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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

ASSESMENT OF IMPURITIES IN NP METAL USING DOUBLE-FOCUSING SF-ICP-MS

In the transmutation process, minor actinides such as neptunium, americium and curium obtained from spent nuclear fuel are incorporated into new fuel that can be placed into a fast reactor, where these elements fission into products with shorter half-lives which reduces the health and safety hazards [1]. In order to better understand the all the involved processes, fundamental physical properties of actinides should be investigated, and for that reason, high-purity materials need to be produced. One of the main challenges in characterizing these materials is the lack of pure metal available for study, and lack of analytical methods to determine the purity. Trans-uranic elements are challenging to study because of the need to be handled in specialized facilities, safeguards concerns and they are not easily purchased and/or produced. High-purity Np metal is being produced at the Materials and Fuels Complex (MFC) of Idaho National Laboratory (INL), in a process of direct oxide reduction developed by Squires and Lessing [2], with a target purity of 99.999%. The goal of this research is to develop methods to determine the impurities in the Np metal, with detection limits low enough to achieve this purity level. In this work, we have used several ICP-MS and ICP OES techniques, but the focus was the method development using a recently acquired Double-Focusing Sector Field Inductively Coupled Plasma Mass Spectrometer (SF-ICP-MS). To produce the Np metal, approximately 20 g of the neptunium oxide powder was calcined at 800 oC for 6 h in a magnesium oxide crucible, which is placed inside a stainless steel crucible, that goes into the Hot Uniaxial Press (HUP) furnace insert. After the calcining step, the Np oxide was mixed with approximately 9 g of calcium metal and 100 g of ultra-dry calcium chloride. The HUP furnace was heated in a ramp rate of 50 oC min -1 up to 1000 oC. When the reaction mixture reached 850 oC, a tantalum stirrer was activated at 100 rpm. After the tantalum stirrer was removed and the mixture cooled overnight, the MgO crucible was opened with a hammer and chisel to retrieve the Np metal button at the bottom of the reaction mixture [2]. Prior to the dissolution process, the surface contaminants of the sample were removed. The Np button was washed in 10 mL of ultra-pure water for 1 min, with a faint reaction observed on the surface, indicating the presence of Ca metal. The water-washed sample was placed in a tube with 2 M HCl for only 3 s, as a vigorous reaction in the button surface was observed. The leachates were saved for further analysis. The sample was then rinsed with ultra-pure water and air-dried prior to dissolution. The cleaned sample was placed in a PTFE beaker and 25 mL of 6 M HCl and 150 µL of 24 M HF were added. After 10 minutes of reaction, the beaker was placed on a hot plate for 1 h and 30 min, followed by the addition of 1 mL of 16 M HNO3 and allowed to react for a further 1 h and 20 min. The sample was removed from heat and 10 mL of HNO3 16 M was added to react with the HCl. The beaker was covered and left for overnight reaction, producing a solution with approximately 20 mL of final volume. A Quadrupole Inductively Coupled Plasma Mass Spectrometer (Q-ICP-MS, Perkin Elmer ELAN DRC II Q-ICP-MS) was used to obtain qualitative mass spectra for the dissolution blank, each of the leachates and the dissolved sample. In the water leachate spectrum mainly Ca and Mg were observed, while the acid wash had a similar peak pattern to the one observed for the Np metal sample, indicating that the process not only removed surface contamination, but also reacted with the sample itself. In the Np material spectrum, Ta and actinides were identified as candidates for major contaminants, as the most intense peaks corresponded to the mass-to-charge ratios of these elements. Minor contaminants included Al, Au, Ca, Cr, Fe, I, Na, Nb, Pb, Sn, Ti, Tl, V, Y. The presence of impurities in the material could have originated from several sources, such as the materials used for the casting process, the use of impure NpO2 or contamination of reagents and materials used for the analysis. Some of the isotopes listed as potential contaminants are susceptible to spectral interferences, so Double-Focusing SF-ICP-MS (Nu Instruments Attom ES HR-ICP-MS) was used for the quantitative analysis. For each isotope determined, several items were evaluated: raw signal of a blank solution, sensitivity and determination coefficient of calibration curves, possibility of interferences and comparison of results obtained for at least two resolving powers (RP): 300 and 4000. The evaluation of the signal in a blank solution can indicate if a spectral interference from the plasma gas and/or the solvent was successfully resolved (commonly observed for 52Cr+/40Ar12C+, for example). It is important to highlight that a signal reduction is expected when a higher RP is used, as the ion beam transmission is decreased by the use of na

