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DOE OSTI2023

TGA Study of the Reaction Kinetics of a CuFeMnAlO 4+δ Oxygen Carrier for Methane Chemical Looping Combustion under High Pressure and Atmospheric Pressure Conditions

Reduction and oxidation kinetics of a CuFeMnAlO 4+δ oxygen carrier for methane were studied using an atmospheric thermogravimetric analyzer (TGA) and a pressurized TGA. Important parameters such as temperature (500–900 °C), particle size distribution (150–650 μm), and partial pressures of reactants (methane and oxygen) were evaluated. Results showed that the reduction of the oxygen carrier was not affected by particle size distribution studied in this work, and that above 750 °C, the effect of the temperature on oxygen carrier reduction started to diminish. The reaction time approaches an asymptotic limit as methane partial pressure increases. For oxygen carrier oxidation, it was found that the rate of oxidation increased with increasing oxygen concentration. The effect of the oxygen concentration was more noticeable when the oxygen concentration was below 7.5%. Because of the inherent feature of the oxygen carrier, its chemical looping with oxygen uncoupling property was also assessed. A phase boundary-controlled shrinking sphere model was used to model the test data from the TGAs. Modeling results showed that the oxygen carrier reduction had a reaction order of 1 with an activation energy of ∼46 kJ/mol. Oxygen carrier oxidation demonstrated a reaction order of 1.1 with an activation energy of ∼55 kJ/mol. Additionally, the differences of the experimental results between the atmospheric pressure TGA and the pressurized TGA were discussed in detail and the limitations of the pressurized TGA were highlighted.

Hydrocarbons↗

NASA NTRS1989

Online submicron particle sizing by dynamic light scattering using autodilution

Efficient production of a wide range of commercial products based on submicron colloidal dispersions would benefit from instrumentation for online particle sizing, permitting real time monitoring and control of the particle size distribution. Recent advances in the technology of dynamic light scattering (DLS), especially improvements in algorithms for inversion of the intensity autocorrelation function, have made it ideally suited to the measurement of simple particle size distributions in the difficult submicron region. Crucial to the success of an online DSL based instrument is a simple mechanism for automatically sampling and diluting the starting concentrated sample suspension, yielding a final concentration which is optimal for the light scattering measurement. A proprietary method and apparatus was developed for performing this function, designed to be used with a DLS based particle sizing instrument. A PC/AT computer is used as a smart controller for the valves in the sampler diluter, as well as an input-output communicator, video display and data storage device. Quantitative results are presented for a latex suspension and an oil-in-water emulsion.

Nicoli, David F.↗

NASA NTRS1991

Dust in the Mars atmosphere

The amount of dust suspended in the Martian atmosphere is highly variable with location and with time. The opacity of the sky is best known at the two Viking Lander sites, where visual, vertical-column optical depth never fell below a value of a few tenths during the 1.25 Mars years of observations and yet exceeded 2 to 3 during two great dust storms in 1977. Elsewhere on the planet, optical depths have been estimated from orbiter visible imaging of surface contrasts and from mapping of infrared emission from the surface and the overlying (dusty) atmosphere. In many cases these opacities (and thus dust amounts) may be uncertain by as much as a factor of two. Viking Lander observations of twilight indicate that the background dust haze is more or less uniformly mixed with altitude in the lower atmosphere. Observations from spacecraft indicate that there may be come seasonal variations to the height of these dust hazes, which sometimes extend above 30 km. (Ice haze layers may occur as high as 80 km.) The existing observations do not constrain the composition or the size distribution of the suspended dust particles very well. Remote sensing observations depend principally upon the product of the number of particles, the geometric cross-sections (and so particle size and shape), and the extinction efficiency of the particles (and so the particle composition), as integrated over the particle size distribution and along the line of sight. While the observed variation of dust opacity with wavelength constrains these quantities, it does not often permit the unique determination of the individual properties of the suspended dust. A size distribution having a cross-section weighted mean particle radius of 2.5 microns was deduced from a synthesis of the IR thermal emission spectra observed in the Southern Hemisphere by Mariner 9 during the 1971 global dust storm. Although the IR thermal emission is relatively insensitive to the sub-micron sized particles which tend to dominate visible opacity, this same size distribution was consistent with modeling of the sky brightness variation near the sun, as seen through the background haze above the Viking lander sites in the Northern Hemisphere.

