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At least 811 records · Page 45

Challenges in selecting appropriate electrodes for high-temperature molten salt systems

Based on a specific molten salt (e.g., chloride, fluoride, iodide) investigated, different working and reference electrode materials can be selected considering the chemical and thermal stability of the electrochemical cell components. In this talk, the electrode materials and challenges encountered with a spectro-electrochemical setup installed inside a glovebox, and the solutions implemented to address these challenges, specifically for the chloride and iodide molten salts will be presented. For molten chlorides, the fundamental interactions between neodymium chloride (NdCl3) and Nd metal in lithium chloride-potassium chloride eutectic salt were investigated at 773 K. The electrochemical transitions Nd2+,3+/Nd(s) were analyzed using an inert W electrode with cyclic voltammetry and chronoamperometry techniques, coupled with in-situ UV-Vis spectroscopy to elucidate the kinetic pathways of this disproportionation reaction (eq. 1). Nd(s) + NdCl3 = NdCl2 (1) For molten iodides, the challenges related to working electrode selectivity and present spectro-electrochemical results obtained from cyclic voltammetry measurements conducted at 673 K will be discussed.

36 - MATERIALS SCIENCE↗

Mercury speciation comparison. BrooksApplied Laboratories and Eurofins Frontier Global Sciences

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences (FGS), Inc. in Bothell, WA on behalf of the Savannah River Remediation (SRR) Mercury Program Team. These samples were analyzed for seven species including: total mercury, dissolved mercury, inorganic mercury ((Hg(I) and Hg(II)), elemental mercury, methylmercury, ethylmercury, and dimethylmercury, with an eighth species, particulate mercury, calculated from the difference between total and dissolved mercury after subtracting the elemental mercury. The species fraction of total mercury measured has ranged broadly from a low of 32% to a high of 146%, though the vast majority of samples have been <100%. This can be expected since one is summing multiple values that each have at least a ± 20% measurement uncertainty. Two liquid waste tanks particularly important to understanding the distribution of mercury species in the Savannah River Site (SRS) Tank Farm were selected for a round robin analysis by Eurofins FGS and BrooksApplied Laboratories (BAL). The analyses conducted by BAL on the Tank 22 and 38 samples and their agreement with those obtained from Eurofins FGS for total mercury, dissolved mercury, methylmercury, ethylmercury, and dimethylmercury provide a strong degree of confidence in these species measurements

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Concomitant ion effects on isotope ratio measurements with liquid sampling – atmospheric pressure glow discharge ion source Orbitrap mass spectrometry

RATIONALE: The field of highly accurate and precise isotope ratio (IR) analysis has been dominated by inductively coupled plasma and thermal ionization mass spectrometers. While these instruments are considered the gold standard for IR analysis, the International Atomic Energy Agency desires a field deployable instrument capable of accurately and precisely measuring U isotope ratios. METHODS: The proposed system interfaces the liquid sampling – atmospheric pressure glow discharge (LS-APGD) ion source with a high resolution Exactive Orbitrap mass spectrometer. With this experimental setup certified U isotope standards and unknown samples were analyzed. The accuracy and precision of the system were then determined. RESULTS: The LS-APGD /Exactive instrument measures a certified reference material of natural U (235U/238U = 0.007258) as 0.007041 with a relative standard deviation of 0.158% meeting the International Target Values for Uncertainty for the destructive analysis of U. Additionally, when three unknowns measured and compared to the results from an ICP multi collector instrument, there is no statistical difference between the two instruments. CONCLUSIONS: The LS-APGD / Orbitrap system, while still in the preliminary stages of development, offers highly accurate and precise IR analysis that suggest a paradigm shift in the world of IR analysis. Furthermore, the portability of the LS-APGD as an elemental ion source combined with the low overhead and small size of the Orbitrap suggest that the instrumentation is capable of being field deployable. With liquid sampling glow discharge-Orbitrap MS, isotope ratio and precision performance improves with rejection of concomitant ion species.

