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Graphic Three-Axes Presentation of Residual Gas Analyser Data

Residual gas analyzers (RGA) are commonly used to measure the composition of residual gases in thermal-vacuum test chambers. Measurements from RGAs are often used to identify and quantify outgassing contaminants from a test article during thermal-vacuum testing. RGA data is typically displayed as snapshots in time, showing instantaneous concentrations of ions from ionized residual gas molecules at different atomic masses. A method was devised by the authors to present RGA data in a three-axis format, plotting atomic mass unit (AMU), ion concentration as a function of AMU, and time, to provide a clear graphic visualization ot trends in gas concentration changes and to initiate a valuable analytical tool to interpret test article outgassing rates during thermal-vacuum testing.

data analysis↗

Outgassing of Flown and Unflown MIR Solar Cells

A solar panel array with more than ten years space exposure was removed from the Mir core module in November 1997, and an eight panel section was returned to Earth in January 1998. Several solar cells were removed from panel eight of the returned array and placed in a high vacuum system with a residual gas analyzer (200 amu mass spectrometer) and a cold finger. Similar unflown solar cells of the same vintage were later obtained from Energia. Several of the unflown cells were also placed in the vacuum system and outgassed residues were collected on the LN2 cold finger. Almost 3 mg of outgassed residue was collected -from a string of three unflown solar cells over a period of 94 hours under vacuum. The collected residue was weighed with a microbalance, and then the residue was analyzed by FTIR spectroscopy, and by gas chromatograph-mass spectroscopy. About 25 outgassed constituents were separated by the gas chromatograph, and a high-resolution mass spectrum was obtained of each constituent. Molecular identifications have been made for the constituents. The constituents are primarily cyclic siloxanes, and several of the constituents are isomers of the same molecule. Most of the outgassed constituents have a molecular mass of about 500 amu. Almost one mg of residue was extracted from one sq cm of coverglass/adhesive from a flown solar cell by soaking in isopropyl alcohol for 30 minutes. The gas chromatograph separated about 20 constituents. The constituents are mostly cyclic siloxanes with linear branches, hydrocarbons, and phthalates. The typical molecular mass is about 600 amu. These identifications of specific outgassing molecules have resulted in a more complete understanding of the SiO(x) contamination on the Mir solar cell coverglasses, and on the MEEP experiment trays and optical specimens during the Shuttle-Mir Phase One flight experiment program. Adjusted outgassing rates based on the data reported here, and/or measured outgassing rates and specific molecular identifications of ISS hardware samples are needed to input into model predictions of induced environment effects of the ISS.

Harvey, Gale A.↗

Developing Mass Spectrometry for Water Quantitation and Volatiles Analysis from In-Situ Regolith

With a revived focus to create a sustainable hu-man presence on the moon, and in preparation for future Mars exploration, it is imperative that all resources are utilized to their fullest potential [1]. In-Situ Resource Utilization (ISRU) will be critical for future mission success as it would enable in-dependent operation of missions while reducing the dependence on the complex supply chain created between the Earth, the moon and Mars. One of the most critical resources that has been identified for ISRU on the lunar surface is water [2]. Water is a versatile resource that can be used in various space operations, such as ra-diation shielding and conversion to oxygen (O2) for propellant [3,4]. One of the most water rich resources is thought to be within the regolith lo-cated in the permanently shadowed regions (PSR) of the Moon; several upcoming missions, such as PRIME-1 and VIPER, are already sched-uled to confirm this hypothesis [5,6]. However, there are currently no missions planned to quanti-fy the abudance of water at these regions. The quantity of water contained in the ice will inform and help the development of future ISRU plants and operation. Water and other volatile gases can be detect-ed upon controlled heating of icy lunar regolith for an accurate quantification of water. This method is similar to thermogravimetric analysis, which was used to analyze Apollo lunar regolith sam-ples. However, losses via sublimation/evaporation or contamination may have occurred with the samples due to the transit and exposure to the terrestrial environment. Furthermore, water would not be expected for these samples since they were not collected from a PSR. Thus, for more accurate results, icy lunar regolith should be ana-lyzed in situ to provide the most representative composition of both water and other volatile gas-es. The Light Water Analysis and Volatile Extract (LightWAVE) project aims to address this knowledge gap. A system has been developed to collect, heat and analyze evolved gases from lu-nar regolith on the lunar surface. The gases will be analyzed by a modified commercial off the shelf (COTS) residual gas analyzer (RGA) quad-rupole mass spectrometer. Evolved gases from heated regolith samples can be identified by the observed mass-to-charge (m/z) ratios, and the peak intensities correlate to the abundances of the observed gases for quantitation. Therefore, our group is developing a calibration methodology utilizing a COTS RGA to quantitate water from in-situ regolith samples on the lunar surface. The partial pressure of water and ideal gas law will be used to quantify the total water evolved from a regolith sample. Here we present our methodol-ogy for the design and calibration for water quan-titation using a COTS RGA.