Zurek, R. W.↗

DOE OSTI2020

Cesium Removal and Hydraulic Performance Comparisons of CST Ion Exchange Media Batches in Support of the Tank Closure Cesium Removal Project - 20522

Three batches of Crystalline Silicotitanate (CST) ion exchange media have been evaluated for cesium removal efficiency from a Savannah River Site (SRS) High Level Waste (HLW) supernate simulant in support of the Tank Closure Cesium Removal (TCCR) Project, which involves at-tank column waste treatment. Results will be utilized to select the CST media batch to be added to the next TCCR unit columns. Two of the CST media samples were recent production batches and the third was an archived batch studied extensively at SRS nearly two decades ago. The archived CST batch had a significantly smaller average particle diameter than more recent batches. Small-scale (∼23 mL), side-by-side column tests were conducted at 35 deg. C with each of the CST batches using the same simulant at flow rates near 1.2 mL/min (3.0-3.4 CST bed volumes/hr). The cesium ion exchange column performance results were lower than expected for all three CST batches, but the data indicated that 30% more simulant volume and 40% more equivalent CST bed volumes of solution can be processed with the older CST batch prior to reaching the 50% cesium breakthrough point than can be processed with the newer CST batches. Hydraulic evaluations of the CST columns were also conducted in simulant at 24 deg. C to determine the impact of the different particle size distributions and associated bed porosities on frictional pressure drop under dynamic flow conditions. Higher differential pressure drops were observed with the archived CST batch relative to recent production batches, due to the smaller particle size distribution and the packing characteristics of the archived batch. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2021

ARM Aerial Facility (AAF) - Unmanned Aircraft Systems, Miniaturized Optical Particle Counter

The Miniaturized Optical Particle Counter (or mini-OPC) measures particle number size distribution.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2026

Portable Optical Particle Spectrometer aboard an Airborne Platform (POPS_AIR) Instrument Handbook

The U.S. Department of Energy Atmospheric Radiation Measurement (ARM) user facility portable optical particle spectrometer (POPS) is a lightweight particle spectrometer designed for aerosol particle size distribution measurement. Several POPS of different versions have been procured to serve as routine instruments for the ARM Aerial Facility (AAF) unmanned aerial systems (UAS) and tethered balloon system (TBS) deployment since 2018. POPS measures the aerosol particle size distribution approximately between 0.13 and 3 μm.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

U Metal Oxidation with Steam (U)

The Savannah Rive National Laboratory 9SRNL) is evaluating a method to produce uranium oxide (UO 2 ) from uranium metal using steam. The typical methods for making UO 2 yield powders with particle-size ranges of 1 to 50 micron. The goal of the steam oxidation is to produce a depleted uranium (DU) product with a larger particle size that can be used as a surrogate for testing physical and mechanical process techniques to refine uranium and/or plutonium bearing residues. Several studies in the literature indicated that reactions between uranium metal and steam will yield UO 2 as fine powders in the 160 to 500 °C range, but granular materials form above 500°C. Above 880 °C, a hard compact scale forms on the U metal. Furthermore, sintering of UO 2 occurs at about 1300 °C, but it has been stated that the presence of steam enhances the sintering characteristics of UO 2 . Initial studies into the oxidation of DU metal in an atmosphere of argon and steam have been completed. Oxidation of depleted uranium metal in Ar/steam at 600, 710, 700, and 830 °C yielded at UO 2 product with little or no impurity at each temperature. Although not enough sample was available to perform sieve analysis for particle size distribution, SEM images reveal that a significant volume fraction of the products at 710, 770, and 830 °C exceeds 100 microns. The material produced at 600 °C was too fine for programmatic needs. Questions associated with the UO 2 include morphology of product, mechanical strength of the particles, and performance in milling operations. The size of the samples produced in these tests did not allow for quantitative assessment of particle size of mechanical strength. A qualitative assessment of the particles formed at 710, 770, and 830 °C was that the samples produced at 710 and 770 °C were friable, and the sample produced 830 °C had more mechanical strength. Sintering of the samples in Ar/steam at 970 °C appeared to increase the strength of the particles without changing their general particle size characteristics. Due to the small sample sizes, the increase in strength could not be quantified. If the sintering at 970 °C is inadequate, higher sintering temperatures in Ar/steam can be evaluated. Future work will increase scale of the steam oxidation conditions which yield the most-favorable particle-size distributions with sufficient mechanical strength for programming usage. Further consideration will be given to oxidation temperature, steam addition to the reaction vessel, U metal pretreatment, and sintering conditions after oxidation. The UO 2 production could involve a two-step process where particles are formed in steam at lower temperatures (700-850 °C) and then sintered in Ar/steam at elevated temperatures (950-1200 °C). Larger samples (50-100 g each) will provide sufficient UO 2 product for sieve analysis and assessment of mechanical strength relatives to subsequent milling operations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1975

