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At least 109 records · Page 6

Determination of nitrogen monoxide in high purity nitrogen gas with an atmospheric pressure ionization mass spectrometer

An atmospheric pressure ionization mass spectrometric (API-MS) method was studied for the determination of residual NO in high purity N2 gas. The API-MS is very sensitive to NO, but the presence of O2 interferes with the NO measurement. Nitrogen gas in cylinders as sample gas was mixed with NO standard gas and/or O2 standard gas, and then introduced into the API-MS. The calibration curves of NO and O2 has linearity in the region of 0 - 2 ppm, but the slopes changed with every cylinder. The effect of O2 on NO+ peak was additive and proportional to O2 concentration in the range of 0 - 0.5 ppm. The increase in NO+ intensity due to O2 was (0.07 - 0.13)%/O2, 1 ppm. Determination of NO and O2 was carried out by the standard addition method to eliminate the influence of variation of slopes. The interference due to O2 was estimated from the product of the O2 concentration and the ratio of slope A to Slope B. Slope A is the change in the NO+ intensity with the O2 concentration. Slope B is the intensity with O2 concentration.

Kato, K.↗

Recovery, Transportation and Acceptance to the Curation Facility of the Hayabusa Re-Entry Capsule

The "Hayabusa" re-entry capsule was safely carried into the clean room of Sagamihara Planetary Sample Curation Facility in JAXA on June 18, 2010. After executing computed tomographic (CT) scanning, removal of heat shield, and surface cleaning of sample container, the sample container was enclosed into the clean chamber. After opening the sample container and residual gas sampling in the clean chamber, optical observation, sample recovery, sample separation for initial analysis will be performed. This curation work is continuing for several manths with some selected member of Hayabusa Asteroidal Sample Preliminary Examination Team (HASPET). We report here on the 'Hayabusa' capsule recovery operation, and transportation and acceptance at the curation facility of the Hayabusa re-entry capsule.

Abe, M.↗

Removal of Bond Sodium from Full-Length Unirradiated Fermi-1 Blanket Elements and Assembly via Melt-Drain-Evaporate Process

Equipment was designed, fabricated, tested, and operated in an inert atmosphere radiological glovebox at Idaho National Laboratory to demonstrate the removal of bond sodium from full-length unirradiated Fermi-1 radial blanket elements and an entire radial blanket assembly using a Melt-Drain-Evaporate process. A series of three runs was performed with individual and multiple radial Fermi-1 blanket elements, and a fourth run was conducted with an entire Fermi-1 radial blanket assembly. After each run, the depleted uranium alloy slugs in every element slid out of its cladding, mechanically exhibiting the effectual absence of bond sodium. Quantitative and further qualitative analyses of the treated Fermi-1 material revealed the substantive, if not complete, absence of sodium metal in blanket element components. Indeed, entire columns of depleted uranium alloy slugs and associated cladding from select treated elements were separately contacted with water to react with residual sodium metal on the element surfaces, forming hydrogen gas. Samples of the resultant gas were analyzed to quantify the hydrogen concentration, which correlated to a residual sodium metal content for the treated element. Accordingly, no detectable sodium metal (<7 µg) was found on the surfaces of multiple depleted uranium alloy slugs after removal from its cladding. Detectable sodium metal, ranging from 14 to 30 µg, was found on the surfaces of one separated column of slugs and two separated full-length cladding segments. Each element originally contained ~25 g of bond sodium, resulting in quantitative sodium metal removal efficiencies of =99.9998%. The remaining separated uranium alloy slugs and cladding segments from the four runs were piece-wise immersed in alcohol while videorecording possible gas bubble formation as an additional qualitative analysis for residual sodium metal on treated surfaces, which identified the predominant absence of sodium reactivity on the balance of treated Fermi-1 blanket material. The results of this demonstration substantiate a path forward for treatment and disposal of 34 metric tons heavy metal of irradiated sodium-bonded Fermi-1 blanket material currently stored at Idaho National Laboratory.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Alternative Fuels Research Laboratory