Nilab Azim↗

Feasibility of fusion plasma burn control via real-time, sub-divertor neutral gas isotopic and compositional analysis

The ability to provide fusion burn control without requiring physical access through the first wall and fuel breeding blankets, would be vital for any future, magnetically confined fusion power reactor. A multi-sensor, fusion fuel cycle exhaust, neutral gas analysis system on JET, capable of delivering real time data, and accessing only the sub-divertor region, provides an excellent example of such capability. Optimized for and operated during the deuterium–tritium experimental campaigns 2 and 3 (DTE2, DTE3), it is proving valuable for planning to explore fusion reactor burn control in ITER with a comparable diagnostic system called the Diagnostic Residual Gas Analyzer (DRGA). This paper aims to show feasibility of developing model-based controllers for ITER and next generation, reactor-relevant devices, by building both on the empirical experience in JET-DTE2, and on the already emerging experience on developing such models specifically for ITER. The paper begins with a specific use-case from JET-DTE2, pertaining to the observed sensitivity of the fusion neutron yield on the concentration of isotopic helium-3 ( 3 He), with data from one of the high-performance DT shots exhibited with emphasis on the 3 He measurement via the sub-divertor. Then, a first model is developed and then explored with simulations that aim to discover how well the controllers in the model react to either insufficient levels of 3 He or excessive levels of 3 He. The simulations then explore potential impact from a delay in the measurement (or the response) that would be comparable to the ∼1 s, conductance limited response for the ITER DRGA system, currently in its final design. The simulations show that control is feasible, and that its effectiveness is not significantly impacted by such delay.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Polycrystalline silicon on tungsten substrates

Thin films of electron-beam-vaporized silicon were deposited on fine-grained tungsten substrates under a pressure of about 1 x 10 to the -10th torr. Mass spectra from a quadrupole residual-gas analyzer were used to determine the partial pressure of 13 residual gases during each processing step. During separate silicon depositions, the atomically clean substrates were maintained at various temperatures between 400 and 780 C, and deposition rates were between 20 and 630 A min. Surface contamination and interdiffusion were monitored by in situ Auger electron spectrometry before and after cleaning, deposition, and annealing. Auger depth profiling, X-ray analysis, and SEM in the topographic and channeling modes were utilized to characterize the samples with respect to silicon-metal interface, interdiffusion, silicide formation, and grain size of silicon. The onset of silicide formation was found to occur at approximately 625 C. Above this temperature tungsten silicides were formed at a rate faster than the silicon deposition. Fine-grain silicon films were obtained at lower temperatures.