Analysis of spectrophotometric observations of Venus in the 3-4 micron region

Spectrophotometric data of Venus in the 3-4 micron region are analyzed in the context of current ideas concerning cloud properties. The results show that a homogeneous cloud model, using a unimodal particle size distribution compatible with the results of previous polarization studies, cannot satisfactorily explain the infrared observations. Assuming a composition of 75% H2SO4, agreement is possible if an upper layer of smaller particles is added to the homogeneous cloud. This inhomogeneous cloud structure, however, is not in agreement with the polarization results. Other models, involving bimodal particle size distributions, were also unsuccessful in explaining both sets of observations in a consistent manner.

Martonchik, J. V.↗

DOE OSTI2021

Estimating reaction parameters in mechanism-enabled population balance models of nanoparticle size distributions: A Bayesian inverse problem approach

In order to quantitatively predict nano- as well as other particle-size distributions, one needs to have both a mathematical model and estimates of the parameters that appear in these models. Here, we show how one can use Bayesian inversion to obtain statistical estimates for the parameters that appear in recently derived mechanism-enabled population balance models (ME-PBM) of nanoparticle growth. The Bayesian approach addresses the question of “how well do we know our parameters, along with their uncertainties?.” The results reveal that Bayesian inversion statistical analysis on an example, prototype $\mathrm{lr(0)_n}$ nanoparticle formation system allows one to estimate not just the most likely rate constants and other parameter values, but also their SDs, confidence intervals, and other statistical information. Moreover, knowing the reliability of the mechanistic model's parameters in turn helps inform one about the reliability of the proposed mechanism, as well as the reliability of its predictions. Importantly, the paper can also be seen as a tutorial with the additional goal of achieving a “Gold Standard” Bayesian inversion ME-PBM benchmark that others can use as a control to check their own use of this methodology for other systems of interest throughout nature. Overall, the results provide strong support for the hypothesis that there is substantial value in using a Bayesian inversion methodology for parameter estimation in particle formation systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1985

A calculation of the Rosseland mean opacity of dust grains in primordial solar system nebulae

The Rosseland mean opacity owing to grains was calculated as a function of temperature and density for nebulae having solar elemental abundances. The values of the mean opacity were evaluated with a generalized formulation allowing for anisotropic scattering. The values of the mean opacity do not depend sensitively on the choice of the particle size distribution function, provided that there are few particles having sizes in excess of several tens of microns. The results indicate that thermal convection in primordial nebulae occurs over broader ranges of altitudes at low temperatures than at high temperatures, and for size distributions for which extensive aggregation has not yet occurred.

Pollack, J. B.↗

NASA NTRS2016

Aerosol Complexity and Implications for Predictability and Short-Term Forecasting

There are clear NWP and climate impacts from including aerosol radiative and cloud interactions. Changes in dynamics and cloud fields affect aerosol lifecycle, plume height, long-range transport, overall forcing of the climate system, etc. Inclusion of aerosols in NWP systems has benefit to surface field biases (e.g., T2m, U10m). Including aerosol affects has impact on analysis increments and can have statistically significant impacts on, e.g., tropical cyclogenesis. Above points are made especially with respect to aerosol radiative interactions, but aerosol-cloud interaction is a bigger signal on the global system. Many of these impacts are realized even in models with relatively simple (bulk) aerosol schemes (approx.10 -20 tracers). Simple schemes though imply simple representation of aerosol absorption and importantly for aerosol-cloud interaction particle-size distribution. Even so, more complex schemes exhibit a lot of diversity between different models, with issues such as size selection both for emitted particles and for modes. Prospects for complex sectional schemes to tune modal (and even bulk) schemes toward better selection of size representation. I think this is a ripe topic for more research -Systematic documentation of benefits of no vs. climatological vs. interactive (direct and then direct+indirect) aerosols. Document aerosol impact on analysis increments, inclusion in NWP data assimilation operator -Further refinement of baseline assumptions in model design (e.g., absorption, particle size distribution). Did not get into model resolution and interplay of other physical processes with aerosols (e.g., moist physics, obviously important), chemistry