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Assessment of Impurities in Neptunium Metal Using Double-Focusing SF-ICP-MS

In the transmutation process, minor actinides such as neptunium, americium and curium obtained from spent nuclear fuel are incorporated into new fuel that can be placed into a fast reactor, where these elements fission into products with shorter half-lives which reduces the health and safety hazards. In order to better understand the all the involved processes, fundamental physical properties of actinides should be investigated, and for that reason, high-purity materials need to be produced. One of the main challenges in characterizing these materials is the lack of pure metal available for study, and lack of analytical methods to determine the purity. Trans-uranic elements are challenging to study because of the need to be handled in specialized facilities, safeguards concerns and they are not easily purchased and/or produced. High-purity Np metal is being produced at the Materials and Fuels Complex (MFC) of Idaho National Laboratory (INL), in a process of direct oxide reduction developed by Squires and Lessing, with a target purity of 99.999%. The goal of this research is to develop methods to determine the impurities in the Np metal, with detection limits low enough to achieve this purity level. In this work, we have used several ICP-MS and ICP OES techniques, but the focus was the method development using a recently acquired Double-Focusing Sector Field Inductively Coupled Plasma Mass Spectrometer (SF-ICP-MS). To produce the Np metal, approximately 20 g of the neptunium oxide powder was calcined at 800 oC for 6 h in a magnesium oxide crucible, which is placed inside a stainless steel crucible, that goes into the Hot Uniaxial Press (HUP) furnace insert. After the calcining step, the Np oxide was mixed with approximately 9 g of calcium metal and 100 g of ultra-dry calcium chloride. The HUP furnace was heated in a ramp rate of 50 oC min -1 up to 1000 oC. When the reaction mixture reached 850 oC, a tantalum stirrer was activated at 100 rpm. After the tantalum stirrer was removed and the mixture cooled overnight, the MgO crucible was opened with a hammer and chisel to retrieve the Np metal button at the bottom of the reaction mixture. Prior to the dissolution process, the surface contaminants of the sample were removed. The Np button was washed in 10 mL of ultra-pure water for 1 min, with a faint reaction observed on the surface, indicating the presence of Ca metal. The water-washed sample was placed in a tube with 2 M HCl for only 3 s, as a vigorous reaction in the button surface was observed. The leachates were saved for further analysis. The sample was then rinsed with ultra-pure water and air-dried prior to dissolution. The cleaned sample was placed in a PTFE beaker and 25 mL of 6 M HCl and 150 µL of 24 M HF were added. After 10 minutes of reaction, the beaker was placed on a hot plate for 1 h and 30 min, followed by the addition of 1 mL of 16 M HNO3 and allowed to react for a further 1 h and 20 min. The sample was removed from heat and 10 mL of HNO3 16 M was added to react with the HCl. The beaker was covered and left for overnight reaction, producing a solution with approximately 20 mL of final volume. A Quadrupole Inductively Coupled Plasma Mass Spectrometer (Q-ICP-MS, Perkin Elmer ELAN DRC II Q-ICP-MS) was used to obtain qualitative mass spectra for the dissolution blank, each of the leachates and the dissolved sample. In the water leachate spectrum mainly Ca and Mg were observed, while the acid wash had a similar peak pattern to the one observed for the Np metal sample, indicating that the process not only removed surface contamination, but also reacted with the sample itself. In the Np material spectrum, Ta and actinides were identified as candidates for major contaminants, as the most intense peaks corresponded to the mass-to-charge ratios of these elements. Minor contaminants included Al, Au, Ca, Cr, Fe, I, Na, Nb, Pb, Sn, Ti, Tl, V, Y. The presence of impurities in the material could have originated from several sources, such as the materials used for the casting process, the use of impure NpO2 or contamination of reagents and materials used for the analysis. Some of the isotopes listed as potential contaminants are susceptible to spectral interferences, so Double-Focusing SF-ICP-MS (Nu Instruments Attom ES HR-ICP-MS) was used for the quantitative analysis. For each isotope determined, several items were evaluated: raw signal of a blank solution, sensitivity and determination coefficient of calibration curves, possibility of interferences and comparison of results obtained for at least two resolving powers (RP): 300 and 4000. The evaluation of the signal in a blank solution can indicate if a spectral interference from the plasma gas and/or the solvent was successfully resolved (commonly observed for 52Cr+/40Ar12C+, for example). It is important to highlight that a signal reduction is expected when a higher RP is used, as the ion beam transmission is decreased by the use of narrower slits

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Calibration of the IMB Detector