NASA Glenn has invested over $1.5 million in engineering, and infrastructure upgrades to renovate an existing test facility at the NASA Glenn Research Center (GRC), which is now being used as an Alternative Fuels Laboratory. Facility systems have demonstrated reliability and consistency for continuous and safe operations in Fischer-Tropsch (F-T) synthesis and thermal stability testing. This effort is supported by the NASA Fundamental Aeronautics Subsonic Fixed Wing project. The purpose of this test facility is to conduct bench scale F-T catalyst screening experiments. These experiments require the use of a synthesis gas feedstock, which will enable the investigation of F-T reaction kinetics, product yields and hydrocarbon distributions. Currently the facility has the capability of performing three simultaneous reactor screening tests, along with a fourth fixed-bed reactor for catalyst activation studies. Product gas composition and performance data can be continuously obtained with an automated gas sampling system, which directly connects the reactors to a micro-gas chromatograph (micro GC). Liquid and molten product samples are collected intermittently and are analyzed by injecting as a diluted sample into designated gas chromatograph units. The test facility also has the capability of performing thermal stability experiments of alternative aviation fuels with the use of a Hot Liquid Process Simulator (HLPS) (Ref. 1) in accordance to ASTM D 3241 "Thermal Oxidation Stability of Aviation Fuels" (JFTOT method) (Ref. 2). An Ellipsometer will be used to study fuel fouling thicknesses on heated tubes from the HLPS experiments. A detailed overview of the test facility systems and capabilities are described in this paper.

Surgenor, Angela D.↗

Differential Organic Carbon Mineralization Responses to Soil Moisture in Three Different Soil Orders Under Mixed Forested System: Supporting Data

This data contains data from 90-day long incubation study which aimed to look at the soil moisture-texture relationship on soil organic carbon (SOC) cycling. Soils were collected from three distinct soil textures from mixed forests in 2017: sandy (Georgia, 2017-05-01), loamy (Missouri, 2017-06-14) and clayey (Texas, December 2017) were incubated at different soil moisture levels (air-dried, 25% water holding capacity (WHC), 50% WHC, 100% WHC and 175% WHC) at room temperature for a period of 90 days. Files contain microbial respiration, active and slow SOC pools, and their respective mineralization rates, extractable organic carbon (C), and C-acquiring extracellular enzymes. Findings from these data were used in Singh et al. (2021). This study aimed to examine the interactive effect of soil moisture and texture on SOC mineralization. Soil samples of three distinct textures (sandy, loamy, and clayey) were collected from mixed forests of Georgia, Missouri, and Texas, respectively. Soil cores of 5 cm diameter were collected from numerous random locations at each site from 0-15 cm depth after scraping the litter layer and mixed thoroughly to obtain a composite sample per site. Three additional soil cores were collected to determine the WHC using pressure plate extractors. Soil samples were composited, and triplicate soil samples were incubated in mason jars for a period of 90 days at room temperature under different moisture regimes: air dried, 25% WHC, 50% WHC, at WHC and 100% saturation. Soil respiration was measured weekly, and destructive sampling was conducted at 1, 15, 60, and 90 days to determine extractable organic C, C acquiring enzyme activity, and active and slow SOC pools with their respective mineralization rates. The C acquiring enzyme activity was the total activity of α-glucosidase, β-glucosidase, cellobiohydrolase, and β-xylosidase enzymes. Gas samples for microbial respiration measurements were collected from headspace of incubation jars through the sampling ports on the lids and then analyzed using a Shimadzu Gas Chromatograph (GC-2014). Prior to sampling, the vials were evacuated. Blank correction was also done by collecting gas samples from empty incubation jars. Double pool exponential decay model was used in SigmaPlot to determine the active and slow SOC pools and their mineralization rates (Farrar et al., 2012; Jagadamma et al., 2014). The C-acquiring extracellular enzymes were measured using the microplate method by German et al., (2011). Microbial community structure was determined using the phospholipid fatty acid (PLFA) and neutral lipid fatty acid (NLFA) analyses (Buyer and Sasser, 2012). This dataset has seven data files provided in comma-separate (*.csv) format. Additional metadata are provided: seven data dictionaries and a file-level metadata file in comma separate (*.csv) format and a user guide in PDF (*.pdf) format.