Predictability↗

NASA NTRS2018

Particle Size Calibration Testing in the NASA Propulsion Systems Laboratory

The particle size characterization portion of the 2017 Propulsion Systems Laboratory (PSL) Cloud Calibration is described. The work focuses on characterizing the particle size distribution of the icing cloud as a function of simulated atmospheric conditions.These results will aid in upcoming ice crystal and supercooled liquid icing tests in PSL. Measurements acquired with the Phase Doppler Interferometer and High Speed Imaging instruments are presented. Experimental results indicate that the particle size distribution is primarily a function nozzle air and water pressures, and that air speed is not a significant effect for ice crystal clouds in PSL and both thermodynamic conditions and air speed are not significant effects for supercooled liquid water clouds in PSL.

Engine icing↗

NASA NTRS2019

Particle Size Calibration Testing in the NASA Propulsion Systems Laboratory

Engine Icing↗

NASA NTRS2008

Lunar Dust Characterization Activity at GRC

The fidelity of lunar simulants as compared to actual regolith is evaluated using Figures of Merit (FOM) which are based on four criteria: Particle Size, Particle Shape, Composition, and Density of the bulk material. In practice, equipment testing will require other information about both the physical properties (mainly of the dust fraction) and composition as a function of particle size. At Glenn Research Center (GRC) we are involved in evaluating a number of simulant properties of consequence to testing of lunar equipment in a relevant environment, in order to meet Technology Readiness Level (TRL) 6 criteria. Bulk regolith has been characterized for many decades, but surprisingly little work has been done on the dust fraction (particles less than 20 micrometers in diameter). GRC is currently addressing the information shortfall by characterizing the following physical properties: Particle Size Distribution, Adhesion, Abrasivity, Surface Energy, Magnetic Susceptibility, Tribocharging and Surface Chemistry/Reactivity. Since some of these properties are also dependent on the size of the particles we have undertaken the construction of a six stage axial cyclone particle separator to fractionate dust into discrete particle size distributions for subsequent evaluation of these properties. An introduction to this work and progress to date will be presented.

Street, Kenneth W.↗

DOE OSTI2021

Polarimetric Radar Variables in Snowfall at Ka- and W-Band Frequency Bands: A Comparative Analysis

Dual-frequency millimeter-wavelength radar observations in snowfall are analyzed in order to evaluate differences in conventional polarimetric radar variables such as differential reflectivity (ZDR) specific differential phase shift (K DP ) and linear depolarization ratio (LDR) at traditional cloud radar frequencies at Ka and W bands (~35 and ~94 GHz, correspondingly). Low radar beam elevation (~5°) measurements were performed at Oliktok Point, Alaska, with a scanning fully polarimetric radar operating in the horizontal–vertical polarization basis. This radar has the same gate spacing and very close beam widths at both frequencies, which largely alleviates uncertainties associated with spatial and temporal data matching. It is shown that observed Ka- and W-band Z DR differences are, on average, less than about 0.5 dB and do not have a pronounced trend as a function of snowfall reflectivity. The observed Z DR differences agree well with modeling results obtained using integration over nonspherical ice particle size distributions. For higher signal-to-noise ratios, KDP data derived from differential phase measurements are approximately scaled as reciprocals of corresponding radar frequencies indicating that the influence of non-Rayleigh scattering effects on this variable is rather limited. This result is also in satisfactory agreement with data obtained by modeling using realistic particle size distributions. Observed Ka- and W-band LDR differences are strongly affected by the radar hardware system polarization “leak” and are generally less than 4 dB. Smaller differences are observed for higher depolarizations, where the polarization “leak” is less pronounced. Realistic assumptions about particle canting and the system polarization isolation lead to modeling results that satisfactorily agree with observational dual-frequency LDR data.

