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Particle Analysis Pitfalls

This viewgraph presentation reviews the use of particle analysis to assist in preparing for the 4th Hubble Space Telescope (HST) Servicing mission. During this mission the Space Telescope Imaging Spectrograph (STIS) will be repaired. The particle analysis consisted of Finite element mesh creation, Black-body viewfactors generated using I-DEAS TMG Thermal Analysis, Grey-body viewfactors calculated using Markov method, Particle distribution modeled using an iterative Monte Carlo process, (time-consuming); in house software called MASTRAM, Differential analysis performed in Excel, and Visualization provided by Tecplot and I-DEAS. Several tests were performed and are reviewed: Conformal Coat Particle Study, Card Extraction Study, Cover Fastener Removal Particle Generation Study, and E-Graf Vibration Particulate Study. The lessons learned during this analysis are also reviewed.

Hughes, David

Ice Particle Analysis of the Honeywell AL502 Engine Booster

A flow and ice particle trajectory analysis was performed for the booster of the Honeywell ALF502 engine. The analysis focused on two closely related conditions one of which produced an icing event and another which did not during testing of the ALF502 engine in the Propulsion Systems Lab (PSL) at NASA Glenn Research Center. The flow analysis was generated using the NASA Glenn GlennHT flow solver and the particle analysis was generated using the NASA Glenn LEWICE3D v3.63 ice accretion software. The inflow conditions for the two conditions were similar with the main differences being that the condition that produced the icing event was 6.8 K colder than the non-icing event case and the inflow ice water content (IWC) for the non-icing event case was 50% less than for the icing event case. The particle analysis, which considered sublimation, evaporation and phase change, was generated for a 5 micron ice particle with a sticky impact model and for a 24 micron median volume diameter (MVD), 7 bin ice particle distribution with a supercooled large droplet (SLD) splash model used to simulate ice particle breakup. The particle analysis did not consider the effect of the runback and re-impingement of water resulting from the heated spinner and anti-icing system. The results from the analysis showed that the amount of impingement for the components were similar for the same particle size and impact model for the icing and non-icing event conditions. This was attributed to the similar aerodynamic conditions in the booster for the two cases. The particle temperature and melt fraction were higher at the same location and particle size for the non-icing event than for the icing event case due to the higher incoming inflow temperature for the non-event case. The 5 micron ice particle case produced higher impact temperatures and higher melt fractions on the components downstream of the fan than the 24 micron MVD case because the average particle size generated by the particle breakup was larger than 5 microns which yielded less warming and melting. The analysis also showed that the melt fraction and wet bulb temperature icing criterion developed during tests in the Research Altitude Test Facility (RATFac) at the National Research Council (NRC) of Canada were useful in predicting icing events in the ALF502 engine. The development of an ice particle impact model which includes the effects of particle breakup, phase change, and surface state is necessary to further improve the prediction of ice particle transport with phase change through turbomachinery.

Ice Accretion Codes

LEWICE3D/GlennHT Particle Analysis of the Honeywell Al502 Low Pressure Compressor

A flow and ice particle trajectory analysis was performed for the booster of the Honeywell AL502 engine. The analysis focused on two closely related conditions one of which produced a rollback and another which did not rollback during testing in the Propulsion Systems Lab at NASA Glenn Research Center. The flow analysis was generated using the NASA Glenn GlennHT flow solver and the particle analysis was generated using the NASA Glenn LEWICE3D v3.56 ice accretion software. The flow and particle analysis used a 3D steady flow, mixing plane approach to model the transport of flow and particles through the engine. The inflow conditions for the rollback case were: airspeed, 145 ms; static pressure, 33,373 Pa; static temperature, 253.3 K. The inflow conditions for the non-roll-back case were: airspeed, 153 ms; static pressure, 34,252 Pa; static temperature, 260.1 K. Both cases were subjected to an ice particle cloud with a median volume diameter of 24 microns, an ice water content of 2.0 gm3 and a relative humidity of 100 percent. The most significant difference between the rollback and non-rollback conditions was the inflow static temperature which was 6.8 K higher for the non-rollback case.