atmospheric pressure sampling↗

Characterization of Neutron Emission Rates of Commercial 252 Cf Sources

Accurate knowledge of 252 Cf neutron emission rates is critical for modeling and fast-neutron experiments, yet commercial sources are often supplied without traceable calibration or uncertainty estimates. This report describes a method to characterize 252 Cf sources using a pulse-shape-discrimination (PSD) scintillator. The scintillator was efficiency-calibrated against a time-tagged 252 Cf fission chamber manufactured at ORNL over 40 years ago. Isotopic evolution of the calibration source was modeled using Bateman equations to account for changes in the effective average neutrons per fission at the time of measurement. The calibrated scintillator was then used to measure absolute emission rates of several commercial 252 Cf sources, revealing deviations of up to 12% from nominal manufacturer values. This methodology provides a practical approach for establishing uncertainty-quantified 252 Cf neutron emission rates, improving fidelity in simulations and supporting the accurate interpretation of measurements.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗

Modular Autonomous Experimentation for Biological Applications

The Modular Autonomous Research System (MARS) was created to address a key challenge in scientific discovery: experiments are often slow, require significant manual labor, and generate data that is not easily integrated across different tools. This limits how quickly scientists can explore new materials, processes, and chemical reactions. Our motivation was to design a system that makes research faster, more reliable, and adaptable by combining automation with artificial intelligence. By doing so, we aimed to reduce human error, accelerate discovery, and allow researchers to quickly test many possibilities that would otherwise take months or years. Our approach was to build a flexible platform that connects laboratory robots, measurement instruments, and a central data system, all guided by artificial intelligence. MARS integrates liquid handling robots, robotic arms, and plate readers with an intelligent decision-making system that chooses the most informative experiments to run next. This creates a closed loop where experiments are performed automatically, the data is analyzed in real time, and new conditions are immediately tested. Through this work, we demonstrated that MARS can carry out multiple experiments with little or no human intervention, adapt to different scientific problems, and handle uncertain or noisy measurements in a robust way. The results show that modular and intelligent automation can significantly accelerate the pace of discovery, providing a model for future self-driving laboratories. This approach addresses the growing scientific need for adaptable, data-driven research platforms that can keep up with the complexity and scale of modern science.

59 BASIC BIOLOGICAL SCIENCES↗

Astronomy and Space Science from the Moon: Proceedings of Symposium E4 of the COSPAR 29th Plenary Meeting held in Washington, DC, 28 Aug.-5 Sep., 1992

The goal of the conference was to assess the moon as a base for conducting astronomy, solar system observations, and space sciences. The lunar vacuum allows a complete opening of the electromagnetic window and distortion-free measurements at the highest angular resolution, precision, and temporal stability. The moon is perfect for continuous monitoring of the Sun, Solar System targets, and for deep observations of galactic and extragalactic objects. It is an in-situ laboratory for selenophysics, chemistry, and exobiology. The moon contains useful resources and is accessible from Earth for installation, operations maintenance, robotics, and human activities.

Foing, B. H.↗

H2SO4 photolysis: A souce of sulfur dioxide in the upper stratosphere

Numerous absoption lines of stratospheric sulfer dioxide (SO2) were identified in solar occulation spectra recorded by the Atmospheric Trace Molecule Spectroscopy (ATMOS) Fourier transform spectrometer during the Atmospheric Laboratory for Applications and Science (ATLAS)-1 shuttle mission (March 24-April 2, 1992). based on their analysis, a volume mixing ratio profile of SO2 increasing from (13 +/- 4) p.p.t.v. (parts per 10(exp -12) by volume) at 16 mbar (approximately 28 km) to 455 +/- 90 p.p.t.v. at 0.63 mbar (approximately 52 km) was measured with no significant profile differences between 20 deg N and 60 deg S latitude. The increase in the SO2 mixing ratios with altitude indicates the presence of a source of SO2 in the upper stratosphere. Profiles retrieved from ATMOS spectra recorded during shuttle flights in April-May 1985 and April 1993 show similar vertical distributions but lower concentrations. Two-dimensional model calculations with SO2 assumed as the end product of H2SO4 photolysis produce SO2 profiles consistent with the ATMOS measuremnts to within about a factor 2.