Bevolo, A. J.↗

Efficient solar cells by space processing

Thin films of electron beam evaporated silicon were deposited on molybdenum, tantalum, tungsten and molybdenum disilicide under ultrahigh vacuum conditions. Mass spectra from a quadrapole residual gas analyzer were used to determine the partial pressure of 13 residual gases during each processing step. Surface contamination and interdiffusion were monitored by in situ Auger electron spectrometry. The presence of phosphorus in the silicon was responsible for attaining elevated temperatures with silicide formations. Heteroepitaxial silicon growth was sensitive to the presence of oxygen during deposition, the rate and length of deposition as well as the substrate orientation.

Schmidt, F. A.↗

Discourse for slide presentation: An overview of chemical detection systems

A brief overview of some of the analytical techniques currently used in monitoring and analyzing permanent gases and selected volatile organic compound in air are presented. Some of the analytical considerations in developing a specific method are discussed. Four broad groups of hardware are discussed: compound class specific personal monitors, gas chromatographic systems, infrared spectroscopic systems, and mass spectrometric residual gas analyzer systems. Three types of detectors are also discussed: catalytic sensor based systems, photoionization detectors, and wet or dry chemical reagent systems. Under gas chromatograph based systems five detector systems used in combination with a GC are covered: thermal conductivity detectors, photoionization detectors, Fourier transform infrared spectrophotometric systems, quadrapole mass spectrometric systems, and a relatively recent development, a surface acoustic wave vapor detector.

Peters, Randy Alan↗

Solid Hydrogen Particles and Flow Rates Analyzed for Atomic Fuels

The experiments were conducted at Glenn's Small Multipurpose Research Facility (SMIRF, ref. 5). The experimental setup was placed in the facility's vacuum tank to prevent heat leaks and subsequent boiloff of the liquid helium. Supporting systems maintained the temperature and pressure of the liquid helium bath where the solid particles were created. Solid hydrogen particle formation was tested from February 23 to April 2, 2001. Millimeter-sized solid-hydrogen particles were formed in a Dewar of liquid helium as a prelude to creating atomic fuels and propellants for aerospace vehicles. Atomic fuels or propellants are created when atomic boron, carbon, or hydrogen is stored in solid hydrogen particles. The current testing characterized the solid hydrogen particles without the atomic species, as a first step to creating a feed system for the atomic fuels and propellants. This testing did not create atomic species, but only sought to understand the solid hydrogen particle formation and behavior in the liquid helium. In these tests, video images of the solid particle formation were recorded, and the total mass flow rate of the hydrogen was measured. The mass of hydrogen that went into the gaseous phase was also recorded using a commercially available residual gas analyzer. The temperatures, pressures, and flow rates of the liquids and gases in the test apparatus were recorded as well. Testing conducted in 1999 recorded particles as small as 2 to 5 mm in diameter. The current testing extended the testing conditions to a very cold Dewar ullage gas of about 20 to 90 K above the 4 K liquid helium. With the very cold Dewar gas, the hydrogen freezing process took on new dimensions, in some cases creating particles so small that they seemed to be microscopic, appearing as infinitesimally small scintillations on the videotaped images.

Palaszewski, Bryan A.↗

In situ effective pumping speed measurements as a tool for non-evaporable getter activation and saturation monitoring

We have developed method of in situ effective pumping speed measurements based on injecting finite gas pulse into a vacuum volume and subsequent recording of pressure response using a Residual Gas Analyzer (RGA). The pressure burst caused by injected gas pulse falls exponentially in time and the exponential coefficient of such pressure decay is proportional to total effective pumping speed of all vacuum pumps acting on vacuum chamber volume. The effective pumping speed can be extracted from the dependence of injected gas species pressure vs time recorded by an RGA. Non-Evaporable Getters (NEGs) are widely used in multiple ultra and extremely high vacuum devices and applications during the last several decades. Areas of NEG applications were recently expanded into vacuum devices with relatively high-pressure levels (up to 10 -7 Torr) by the invention of high capacity ZAO NEG which can be operated at elevated temperatures. The intrinsic property of all NEG-based vacuum pumps is the reduction of their pumping speed, called “NEG saturation”, after an extended period of operation. Typical time interval for such process can span from about a month and up to a few years depending on NEG type, vacuum level of NEG pump operation, and residual gas content. After that, the NEG pump will require a re-activation cycle to restore its pumping speed close to the initial value. For many applications it is difficult to realize what is the current pumping speed of NEG pump is and when the pump should be re-activated. A method for in situ effective pumping speed measurements developed in this study can be used as a tool for NEG-based pump activation and saturation monitoring. Application of such an approach to monitor pumping status of NEG pumps was utilized and will be continually used at Extended EBIS which was recently developed and commissioned for Relativistic Heavy Ion Collider (RHIC) and future Electron Ion Collider (EIC). The results obtained during commissioning are presented and discussed.