Ice Accretion Codes

Identifying Sample Provenance From SEM/EDS Automated Particle Analysis via Few-Shot Learning Coupled With Similarity Graph Clustering

Automated particle analysis (APA) provides a vast amount of compositional data via energy-dispersive X-ray spectroscopy along with size and shape data via scanning electron microscopy for individual particles in a sample. In many instances, APA data are leveraged to support identification of the source of a sample based on the detection of particles of a specific composition. Often, the particles that provide context make up a minuscule portion of the sample. Additionally, the interpretation of complex samples can be difficult due to the diversity of compositions both in the mixture and within a particle. In this work, we demonstrate a method to compute and cluster similarity graphs that describe inter-particle relationships within a sample using a multi-modal few-shot learning neural network. Here, as a proof-of-concept, we show that samples known to have been exposed to gunshot residue can be distinguished from samples occasionally mistaken for gunshot residue. Our workflow builds upon standard APA techniques and data processing methods to unveil additional information in a readily interpretable and quantitatively comparable format.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND

Automated Particle Analysis of Hanford Tank Wastes 241-AN-106, 241-AN-101, and 241-AW-105

This effort is involved in developing particle size and density distribution (PSDD) for the major phases within Hanford tank waste sludge. The object of this work has been to use automated particle analysis (APA) methods on the Scanning Electron Microscope (SEM) to provide PSDDs. The PSDD can be used to quantify the proportion of gibbsite particles likely to settle quickly and enable blending of wastes that may be prone to pipeline plugging such as the uranium phase, clarkeite with other wastes. The Hanford tank waste solids were analyzed with SEM combined with x-ray Energy Dispersive Spectroscopy (EDS) using APA. This method can allow thousands of individual particles to be characterized and so may provide a more representative view of the samples and information PSDDs. We characterized several as-received sludge samples and developed PSDD with APA. Sample preparation methods were found to impact the collected results, as it was more difficult to collect representative samples of the larger particles. Much of the material was also dried and cemented together that further impacted results.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W

Biological particle analysis by mass spectrometry

An instrument that analyzes the chemical composition of biological particles in aerosol or hydrosol form was developed. Efforts were directed toward the acquisition of mass spectra from aerosols of biomolecules and bacteria. The filament ion source was installed on the particle analysis by mass spectrometry system. Modifications of the vacuum system improved the sensitivity of the mass spectrometer. After the modifications were incorporated, detailed mass spectra of simple compounds from the three major classes of biomolecules, proteins, nucleic acids, and carbohydrates were obtained. A method of generating bacterial aerosols was developed. The aerosols generated were collected and examined in the scanning electron microscope to insure that the bacteria delivered to the mass spectrometer were intact and free from debris.

Vilker, V. L.

Quantitative Particle Analysis of Neptunium-237 Oxides: Optimization of MAMA Analysis for Modified Direct Denitration Products

The production of plutonium-238 through irradiation of neptunium-237 ( 237 Np) target materials for the use in radioisotope thermoelectric generators is paramount for continued deep space exploration. This work employs scanning electron microscopy to analyze 237 Np materials coupled with a well-developed image analysis framework (Morphological Analysis for Material Attribution, or MAMA) to determine the degree of micron-scale homogeneity in the materials. This work demonstrated how the quantification of particle characteristics can validate production materials and affirm the qualitative similarities observed in micrographs. The 237 Np oxide particle analysis determined that the materials from five production runs were quantitatively homogenous (significant at α = 0.05) in particle area, circularity, equivalent circular diameter, and ellipse aspect ratio, with two of the sampling dates having statistically significant different means for one of the four characteristics. Furthermore, these metrics not only confirm general homogeneity of the material but also expand the application of MAMA workflows to 237 Np materials, demonstrating the utility of MAMA analysis for a wider breadth of nuclear materials than previously reported. In the open literature, this study is the first time that these microanalytical techniques were applied to 237 Np materials to this degree.

MAMA

Cleaning Genesis Solar Wind Collectors with Ultrapure Water: Residual Contaminant Particle Analysis

Additional experience has been gained in removing contaminant particles from the surface of Genesis solar wind collectors fragments by using megasonically activated ultrapure water (UPW)[1]. The curatorial facility has cleaned six of the eight array collector material types to date: silicon (Si), sapphire (SAP), silicon-on-sapphire (SOS), diamond-like carbon-on-silicon (DOS), gold-on-sapphire (AuOS), and germanium (Ge). Here we make estimates of cleaning effectiveness using image analysis of particle size distributions and an SEM/EDS reconnaissance of particle chemistry on the surface of UPW-cleaned silicon fragments (Fig. 1). Other particle removal techniques are reported by [2] and initial assessment of molecular film removal is reported by [3].

Allton, J. H.