The IMB detector (named after its founding institutions: University of California, Irvine, the University of Michigan and Brookhaven National Laboratory) collected data on a wide range of phenomena for over eight years. It was the first and the largest of the ring imaging water Cherenkov detectors. The detector consisted of 8000 metric tons of ultra-pure water instrumented with 2048 photomultiplier tubes (PMTs). The PMTs were placed on the roof, floor, and walls of the detector in a lattice of approximately 1 m spacing. It made measurements of contained events that ranged in energy from 15 MeV up to 1.5 GeV. This paper describes the calibration of the IMB detector. This procedure was accurate and stable over a wide range of physical variables. It was used with little change throughout the entire eight-year lifetime of the experiment. The IMB calibration is a model for future large-scale detectors that employ the water Cherenkov technique.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2018

Contribution of electrolyte in nanoscale electrolysis of pure and buffered water by particulate photocatalysis

Photocatalysis using semiconductor powders in suspension performs reduction and oxidation reactions at nanometer-scale distances. Such short distances between the reduction (cathode) and the oxidation (anode) sites enable photocatalytic water splitting to generate H 2 and O 2 from pure water without a supporting electrolyte, which is otherwise impossible in conventional electrode systems due to the high solution resistance. A CrO x /Pt/SrTiO 3 model photocatalyst achieves high efficiency under UV irradiation in ultra-pure water splitting at rates (>1 μmol-H 2 per cm 2 per h) corresponding to electrocatalysis on the order of mA cm -2 . The introduction of an unbuffered supporting electrolyte did not improve the photocatalytic rates, consistent with the negligible ohmic losses (<1 mV) numerically calculated using the Poisson–Nernst–Planck equations. The Nernstian potential loss resulting from pH gradients became apparent at high photocatalytic rates (>100 mV when rate >1 μmol-H 2 per cm 2 per h) even when the distance between redox sites was below 10 nm. Substantial improvements in photocatalytic rates were observed when buffer ions were introduced into near-neutral pH media by not only circumventing pH gradients but introducing kinetically facile H + reduction to H 2 instead of the kinetically sluggish direct reduction of H 2 O to H 2 . In this work, the quantitative descriptions of the electric potential, concentration gradients, and catalytic performance in nanoscale water electrolysis are presented with emphasis on (1) the advantages of performing redox reactions at the nanoscale, (2) the use of electrolyte engineering at near-neutral pH as a universal and effective strategy, and (3) the effectiveness of transferring knowledge from electrocatalysis to photocatalysis, where the potential is quantitatively defined regarding the former and poorly quantified regarding the latter.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Design and commissioning of an e-beam irradiation beamline at the Upgraded Injector Test Facility at Jefferson Lab

We report the Upgraded Injector Test Facility (UITF) at Jefferson Lab is a continuous-wave superconducting linear accelerator capable of providing an electron beam with energy up to 10 MeV. A beamline for electron-beam irradiation has been designed, installed and successfully commissioned at this facility, aimed at the degradation study of 1,4-dioxane and per- and polyfluoroalkyl substances (PFAS) in wastewater treatment. A solenoid with a peak axial magnetic field of up to 0.28 T and a set of raster coils were used to obtain a Gaussian beam profile with a transverse standard deviation of ~ 15.0 mm at the target location. Monte-Carlo simulations using FLUKA were carried out to calculate the total absorbed dose and the dose distribution in the sample volume inside the target cell. The simulations were benchmarked experimentally by dosimetry mapping using optichromic dosimeters. The results of the irradiation experiments showed a ~ 95% reduction of 1,4-dioxane in ultra-pure water for a dose of 1 kGy, demonstrating the potential of electron-beam irradiation towards addressing growing challenges in environmental remediation.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2015

Understanding the SNO+ Detector

SNO+, a large liquid scintillator experiment, is the successor of the Sudbury Neutrino Observatory (SNO) experiment. The scintillator volume will be loaded with large quantities of 130 Te, an isotope that undergoes double beta decay, in order to search for neutrinoless double beta decay. In addition to this search, SNO+ has a broad physics program due to its sensitivity to solar and supernova neutrinos, as well as reactor and geo anti-neutrinos. SNO+ can also place competitive limits on certain modes of invisible nucleon decay during its first phase. The detector is currently undergoing commissioning in preparation for its first phase, in which the detector is filled with ultra pure water. This will be followed by a pure scintillator phase, and then a Tellurium-loaded scintillator phase to search for neutrinoless double beta decay. Here we present the work done to model detector aging, which was first observed during SNO. The aging was found to reduce the optical response of the detector. We also describe early results from electronics calibration of SNO+.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2015