Carbon acquiring enzyme activity↗

Specification of FIPD Fission Gas Chemistry Data

The current FIPD library contains two main sets of fission gas chemistry data. The first set is data collected during the Integral Fast Reactor (IFR) program from 1984 to 1994, using a gas mass spectrometry system located in the Analytical Laboratory (AL) at Argonne National Laboratory-West (Argonne-West). Throughout this period, numerous fission gas release and chemistry datasets were gathered from a variety of metallic fuel pins. The fission gas was sampled by the Gas Assay, Sample and Recharge (GASR) System in the Hot Fuel Examination Facility (HFEF) and transferred to the AL to perform gas composition and isotopic abundance analysis. The second set is data collected after the IFR program. The fission gas samples were also collected by the GASR system at the HFEF, but analyzed using a similar gas mass spectrometer located in Pacific Northwest National Laboratory (PNNL). Many fuel pins irradiated in Experimental Breeder Reactor II (EBR-II) and the Fast Flux Test Facility (FFTF) were measured, including the fuel pins for the MFF series of experiments, designed to qualify metal fuel for use as driver fuel in the FFTF and X496 experiment. For either set of data, fission gas was sampled with the gas sampling line in GASR using sample bottles after the capsule/element volume has been determined and the system is still full of radioactive gas. The sample bottles were then transferred to the sample packaging cylinder or an approved storage location pending transfer to the AL or prepared for shipment to another laboratory (such as PNNL) for analysis of the collected gas as directed on the GASR data form, other approved form. The receiving laboratories (AL or PNNL) required their Analytical Service Request form to be completed prior to sample transfer. Typical sample transfer processes were initiated at HFEF by the principal or process engineer. The laboratories performing the analyses (AL or PNNL) use the sample bottle numbers as well as a sample number produced by the respective laboratory. HFEF and the responsible experimenter tracked the sample using the analysis number, the gas bottle number, and the fuel pin number.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Near-Surface Imaging of the Multicomponent Gas Phase above a Silver Catalyst during Partial Oxidation of Methanol

Fundamental chemistry in heterogeneous catalysis is increasingly explored using operando techniques in order to address the pressure gap between ultrahigh vacuum studies and practical operating pressures. Because most operando experiments focus on the surface and surface-bound species, there is a knowledge gap of the near-surface gas phase and the fundamental information the properties of this region convey about catalytic mechanisms. In this work, we demonstrate in situ visualization and measurement of gas-phase species and temperature distributions in operando catalysis experiments using complementary near-surface optical and mass spectrometry techniques. The partial oxidation of methanol over a silver catalyst demonstrates the value of these diagnostic techniques at 600 Torr (800 mbar) pressure and temperatures from 150 to 410 °C. Planar laser-induced fluorescence provides two-dimensional images of the formaldehyde product distribution that show the development of the boundary layer above the catalyst under different flow conditions. Raman scattering imaging provides measurements of a wide range of major species, such as methanol, oxygen, nitrogen, formaldehyde, and water vapor. Near-surface molecular beam mass spectrometry enables simultaneous detection of all species using a gas sampling probe. Detection of gas-phase free radicals, such as CH 3 and CH 3 O, and of minor products, such as acetaldehyde, dimethyl ether, and methyl formate, provides insights into catalytic mechanisms of the partial oxidation of methanol. The combination of these techniques provides a detailed picture of the coupling between the gas phase and surface in heterogeneous catalysis and enables parametric studies under different operating conditions, which will enhance our ability to constrain microkinetic models of heterogeneous catalysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A Study of the Combustion of Aluminum Borohydride in a Small Supersonic Wind Tunnel

The combustion of aluminum borohydride in the Mach 2 airstream of a 3.84- by 10-inch wind tunnel was studied by analyzing gas samples taken from the airstream. Gas mixture composition was determined with the aid of a vacuum apparatus and gas chromatograph. The overall combustion efficiency of the fuel was assumed to be good because the combustion efficiency of its hydrogen component was found to be high. The increase of the lateral surface area of the combustion region was dependent upon the degree of mixing of fuel and its combustion products with air. In the flame zone where there was insufficient oxygen for complete combustion, the metal components of the fuel appeared to burn preferentially to the hydrogen component.

Allen, Harrison, Jr.↗

Gas-flow restrictor

Gas flow restrictor is described, consisting of predetermined length and size of capillary tubing to control flow rate of carrier gas into gas chromatograph of flow rate of sample gas into mass spectrometer inlet system. Length and inner diameter of capillary tubing was estimated with mathematical expressions for viscous flow.

