 20464

Structural health of waste transfer infrastructure is of utmost importance to DOE and communities surrounding their active sites. A Fitness-for-Service (FFS) program for the Waste Transfer System has been implemented by the US Department of Energy (DOE) for the purposes of evaluating and quantifying the degradation of critical components. Currently, the method of approach is to section and evaluate pipelines that have been removed at end service. In order to augment data collection methods applied to making lifespan estimates of waste transfer system components, Florida International University (FIU) has been investigating new-technology based strategies for quantifying the rate of degradation. Present research considers the option of a coupon system installed on a section of pipe at points of interest that will provide easy access to high resolution measurements of erosion/corrosion rates during operation. Researchers at Savannah River National Laboratory (SRNL) have developed this novel solution for in situ erosion and corrosion measurements in many applicable locations such as tanks, pipes, ducts, and injection points. The coupons are approximately 12.7 mm (1/2 inch) in diameter and 25.4 mm (1 inch) in length and can be placed in the pipe sections using Swagelok compression fittings. The coupon design allows for monitoring of the total degradation resulting from corrosion and erosion. High-resolution Ultrasonic Thickness (UT) testing allows in-situ monitoring of both degradation mechanisms. When removed from the system mass loss resulting from corrosion and erosion may also be evaluated. Experimental testing at FIU implemented the SRNL coupon system in a 6.10 meter (20 foot) pipe loop system comprised of 50.8 mm (2 inch) and 76.2 mm (3 inch) pipe sections in order to replicate expected use cases at the sites. Operational conditions were emulated by pumping abrasive materials through the pipeline at full capacity and collecting measurements from the SRNL coupons. Initial testing was conducted by circulating water followed by a mixture of sand and water for uniform wear rates. Thickness changes and mass loss were measured, and the surface exposed to the process fluid was observed for visual evidence of characteristic wear patterns resulting from an erosive environment. The test matrix consisted of several hours of operation and using fine, medium and coarse grain sands. Test results were analyzed to check for all three parameters (mass loss/gain, thickness change and surface patters) which could provide estimates of the remaining useful life of the pipe sections. Thus, the research presents the findings of this evaluation of the SRNL coupons as a means for conducting high accuracy, cost effective in-situ analysis of pipeline and waste transfer systems for erosion and corrosion susceptibility. (authors)

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