Rinsland, C. P.↗

Mass Spectrometers in Deep Space Missions

Mass spectrometers have been included in the payloads of several deep space missions over the past three decades. Our laboratory has designed and developed mass spectrometers for the Galileo Probe into the atmosphere of Jupiter, the Pioneer Venus Orbiter, the Cassini Orbiter Mission to Saturn, the Cassini/Huygens Probe Mission to Saturn's moon Titan, the Nozomi Mission to Mars, and most recently the CONTOUR comet nucleus flyby mission. Each mission has required attention to miniaturization, autonomous sampling, and consideration of the special hazards and measurement requirements of the target environment. Development ongoing in our laboratory includes further miniaturization, improved performance in the areas of sensitivity and precision for the important isotope measurements, and adaptation for the unusual environments to be encountered in locations such as the surface or subsurface of Europa or Mars. Various aspects of both the technical implementation of these delivered and planned experiments and the science drivers will be described.

Mahaffy, Paul↗

Sampling for Air Chemical Emissions from the Life Sciences Laboratory II

Sampling for air chemical emissions from the Life Science Laboratory II (LSL-II) ventilation stack was performed in an effort to determine potential exposure of maintenance staff to laboratory exhaust on the building roof. The concern about worker exposure was raised in December 2015 and several activities were performed to assist in estimating exposure concentrations. Data quality objectives were developed to determine the need for and scope and parameters of a sampling campaign to measure chemical emissions from research and development activities to the outside air. The activities provided data on temporal variation of air chemical concentrations and a basis for evaluating calculated emissions. Sampling for air chemical emissions was performed in the LSL-II ventilation stack over the 6-week period from July 26 to September 1, 2016. A total of 12 sampling events were carried out using 16 sample media. Resulting analysis provided concentration data on 49 analytes. All results were below occupational exposure limits and most results were below detection limits. When compared to calculated emissions, only 5 of the 49 chemicals had measured concentrations greater than predicted. This sampling effort will inform other study components to develop a more complete picture of a worker’s potential exposure from LSL-II rooftop activities. Mixing studies were conducted to inform spatial variation in concentrations at other rooftop locations and can be used in conjunction with these results to provide temporal variations in concentrations for estimating the potential exposure to workers working in and around the LSL-II stack.

54 ENVIRONMENTAL SCIENCES↗

Particle tracking during Ostwald ripening using time-resolved laboratory X-ray microtomography

Laboratory X-ray microtomography is investigated as a method for obtaining time-resolved images of microstructural coarsening of the semisolid state of Al–5 wt.% Cu samples during Ostwald ripening. Owing to the 3D imaging capability of tomography, this technique uniquely provides access to the growth rates of individual particles, thereby not only allowing a statistical characterization of coarsening—as has long been possible by conventional metallography—but also enabling quantification of the influence of local environment on particle boundary migration. The latter information is crucial to understanding growth kinetics during Ostwald ripening at high volume fractions of the coarsening phase. Automated image processing and segmentation routines were developed to close gaps in the network of particle boundaries and to track individual particles from one annealing step to the next. The particle tracking success rate places an upper bound of only a few percent on the likelihood of segmentation errors for any given particle. The accuracy of particle size trajectories extracted from the time-resolved tomographic reconstructions is correspondingly high. Statistically averaged coarsening data and individual particle growth rates are in excellent agreement with the results of prior experimental studies and with computer simulations of Ostwald ripening. - Highlights: • Ostwald ripening in Al–5 wt.% Cu measured by laboratory X-ray microtomography • Time-resolved measurement of individual particle growth • Automated segmentation routines developed to close gaps in particle boundary network • Particle growth/shrinkage rates deviate from LSW model prediction.

36 MATERIALS SCIENCE↗

Stitching methods at the European Synchrotron Radiation Facility (ESRF)

X-ray mirror quality has continuously improved over the past 20 years and manufacturers are now able to provide long mirrors with slope errors below 0.2 μrad. Nevertheless, these mirrors are mounted on holders or even mechanical benders to adjust their curvature and their intrinsic quality must be preserved from any parasitic deformation such as twist. The most direct method of detecting these deformations is to measure the 3D topography of the optical surface. At the ESRF metrology laboratory, three different stitching systems are under development based on Fizeau sub-aperture measurements. The first one consists of measuring long flat mirrors, the second based on the relative angle determinable stitching interferometry (RADSI) method developed at SPring-8 is aimed primarily at the measurement of short mirrors with strong curvature down to a few meters, and the last, also based on the RADSI method, is dedicated to characterize longer mirrors with intermediate curvature. For each method we will describe the measurement setup and discuss first results obtained. Micro-stitching interferometry is also currently used at the ESRF metrology laboratory. The technique is suitable for measuring deeply curved aspherical profiles and will be illustrated with results from a Kirkpatrick-Baez mirror system for nano-focusing.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Livermore Site Spill Prevention, Control, and Countermeasures Plan, May 2017

This Spill Prevention, Control, and Countermeasure (SPCC) Plan describes the measures that are taken at Lawrence Livermore National Laboratory’s (LLNL) Livermore Site in Livermore, California, to prevent, control, and handle potential spills from aboveground containers that can contain 55 gallons or more of oil.