Background reduction in the SNO+ experiment

SNO+ is a large multi-purpose liquid scintillator experiment, which first aim is to detect the neutrinoless double beta decay of {sup 130}Te. It is placed at SNOLAB, at 6000 m.w.e. and it is based on the SNO infrastructure. SNO+ will contain approximately 780 tonnes of liquid scintillator, loaded with {sup 130}Te inside an acrylic vessel (AV) with an external volume of ultra pure water to reduce the external backgrounds. Light produced in the scintillator by the interaction of particles will be detected with about 9,000 photomultiplier’s. For the neutrinoless double beta decay phase, due to its the extremely low rate expected, the control, knowledge and reduction of the background is essential. Moreover, it will also benefit other phases of the experiment focused on the study of solar neutrinos, nucleon decay, geoneutrinos and supernovae. In order to reduce the internal background level, a novel purification technique for tellurium loaded scintillators has been developed by the collaboration that reduces the U/Th concentration and several cosmic-activated isotopes by at least a factor 10{sup 2} -10{sup 3} in a single pass. In addition, different rejection techniques have been developed for the remaining internal backgrounds based on Monte-Carlo simulations. In this work, the scintillator purification technique and the levels obtained with it will be discussed. Furthermore, an overview of the different backgrounds for the double-beta phase will be presented, highlighting some of the techniques developed to reject the remained decays based on their expected timing differences.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2016

Super-Kamiokande [CETUP 2015: Workshop on dark matter, neutrino physics and astrophysics; PPC 2015: 9. international conference on interconnections between particle physics and cosmology]

The Super-Kamiokande experiment performs a large variety of studies, many of them in the neutrino sector. The archetypes are atmospheric neutrino (recently awarded with the Nobel prize for Mr. T. Kajita) and the solar neutrinos analyses. In these proceedings we report our latest results and present updates to indirect dark matter searches, our solar neutrino analysis and discuss the future upgrade of Super-Kamiokande by loading gadolinium into our ultra-pure water.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2024

The design, implementation, and performance of the LZ calibration systems

LUX-ZEPLIN (LZ) is a tonne-scale experiment searching for direct dark matter interactions and other rare events. It is located at the Sanford Underground Research Facility (SURF) in Lead, South Dakota, USA. The core of the LZ detector is a dual-phase xenon time projection chamber (TPC), designed with the primary goal of detecting Weakly Interacting Massive Particles (WIMPs) via their induced low energy nuclear recoils. Surrounding the TPC, two veto detectors immersed in an ultra-pure water tank enable reducing background events to enhance the discovery potential. Intricate calibration systems are purposely designed to precisely understand the responses of these three detector volumes to various types of particle interactions and to demonstrate LZ's ability to discriminate between signals and backgrounds. In this paper, we present a comprehensive discussion of the key features, requirements, and performance of the LZ calibration systems, which play a crucial role in enabling LZ's WIMP-search and its broad science program. The thorough description of these calibration systems, with an emphasis on their novel aspects, is valuable for future calibration efforts in direct dark matter and other rare-event search experiments.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2023

First Experience with Liquid Nitrogen Cleaning

Field emission caused by microscopic particulate contamination is a limiting factor for the performance of superconducting RF (SRF) cavities. In an SRF based accelerator, particulates may be transported over the surface of an operational SRF cavity, becoming field emitters and consequentially degrading the performance of the SRF cavity. The most commonly used method for removing particulates from cavity surfaces is high-pressure ultra-pure water rinsing. We are developing a novel high-pressure liquid nitrogen cleaning technique that may possibly enable superior cleaning power and particulate removal from cavities in a cryomodule without taking apart the cryomodule components. This technique provides cleaning mechanisms beyond what are accessible by its high-pressure water rinsing counterpart and leaves no residues on the cleaned surface.

Ruber, R.J.M.Y.↗
DOE OSTI2013

Performance characteristics of Jefferson Lab's new SRF infrastructure

In the past two years, Jefferson Lab has reconfigured and renovated its SRF support infrastructure as part of the Technology and Engineering Development Facility project, TEDF. The most significant changes are in the cleanroom and chemistry facilities. We report the initial characterization data on the new ultra-pure water systems, cleanroom facilities, describe the reconfiguration of existing facilities and also opportunities for flexible growth presented by the new arrangement.