43 PARTICLE ACCELERATORS↗

Hydrogen Analysis by Gas Chromatography–Mass Spectrometry

The detection of hydrogen in complex gas mixtures is essential for many applications. Conventional approaches such as gas chromatography (GC) with thermal conductivity detection (TCD) and residual gas analyzers (RGAs) face significant limitations: TCD exhibits poor response when helium is used as a carrier gas, whereas RGAs lack chromatographic separation, preventing reliable quantification of hydrogen because of interference from other species. Traditional GC methods rely on dual-column configurations with packed or molecular-sieve porous layer open tubular (PLOT) columns to separate hydrogen from O2, N2, CO, CO2, CH4, and other hydrocarbons, increasing system complexity and limiting compatibility with mass spectrometry (MS) detection. In this work, we developed and validated a robust GC–MS method capable of directly detecting and quantifying hydrogen using electron ionization (EI) without dopants, reagent gases, or ion–molecule reaction schemes. By integrating a modified EI source and a cryogenically cooled single capillary column configuration, we achieved baseline separation of hydrogen from all major permanent gases and hydrocarbons in a refinery gas mixture using helium as the carrier gas. The method demonstrated excellent linearity, high sensitivity, and exceptional reproducibility. Adjustable sample-loop volumes and split ratios enabled optimization of peak shape and signal-to-noise performance for trace-level and percent-level hydrogen concentrations. Beyond hydrogen quantitation, the method provides simultaneous compositional profiling of other gases in a mixture in a single run, making it valuable for a wide range of tasks.

Lobodin, Vlad [ORNL]↗

Diagnostics: Chapter 8 of the special issue: on the path to tokamak burning plasma operation