54 ENVIRONMENTAL SCIENCES↗

Materials Dynamics

The Materials Dynamics area of leadership focuses on understanding structure-properties-performance relationships for the extreme conditions of dynamic loading. This research encompasses controlled synthesis of materials to meet dynamic performance requirements and requires computational coupling across length and time scales for three-dimensional microstructure modeling. For this leadership area, we define dynamic loading as strain rates greater than 103/s. A key grand challenge of this area is to predict and measure the evolution of microstructural phases, defect structures, and electronic structure under dynamic conditions while also dynamically measuring local temperature to understand transition states. Solving this challenge will require agile, multidimensional data analysis and interpretation capability.

36 MATERIALS SCIENCE↗

Acoustic sensors devoted to the detection of leaking irradiated fuel rod in spent fuel pool

The acoustic sensor has been specially designed in order to provide a non-destructive technique to easily carry out the measurement of the internal gas pressure and gas composition of a LWR nuclear fuel rod. This sensor has been achieved in 2007 and is now covered by an international patent. In 2015, we presented a generation of acoustic sensors devoted to the characterization of fission gas. The gas composition can be defined with an uncertainty of about 1% and the pressure with an uncertainty of about 10 % (for around 50 bars and a gas mixture containing 20% Xe/Kr). This measurement is possible in hot laboratory facility using viscous liquid to couple the sensor with the rod. We develop a new acoustic sensor for an application in a spent fuel pool without viscous liquid to couple the sensor with the rod. This application consists in determining the default rod in a fuel assembly which has been declared 'no leak-proof' during the fuel discharging of the reactor. We develop a new method based on the detection of gas pressure drop into the fuel rod. This new method could replace the current one which is based on the detection of water into the fuel rod. The new generation of transducer and the associated methodology are now operational in laboratory for nondestructive measurement under water and enable to detect the gas pressure drop into the fuel rod. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A GEO Hyperspectral Mission For Continental-Scale Carbon Cycle Observations

For both terrestrial and ocean carbon cycle science objectives, a hyperspectral geostationary sensor should enable the development of new remote sensing measurements for important but as yet unobservable variables, and with the overall goal of linking both terrestrial and ocean carbon cycle processes to climate variability. For terrestrial research, accurate estimates of carbon, water and energy (CWE) exchange between the terrestrial biosphere and atmosphere are needed to identify the geographical locations of carbon sources/sinks and to improve regional climate models and global climate change assessments. It is an enormous challenge to estimate CWE exchange from the infrequent temporal coverage provided by most polar-orbiting satellites, and without benefit of spectral indices that capture vegetation responses to stress conditions that down-regulate photosynthesis. Physiological status can be better assessed with spectral indices based on continuous, narrow (5 nm) bands, as can seasonal and annual terrestrial productivity. For coastal and ocean constituents, narrow-band observations in the ultraviolet and visible are essential to investigate the variability, dynamics and biogeochemical cycles of the world s coastal and open ocean regions, which will in turn help in measuring ocean productivity and predicting the variability of Ocean carbon uptake and its role in climate change scenarios. The GSFC Carbon Team has been pursuing a geostationary hyperspectral instrument, which would revolutionize our knowledge of biological processes on land, in the ocean, and along the coast by providing multiple, diurnal coverage. Preliminary studies in Goddard's Instrument Synthesis and Analysis Laboratory (ISAL) indicate that we can meet many of our science requirements: full spectral coverage (360-1000 nm); narrow bandwidths (5-10 nm); adequate ground resolution (100-200 m); and continental-scale coverage 4-6 times per day; all the while achieving a signal to noise ratio of between 500 and 1000 to 1. However, an innovative and bold focal plane design and a large mirror (1.8 meter diameter) would be required. The development of our science requirements and the results of the initial design study will be presented as well as our most recent technological developments.