Skylab contamination results: S052 particle analysis and T025 analysis

The size and velocity distributions of 500 contaminant particles in the near environs of Skylab were determined from video tape data obtained by the high altitude observatory's white light coronagraph. A complete listing of derived particle parameters, their frequency distributions, and their behavior as a function of time are presented. A correlation between particle size and velocity is noted, and at least two prominent directions of the particle spacecraft origins are identified.

Schuerman, D. W.

Multi-Angle Snowflake Camera, particle analysis

The c1 level data product for the Mutli-Angle Snowflake Camera contains snowflake fall speeds and particle size, among other analysis for images associated with each hydrometeor.

54 ENVIRONMENTAL SCIENCES

Wear particle analysis using the ferrograph

The use of the Ferrograph in analyzing wear particles from a variety of different sources is reported. Examples of wear particles from gas turbine engines, bearing tests, friction and wear tests, hydraulic systems, and human joints are illustrated. In addition, the separation of bacteria and human cells is described.

Jones, W. R., Jr.

High-speed particle analysis using forward and backward two-dimensional angular optical scattering

Measurement of two-dimensional angle-resolved optical scattering (TAOS) patterns is an attractive technique for detecting and characterizing micron-sized high-speed flying particles. The elastic-scattering intensity pattern from a single particle as a function of spherical coordinate angles θ and ϕ provides detailed information on the particle’s morphology. By use of an ellipsoidal reflector and a high-speed CCD camera, scattering from a CW-laser was detected and resolved over a large angular range (θ from 12° to 168° and ϕ from 0° to 360°) from spherically shaped particles (e.g., amorphous silica and borosilicate glass) flowing through the reflector’s focal plane at speeds of 20 to 30 m/s. The scattering pattern from individual particles flying through the focal plane of the ellipsoid mirror provides insights about a particle’s size, clustering, roughness, and velocity.

Optics and optical instruments

Preliminary Examination of Returned Samples From Bennu Using Quantitative Particle Analysis in the Scanning Electron Microscope

The sample of regolith collected from asteroid Bennu by NASA’s OSIRIS-REx spacecraft will land in Utah on September 24, 2023. A 100-mg aliquot of fine Bennu dust adhering to the internal surfaces of the sample return capsule and associated hardware will be collected by curation staff during disassembly and analyzed immediately by members of the sample analysis team in a “Quick-Look” (Q-L) procedure. The Q-L objectives are (1) to provide images for release to the public to inform on the nature of the returned sample, and (2) to perform a reconnaissance investigation of the mineralogic characteristics of the returned material for science purposes. We will determine the minerals that occur in the dust, assess their diversity, and determine relative abundances at the >5% level using a combination of optical microscopy, Fourier-transform infrared spectroscopy, X-ray powder diffraction, and field-emission scanning electron microscopy (SEM). Here we describe the procedures and techniques developed for the Q-L analyses using analog samples analyzed by SEM equipped with energy dispersive X-ray spectroscopy (EDX). To test these techniques, we have applied them to several samples, including powders of the Murchison (Fig. 1) and Orgueil meteorites, as well as simulant samples prepared by the mission.

OSIRIS-REx

Evaluating the feasibility of LA-ICP-TOF-MS for the analysis of environmental particle collections

Laser ablation-inductively coupled plasma-time-of-flight-mass spectrometry (LA-ICP-TOF-MS) was employed to rapidly analyze environmental particle samples collected using aerosol contaminate extractors (ACE). The ACE particle collectors were placed at various distances (0.5, 1.3, and 4.5 km) from a source that released Ru-bearing particles. Samples for measurement were then generated (as sub-samples) from the ACE collection plates via particle “lift off” with gunshot residue (GSR) tabs. The LA-ICP-TOF-MS method was employed such that 10+ samples could be analyzed in a single unattended analytical session. A 3 × 1 mm area of individual GSR tab samples were analyzed in less than 30 minutes. This provided spatially resolved elemental and isotopic measurements of the particulate content and confirmed the presence of Ru-bearing particles within the complex background environmental particle loading. As anticipated, measurements showed collectors closest to the source had the highest concentration of the released Ru-bearing particles, while all collectors, regardless of distance, contained similar levels of background particles (e.g., Fe and Sr). Sequential scanning electron microscopy – automated particle analysis (SEM-APA) and LA-ICP-TOF-MS analysis was employed for method validation and a demonstration of the multi-modal approach. The same 2-dimensional region was analyzed by both methods and the particles identified via SEM-APA were also detected using LA-ICP-TOF-MS, with 100% accuracy. Overall, LA-ICP-TOF-MS demonstrated its utility for rapid elemental and isotopic particle analysis from environmental air samples.