This chapter presents the activity conducted by the ITPA topical group (TG) on Diagnostics over about the last 15 years. Following a general introduction of the ITER Diagnostics led by their measurement roles, the document is organized in several subchapters detailing the design support, research and development activity conducted by each of the specialist working groups (WGs) of the TG. Please note that the magnetic diagnostics were supported at the TG without a specific WG. Their status is included in the general introduction. In the following some highlights of the subchapter’s contents are provided. Recent advances in ITER first wall (FW) diagnostics for the measurements of plasma-metallic wall interaction in support of the ITER research plan are reported. An InfraRed imaging Video Bolometer for ITER has been developed and tested on several tokamaks to measure the radiated power loss. A laser-induced breakdown spectroscopy (LIBS) technique which utilizes a pulsed laser beam to ablate locally by forming a crater, will measure local tritium inventory in the FW material. Real-time Residual Gas Analyzers will measure the neutral gas composition in a divertor port and an equatorial port during plasma operation. Due to the full metallic FW environment, the plasma-wall interaction in ITER will face several challenges such as the compromised radiated power and divertor heat flux measurements by reflection. Ray tracing and analysis codes have been developed to eliminate and correct the effects of reflection in the measurements. The characteristics of the reflecting surfaces depending on the roughness and angle of the incidence have been measured by dedicated experiments, and the results were applied to the reflection elimination. For the measurement of the metallic impurity radiation induced by eroded metallic atoms, a vacuum ultraviolet spectrometer has been developed and tested. An extensive thermonuclear diagnostic suite will be required to support the operation of ITER and the planned experimental program for future burning plasma experiments. Due to the harsh environmental conditions, the implementation of diagnostic systems in ITER is a major challenge. These conditions include high levels of neutron and gamma fluxes, neutron heating, particle bombardment. Therefore, the selection and design of diagnostic systems must take into account a number of phenomena previously unseen in diagnostic design. For this reason, the measurement of neutrons and confined or lost fast ions, with particular emphasis on alpha particles, is critical to ITER. The diagnostics associated with these measurements will be important for future plasma-burning experiments at ITER. The high neutron emission and very large plasma size in ITER make neutron diagnostics the main diagnostic method used to measure plasma parameters such as fusion power, fusion power density, ion temperature, energy of fast ions and their spatial distributions in the plasma core. Active spectroscopy techniques are methods where a neutral particle beam is injected into the plasma and information on plasma parameters is extracted from the measurement of line emission resulting from the beam-plasma interaction, either by plasma ions or by beam atoms. Spatial localization is achieved by crossing the beamline and multiple observation lines. The ITER plasma will be a high temperature, moderately dense, fully ionized collisional plasma. The plasma facing surfaces are principally metallic being fashioned from beryllium or tungsten but many other elements, arising from either structural or from operational needs, may enter this plasma. The energy range of the emitted photons range from meV (infra-red) to multi keV (x-rays) and originate from all areas of the plasma volume. The primary role of passive emission diagnostics is to identify what is in the plasma from spectral signatures. Extracting quantitative information from these measurements such as impurity content, ion temperature, rotation, degree of detachment and radiated power depends on calibrated instruments, a physics model of the atomic and molecular processes and plasma transport and an analysis workflow that takes into account environmental effects such as reflections. The particular needs for ITER have prompted a multi-machine, many-year effort to address all these aspects and this chapter reviews the work on diagnostic design, experiments and new analysis techniques. An overview of the laser diagnostics to be implemented on ITER is also provided in this paper. This includes descriptions of the Thomson scattering in the core, edge and divertor regions, polarimetry and interferometry diagnostics used for measuring plasma density and also measurements of helium density in the divertor using Laser Induced Flourescence. Techniques which can allow improvements on current measurements are also addressed in particular expanding poloidal polarimetry measurements to measure field fluctuations and proposed use of dispersion interferometery which has a number of advantages over existing methods. This paper identifies particular areas where further research and testing on existing tokamaks is useful even at this advanced stage to inform the design of diagnostics for ITER. Outstanding areas of concern for the implementation of laser diagnostics, in particular with a view to reliable operation are identified. An overview of the latest developments of microwave diagnostic systems and techniques is given. The primary focus is the contributions for ITER—the next step burning plasma experiment—which is supplemented by describing recent progress of techniques applicable for fusion experiments beyond ITER. The contributions are intentionally kept concise, and are being supplemented by a rich list of references for further studies. Radiation induced effects are receiving continuous and well-deserved attention of the ITER diagnostic community and they are in many cases one of the primary design drivers of the ITER diagnostic systems. The paper summarizes recent progress in this area focusing primarily on the ITER diagnostics but in some cases provides also outlook