Gervin, Janette C.↗

Microgravity Vibration Output Testing of Space Station Rotary Joints

The mission of the International Space Station is to provide a working laboratory in orbit for research in engineering, life sciences, and microgravity. Ensuring that the mechanical equipment on Space Station does not unduly disturb the microgravity environment is of paramount importance in meeting the Station's mission. The large inertia being moved by the Space Station's solar array and thermal radiator rotary joints make them one of the largest potential disturbance sources. The present paper describes the mechanical and control system design of these joints, their disturbance producing characteristics, and analytical predictions of some key performance indicators. The component and system functional tests performed to measure the actual vibration output of the joints are detailed and the test results discussed. Results of the rotary joint test program presented here show that the joints do meet the Space Station microgravity requirements, ensuring that this unique laboratory for microgravity research will be unaffected by the operation of the largest moving machinery on board.

Boucher, Robert L.↗

Microwave Resonator Measurements of Atmospheric Absorption Coefficients: A Preliminary Design Study

A preliminary design study examined the feasibility of using microwave resonator measurements to improve the accuracy of atmospheric absorption coefficients and refractivity between 18 and 35 GHz. Increased accuracies would improve the capability of water vapor radiometers to correct for radio signal delays caused by Earth's atmosphere. Calibration of delays incurred by radio signals traversing the atmosphere has applications to both deep space tracking and planetary radio science experiments. Currently, the Cassini gravity wave search requires 0.8-1.0% absorption coefficient accuracy. This study examined current atmospheric absorption models and estimated that current model accuracy ranges from 5% to 7%. The refractivity of water vapor is known to 1% accuracy, while the refractivity of many dry gases (oxygen, nitrogen, etc.) are known to better than 0.1%. Improvements to the current generation of models will require that both the functional form and absolute absorption of the water vapor spectrum be calibrated and validated. Several laboratory techniques for measuring atmospheric absorption and refractivity were investigated, including absorption cells, single and multimode rectangular cavity resonators, and Fabry-Perot resonators. Semi-confocal Fabry-Perot resonators were shown to provide the most cost-effective and accurate method of measuring atmospheric gas refractivity. The need for accurate environmental measurement and control was also addressed. A preliminary design for the environmental control and measurement system was developed to aid in identifying significant design issues. The analysis indicated that overall measurement accuracy will be limited by measurement errors and imprecise control of the gas sample's thermodynamic state, thermal expansion and vibration- induced deformation of the resonator structure, and electronic measurement error. The central problem is to identify systematic errors because random errors can be reduced by averaging. Calibrating the resonator measurements by checking the refractivity of dry gases which are known to better than 0.1% provides a method of controlling the systematic errors to 0.1%. The primary source of error in absorptivity and refractivity measurements is thus the ability to measure the concentration of water vapor in the resonator path. Over the whole thermodynamic range of interest the accuracy of water vapor measurement is 1.5%. However, over the range responsible for most of the radio delay (i.e. conditions in the bottom two kilometers of the atmosphere) the accuracy of water vapor measurements ranges from 0.5% to 1.0%. Therefore the precision of the resonator measurements could be held to 0.3% and the overall absolute accuracy of resonator-based absorption and refractivity measurements will range from 0.6% to 1.

Walter, Steven J.↗

Solid State Streak Camera Prototype Electronic Performance Testing and Characterization

Streak Cameras are an essential diagnostic tool used in shock physics and high energy density physics experiments. Such experiments require well calibrated temporally resolved diagnostics for studying events that occur in the nanosecond to microsecond time scales. Although streak cameras are among the most common detectors used within the high energy density physics community, they require frequent calibration and typically lack reproducibility in the fine detail. A solid state device with similar temporal performance characteristics could provide several advantages to current streak camera systems by utilizing discrete spatial resolution set by the sensor diodes. National Security Technologies (NSTec) has built a multi-channel solid state streak camera (SSSC) prototype, in collaboration with Sandia National Laboratories, as part of an ongoing project to develop the technology to a level competitive with analog streak cameras. The device concept and results from electronic testing of our first prototypes will be discussed in this manuscript. These measurements will be used as a base for future SSSC development projects.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