Bastien, G. J.↗

Hot Hydrogen Testing of Refractory Metals and Ceramics

The objective of this investigation is to develop a technique with which refractory metal carbide samples can be exposed to hydrogen containing gases at high temperatures, and to use various microstructural and analytical techniques to determine the chemical and rate processes involved in hydrogen degradation in these materials. Five types of carbides were examined including WC, NbC, HfC, ZrC, and TaC. The ceramics were purchased and were all monolithic in nature. The temperature range investigated was from 850 to 1600 C with a hydrogen pressure of one atmosphere. Control experiments, in vacuum, were also conducted for comparison so that the net effects due to hydrogen could be isolated. The samples were analyzed prior to and after exposure. Gas samples were collected in selected experiments and analyzed using gas chromography. Characterization of the resulting microstructure after exposure to hydrogen was conducted using optical microscopy, x-ray diffraction, scanning electron microscopy, and weight change. The ceramics were purchased and were all monolithic in nature. It was found that all samples lost weight after exposure, both in hydrogen and vacuum. Results from the microstructure analyses show that the degradation processes are different among the five types of ceramics involved. In addition, the apparent activation energy for the degradation process is a function of temperature even within the same material. This indicates that there are more than one mechanism involved in each material, and that the mechanisms are temperature dependent.

Zee, Ralph↗

Analysis of liquid rocket combustion chamber turbulence levels from diffusion data

The intensity of turbulence and the Lagrangian correlation coefficient in a liquid-rocket combustion chamber have been analytically determined from an analysis of experimental diffusion data obtained in a small rocket engine which operated at 300-psia chamber pressure and produced approximately 250 pounds thrust. Results of gas-sample measurements obtained by Orsat and gas-chromatograph techniques to determine helium-concentration profiles were analyzed on the basis of Taylor's (1921) turbulent diffusion theory to obtain turbulence flow-field parameters. The results of the analysis indicate that turbulent diffusion in a combustion chamber can be adequately modeled by the one-dimensional Taylor theory, which assumes that the intensity of turbulence is a function only of axial distance in the chamber and that the Lagrangian correlation coefficient is expressed by a power law. The results indicate a higher intensity of turbulence and lower correlation than previously expected.

Smith, L. O., Jr.↗

Galileo Probe Mass Spectrometer experiment

The chemical and isotopic composition of the Jupiter atmosphere's constituents, including their vertical variations, will be measured by the Galileo Probe Mass Spectrometer instrument through in situ sampling; batch sampling will also be undertaken for noble gas composition and isotopic ratio determinations. The instrument's gas-sampling system is connected to a quadrupole mass analyzer for molecular weight analysis. Threshold values are lowered through sample enrichment by a factor of 100-500 for stable hydrocarbons and by a factor of 10 for noble gases. The instrument follows a sampling sequence of 8192 steps, at a rate of 2 steps/sec.

Niemann, H. B.↗

Isothermal Calorimetric Observations of the Affect of Welding on Compatibility of Stainless Steels with High-Test Hydrogen Peroxide Propellant

Compatibility is determined by the surface area, the chemical constituency and the surface finish of a material. In this investigation exposed area is obviously not a factor as the welded samples had a slightly smaller surface than the unwelded, but were more reactive. The chemical makeup of welded CRES 316L and welded CRES 304L have been observed in the literature to change from the parent material as chromium and iron are segregated in zones. In particular, the ratio of chromium to iron in CRES 316L increased from 0.260 to 0.79 in the heat affected zone (HAZ) of the weld and to 1.52 in the weld bead itself. In CRES 304L the ratio of chromium to iron increased from 0.280 to 0.44 in the HAZ and to 0.33 in the weld bead. It is possible that the increased reactivity of the welded samples and of those welded without purge gas is due to this segregation phenomenon. Likewise the reactivity increased in keeping with the greater roughness of the welded and welded without purge gas samples. Therefore enhanced roughness may also be responsible for the increased reactivity.

Gostowski, Rudy C.↗

Subminiaturized gas chromatograph gives fast, efficient analysis

Space oriented, lightweight, subminiaturized gas chromatograph analyzes gas samples in a few seconds with a carrier gas flow of one milliliter per second. In extraterrestrial exploration, the system could be used with a mass spectrometer for detection of life-supporting compounds.

Wilhite, W. F.↗

Improved "spectrophone"

Spectral lines of gas sample are modulated by electric field in optoacoustic gas analyzer. Pressure fluctuations caused by local heating of absorbing gas are picked up by microphone. Since laser is operated in continuous-wave (CW) mode, background noise due to heating of windows is eliminated.

Margolis, J. S.↗