for the possible solutions for even more demanding radiation environment of fusion reactors beyond ITER. Despite advancements in the area of modeling and simulation of various radiation induced effects, experimental testing in a nuclear environment as close as possible to the target one is still seen as unavoidable for proper qualification of particular diagnostic functional elements. Recent advancement within three diagnostic areas: optical diagnostics, magnetics and bolometers is covered. Encouraging results on qualification of silica glass vacuum window assemblies are presented. In the area of magnetic sensors, progress of irradiation tests performed on ITER in-vessel LTCC inductive sensors is presented with outlook for novel technological approaches to inductive sensors utilizing thick printing and photolithography technologies being highlighted. Summary of advancements in the area of steady state magnetic field sensors based on Hall effect is given. New results of neutron irradiation test of the ITER borosilicate glass inserts for vacuum electrical feedthroughs are summarized finding negligible swelling at target level of neutron fluence. Off-line irradiation tests of fiber optic current sensors for plasma current measurement demonstrated that both for gamma doses up to 5 MGy and a total neutron fluence up to 10 15 cm −2 , radiation induced changes are still compatible with required measurement accuracy on ITER. The ITER bolometers are given as an example how considering radiation effects may influence the diagnostic design. Finally, outlook for future main R&D directions is outlined. All optical and laser-based diagnostics in ITER will be using mirrors to guide plasma radiation toward detectors, cameras and sensors. In the hostile plasma, radiation and particle environment the optical characteristics of diagnostic mirrors will degrade directly affecting the entire performance of involved diagnostic systems. An assessment of factors affecting mirror performance is provided. Among the prime adverse factors are deposition of plasma impurities, sputtering of mirror surface and steam ingress in the vicinity of mirrors. Within the International Tokamak Physics Activity with active support by ITER central team and domestic agencies, the structured research and development (R&D) program on mitigation of risks for diagnostic mirrors is underway. Within this program the mirror material development, the passive mitigation of mirror degradation by using diagnostic ducts and shutters along with an active mirror recovery program comprising the in-situ mirror cleaning and calibration is underway. Recent developments in diagnostic mirror R&D are described in this Chapter along with an example of their implementation of R&D solutions in ITER Infrared Thermography diagnostic. An assessment of still open engineering and physics questions, considerations on mirror risks during an early phase of ITER operation are given along with an overview of diagnostic mirror evolution in the late ITER operation stage toward the demonstration fusion power plant. Several crucial areas of diagnostic R&D outlined in ITER Research Plan are addressed. The basic control groups in a fusion reactor can be broken-down in five categories: (1) plasma position, magnetic configuration, and plasma current control, (2) profile control and confinement optimization, (3) MHD control and suppression, (4) edge dissipation control, radiation and plasma exhaust control and (5) break-down optimization. These categories are coupled via the physics (a control action in one domain will affect the other domains) and via shared actuators (e.g. ECRH for impurity accumulation avoidance, current density distribution control and MHD suppression). Consequently, a supervisory control system should determine the priority of the various control tasks, their couplings, and the interfaces with the safety and interlock system. For the systematic development of the various controllers taking the complexity of the plasma and the control system into account, a model-based approach is required. A short historical overview is given of the developments in systems and control theory and control engineering with special emphasis on those developments that are most relevant for Nuclear Fusion research and operation. An overview is given of the state of the field of fusion plasma control for the control categories. It will be shown how synthetic diagnostics are being developed in ITER and how they are used in diagnostic design and design validation and how they can be in model-based controller synthesis using relatively simple models. In modern control methods, multiple diagnostics are used to constrain relatively simple models. The constrained models provide an estimate for the state. This opens the route to state controllers, such as model predictive control. A major challenge in nuclear fusion research is the coherent combination of data from heterogeneous diagnostics and modeling codes for machine control and safety as well as physics studies. Measured data from different diagnostics often provide information about the same subset of physical parameters. Additionally, information provided by some diagnostics might be needed for the analysis of other diagnostics. A joint analysis of complementary and redundant data allows, e.g. to improve the reliability of parameter estimation, to increase the spatial and temporal resolution of profiles, to obtain synergistic effects, to consider diagnostics interdependencies and to find and resolve data inconsistencies. Physics-based modeling and parameter relationships provide additional information improving the treatment of ill-posed inversion problems. A coherent combination of all kind of available information within a probabilistic framework allows for improved data analysis results. The concept of integrated data analysis (IDA) in the framework of Bayesian probability theory is outlined and contrasted with conventional data analysis. Components of the probabilistic approach are summarized and specific ingredients beneficial for data analysis at fusion devices are discussed.