42 ENGINEERING↗

DOE OSTI2023

ADVANCED TECHNIQUES FOR ENERGY INPUT REDUCTION IN GYPSUM WALLBOARD DRYING

Gypsum has been used for thousands of years in building and construction applications, starting with the pyramids in ancient Egypt, to “Plaster of Paris” in the midcenturies, and to the now-ubiquitous drywall in modern-day houses. Production of gypsum drywall boards takes several steps with high energy and water consumption. The current state of the art in industry is a process that begins by mining gypsum and reducing its particle size by milling. These gypsum particles undergo calcination to convert the gypsum (calcium sulfate dihydrate) into stucco (calcium sulfate hemihydrate). The stucco is mixed with additives and enough water to form a slurry that can be poured onto a conveyor belt and molded into the desired geometry. The stucco reacts with the water, converting back into gypsum. The remaining water is then dried from the board to form the final product. While only ~20 wt. % of water is needed for the conversion of stucco to gypsum, significant excess water is needed to ensure sufficient fluidity of the slurry for processibility. This is due to the low quality of the stucco particles produced in high throughput calcination units, which disintegrate upon mixing with water, thereby reducing the fluidity and processability of the slurry. This project aims to produce high-quality stucco particles by dielectric calcination. In doing so, particle integrity can be maintained through the slurry formulation step, and particle size distribution of the stucco can be adjusted to increase fluidity with less excess water. With less water remaining unreacted in the board, significant energy can be saved in drying the product. The project aims to 1) develop a dielectric calcination method to TRL 3, 2) determine optimal and practical particle size distributions to minimize excess water in the slurry, and 3) reduce the energy consumption of the drying process.

Conforti, Kameron↗

NASA NTRS1980

Numerical simulation of advection fog formation on multi-disperse aerosols due to combustion-related pollutants

The effects of multi-disperse distribution of the aerosol population are presented. Single component and multi-component aerosol species on the condensation/nucleation processes which affect the reduction in visibility are described. The aerosol population with a high particle concentration provided more favorable conditions for the formation of a denser fog than the aerosol population with a greater particle size distribution when the value of the mass concentration of the aerosols was kept constant. The results were used as numerical predictions of fog formation. Two dimensional observations in horizontal and vertical coordinates, together with time-dependent measurements were needed as initial values for the following physical parameters: (1)wind profiles; (2) temperature profiles; (3) humidity profiles; (4) mass concentration of aerosol particles; (5) particle size distribution of aerosols; and (6) chemical composition of aerosols. Formation and dissipation of advection fog, thus, can be forecasted numerically by introducing initial values obtained from the observations.

Hung, R. J.↗

NASA NTRS2016

Optical Extinction Measurements of Dust Density in the GMRO Regolith Test Bin

A regolith simulant test bin was constructed and completed in the Granular Mechanics and Regolith Operations (GMRO) Lab in 2013. This Planetary Regolith Test Bed (PRTB) is a 64 sq m x 1 m deep test bin, is housed in a climate-controlled facility, and contains 120 MT of lunar-regolith simulant, called Black Point-1 or BP-1, from Black Point, AZ. One of the current uses of the test bin is to study the effects of difficult lighting and dust conditions on Telerobotic Perception Systems to better assess and refine regolith operations for asteroid, Mars and polar lunar missions. Low illumination and low angle of incidence lighting pose significant problems to computer vision and human perception. Levitated dust on Asteroids interferes with imaging and degrades depth perception. Dust Storms on Mars pose a significant problem. Due to these factors, the likely performance of telerobotics is poorly understood for future missions. Current space telerobotic systems are only operated in bright lighting and dust-free conditions. This technology development testing will identify: (1) the impact of degraded lighting and environmental dust on computer vision and operator perception, (2) potential methods and procedures for mitigating these impacts, (3) requirements for telerobotic perception systems for asteroid capture, Mars dust storms and lunar regolith ISRU missions. In order to solve some of the Telerobotic Perception system problems, a plume erosion sensor (PES) was developed in the Lunar Regolith Simulant Bin (LRSB), containing 2 MT of JSC-1a lunar simulant. PES is simply a laser and digital camera with a white target. Two modes of operation have been investigated: (1) single laser spot - the brightness of the spot is dependent on the optical extinction due to dust and is thus an indirect measure of particle number density, and (2) side-scatter - the camera images the laser from the side, showing beam entrance into the dust cloud and the boundary between dust and void. Both methods must assume a mean particle size in order to extract a number density. The optical extinction measurement yields the product of the 2nd moment of the particle size distribution and the extinction efficiency Qe. For particle sizes in the range of interest (greater than 1 micrometer), Qe approximately equal to 2. Scaling up of the PES single laser and camera system is underway in the PRTB, where an array of lasers penetrate a con-trolled dust cloud, illuminating multiple targets. Using high speed HD GoPro video cameras, the evolution of the dust cloud and particle size density can be studied in detail.

lunar simulant↗