Reece, Charles E.↗
DOE OSTI2023

Protocol for assembling and operating bipolar membrane water electrolyzers

Renewable energy-driven bipolar membrane water electrolyzers (BPMWEs) are a promising technology for sustainable production of hydrogen from seawater and other impure water sources. Here, we present a protocol for assembling BPMWEs and operating them in a range of water feedstocks, including ultra-pure deionized water and seawater. We describe steps for membrane electrode assembly preparation, electrolyzer assembly, and electrochemical evaluation. For complete details on the use and execution of this protocol, please refer to Marin et al. (2023).

Rios Amador, Isabela↗
DOE OSTI2017

Better Particle Accelerators with SRF Technology

The use of superconducting radio frequency (SRF) technology is a driving force in the development of particle accelerators. Scientists from around the globe are working together to develop the newest materials and techniques to improve the quality and efficiency of the SRF cavities that are essential for this technology.

43 PARTICLE ACCELERATORS↗
DOE OSTI2019

System and method for production of ultra-pure hydrogen from biomass

The disclosure provides a system and method for synthesizing ultra-pure hydrogen from biomass waste. The present invention comprises a gasifier, an oils and tars filter, a steam generator, a water gas shift reactor ("WGS"), a heat-exchange two-phase water separator, a scrubber, a hydrogen separator, and fluid conduits in fluid communication with the various system components, which together convert hydrocarbon-based biomass, e.g., woodchips, into ultra-pure hydrogen gas. Fluid conduits connect the gasifier and the steam generator, separately, to the WGS, the WGS to the two-phase separator, the two-phase separator to the scrubber, and the scrubber to the hydrogen separator, which further comprises an outlet port through which hydrogen gas may flow free of carbon monoxide. The hydrogen may flow to a device that utilizes hydrogen to generate energy, such as a hydrogen fuel cell or to an internal combustion engine.

Tawfik, Hazem↗
DOE OSTI2014

Extreme argon purity in a large, non-evacuated cryostat

Liquid Argon Time Projection Chambers (LArTPCs) show promise as scalable devices for the large detectors needed for long-baseline neutrino oscillation physics. Over the last several years at Fermilab a staged approach to developing the technology for large detectors has been developed. The TPC detectors require ultra-pure liquid argon with respect to electronegative contaminants such as oxygen and water. The tolerable electronegative contamination level may be as pure as 60 parts per trillion of oxygen. Three liquid argon cryostats operated at Fermilab have achieved the extreme purity required by TPCs. These three cryostats used evacuation to remove atmospheric contaminants as the first purification step prior to filling with liquid argon. Future physics experiments may require very large detectors with tens of kilotonnes of liquid argon mass. The capability to evacuate such large cryostats adds significant cost to the cryostat itself in addition to the cost of a large scale vacuum pumping system. This paper describes a 30 ton liquid argon cryostat at Fermilab which uses purging to remove atmospheric contaminants instead of evacuation as the first purification step. This cryostat has achieved electronegative contamination levels better than 60 parts per trillion of oxygen equivalent. The results of this liquid argon purity demonstration will strongly influence the design of future TPC cryostats.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2018

Utilizing of Solar Energy for Extracting Freshwater from Atmospheric Air

It presents a method to extract pure water from atmospheric air, which depends on intensifying the water vapor from the air. The plant was designed to perform the optimum levels to produce high quality water with minimal electricity consumption. The harvesting water was inspected and analyzed based on ISO/IEC 17025 method to check the purity of water. This study also investigates the potential of a solar powered using for atmospheric water generation (AWG) as a new option for fresh water production. A proposed solar AWG unit was assembled, analyzed and modeled using HOMER software. The results demonstrated that the water produced by the water extraction plant is pure, safe, economical, and acceptably tasting. It can be used as drinking water after treated by filter and disinfected by Ultra Violet Light (UV) technique. The feasibility analysis showed that there is a potential to adopt solar powered of AWG as strategic and alternative option for a small area; which is suffering from a shortage of drinking water.

14 SOLAR ENERGY↗
DOE OSTI2012

A shallow underground laboratory for low-background radiation measurements and materials development

Pacific Northwest National Laboratory recently commissioned a new shallow underground laboratory, located at a depth of approximately 30 meters-water-equivalent. This new addition to the small class of radiation measurement laboratories located at modest underground depths houses the latest generation of custom-made, high-efficiency, low-background gamma-ray spectrometers and gas proportional counters. This paper describes the unique capabilities present in the shallow underground laboratory; these include large-scale ultra-pure materials production and a suite of radiation detection systems. Reported data characterize the degree of background reduction achieved through a combination of underground location, graded shielding, and rejection of cosmic-ray events. We conclude by presenting measurement targets and future opportunities.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