ITER↗

Study of electron-induced chemical transformations in polymers

In extreme ultraviolet (EUV) photoresist exposure, the primary and secondary electrons drive chemistry rather than the EUV photons themselves. These electrons have a wide range of energies below approximately 80 eV, which are capable of complex network of reactions during exposure. To better understand the ability of electrons of different energies within the EUV primary and secondary electron range, we want to characterize and compare the chemistry induced in pure polymer films by direct exposure to electrons. Thin films of poly(tert-butyl methacrylate), poly(methyl methacrylate), and poly(4-hydroxystyrene) were exposed to a 20 to 80 eV electron beam. Outgassing during exposure was characterized in-situ using a quadrupole residual gas analyzer. The thickness changes were measured using ellipsometry and chemical bond structure data were collected using Fourier-transform infrared spectroscopy (FTIR) after exposure to compare different exposure conditions. Poly(4-hydroxystyrene) demonstrated stability during electron exposures. Exposures of the other two materials led to outgassing of protecting groups, the intensity of which decayed in time. Outgassing, FTIR, and thickness loss data exhibited approximately linear relationships to each other.

Mueller, Maximillian↗

Understanding the Quadrupole Mass Filter and Testing a High-Resolution QMS RGA for ITER

A common type of residual gas analyzer is the quadrupole mass spectrometer. One of the main components within this instrument is a mass filter known as the quadrupole. It is responsible for the selective throughput of the ionized gas particles - by ascending mass number - prior to ion impacts on the analyzer (or detector) surface from which the ion current signal is generated for processing. However, the quadrupole is not fully described in relation to the electric field characteristics and the function as an ion mass separator. This paper describes the basic origins of the electrical design, the intricate assembly criteria, and performance of the quadrupole within the spectrometer. A specialized quadrupole mass spectrometer is part of a configuration for a diagnostic gas analyzer system planned for ITER, a fusion research machine. It has a verified capability, essential as a diagnostic criterion for this reactor project, to successfully deconvolute the mass signals of Helium-4 and deuterium (reactor fuel exhaust gases, separated by only 0.026 atomic mass units), down to a relative three-percent concentration of the former gas. The associated preliminary testing, performed at the Oak Ridge National Laboratory, is also addressed. Finally, one of the key parameters used to express gas concentration, the relative sensitivity factor, will be explained, including an evaluation of dependency on other variables.

Marcus, Chris [ORNL] (ORCID:0000000190139636)↗

Analysis of Off-Gas Streams from Small- and Large-Scale Sparging Salt Vessels using Laser-Induced Breakdown Spectroscopy

Laser-induced breakdown spectroscopy (LIBS) is being developed as an analytical monitoring tool for molten salt reactor (MSR) systems. A mobile LIBS platform was configured on a small-scale salt vessel (~100 g of salt) and then transported 0.6 km to successfully monitor an engineering-scale pumped salt loop (~100 kg of salt). Several studies on monitoring salt aerosols, hydrogen isotopes, and noble gases were performed on the small-scale system. All these studies were then implemented for monitoring various tests on the engineering-scale loop. Aerosolized salts from both the storage tank and pump bowl were monitored using LIBS to assess bulk salt analyte ratios (Mg, Na, K) and evaluate impurities (H, O, Ca). In addition to monitoring salt aerosols, LIBS was used in tandem with a residual gas analyzer (RGA) and a Raman spectroscopy system to detect hydrogen isotopes as they were sparged through and subsequently depleted from the loop storage tank. Lastly, a similar test with noble gases (100 ppm Kr, 1000 ppm Xe) was performed, in which LIBS demonstrated a faster response than the RGA used in-line. The tests and results are summarized in this report with detailed publications to follow. Key takeaways are listed in the conclusion of the report.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