Manard, Benjamin T. [Oak Ridge National Laboratory

Heliospheric energetic particle transport: Analysis of near-field-aligned particle propagation for SEP events observed by Wind and MAVEN

Magnetic field alignments of spacecraft over large distances in the heliosphere are rare and are usually very limited in duration. Cruise phases of planetary transfers, however, are an exception to this rule, given the Hohmann-Parker effect. The transfer of the MAVEN s/c in 2014 is one such example. Multiple (~10) solar particle events occurred and were detected at both MAVEN and the Wind s/c, originating from solar activity near the foot points of both s/c. We show initial analysis results of the data collected by the solar wind and energetic particle instruments on both s/c while they were more than 0.2 AU apart, but practically Parker field aligned. Using a 1D model, we present initial simulations in qualitative agreement with energetic electron measurements. Next step is to implement the 2D model with approximate particle release from the Sun, and transport durations between Sun, Earth, and MAVEN. We will discuss implications for this data-model comparison, including the possibility to constrain particle scattering inside 1 AU, as well as its radial dependence between Earth and MAVEN.

Solar Energetic Particles

Ice Particle Transport Analysis With Phase Change for the E(sup 3) Turbofan Engine Using LEWICE3D Version 3.2

Ice Particle trajectory calculations with phase change were made for the Energy Efficient Engine (E(sup 3)) using the LEWICE3D Version 3.2 software. The particle trajectory computations were performed using the new Glenn Ice Particle Phase Change Model which has been incorporated into the LEWICE3D Version 3.2 software. The E(sup 3) was developed by NASA and GE in the early 1980 s as a technology demonstrator and is representative of a modern high bypass turbofan engine. The E(sup 3) flow field was calculated using the NASA Glenn ADPAC turbomachinery flow solver. Computations were performed for the low pressure compressor of the E(sup 3) for a Mach 0.8 cruise condition at 11,887 m assuming a standard warm day for ice particle sizes of 5, 20, and 100 microns and a free stream particle concentration of 0.3 g/cu m. The impingement efficiency results showed that as particle size increased average impingement efficiencies and scoop factors increased for the various components. The particle analysis also showed that the amount of mass entering the inner core decreased with increased particle size because the larger particles were less able to negotiate the turn into the inner core due to particle inertia. The particle phase change analysis results showed that the larger particles warmed less as they were transported through the low pressure compressor. Only the smallest 5 micron particles were warmed enough to produce melting and the amount of melting was relatively small with a maximum average melting fraction of 0.836. The results also showed an appreciable amount of particle sublimation and evaporation for the 5 micron particles entering the engine core (22 percent).

Bidwell, Colin, S.

Particle signal considerations for isotope ratio analysis with single particle multi-collector inductively coupled plasma mass spectrometry

Particle analysis has benefitted from the advent of single particle inductively coupled plasma-mass spectrometry (spICP-MS) due to its robustness, sensitivity, and high-throughput nature. Previous methods of spICP-MS have typically utilized quadrupole or time-of-flight mass analyzers and therefore employ electron multiplier-based detectors (such as secondary electron multipliers or microchannel plates). However, to obtain precise measurements on elemental or isotopic ratios within individual particles, multi-collector ICP-MS (MC-ICP-MS) can be used. Here, we investigate Ce isotope ratios, specifically 142 Ce/ 140 Ce, by spMC-ICP-MS using an all-Faraday cup collector array. Using 1 μm (diameter) cerium dioxide particles, integration times of the Faraday cup detectors were varied from 50–500 ms. The signal from the cerium isotopes in the particles was used to determine isotope ratios, which closely matched the expected natural isotopic abundances. Due to the signal decay response from the Faraday cups, the signal from particles lasts much longer than the expected 1–2 ms (up to 100 s of ms). To explore this effect on isotope ratio analysis, multiple ratio analysis methods were used to determine how to obtain optimal precision and accuracy. Relative differences were around 2% for methods that calculated isotope ratios from summing the total signal of an individual particle before calculating the ratio (rather than using every data point individually). It was found that summing all data points per particle, or integrating under the signal peak, yielded both accurate and precise isotope ratios within the particle population. Particles were also sampled off a solid substrate via microextraction, and isotope ratios were determined with relative differences of 0.13% to 9%. This demonstrates the ability to use spMC-ICP-MS to obtain isotope ratios on particles, with little to no relative difference in comparison to the expected ratio, even when operating Faraday detectors at fast 50 ms integration times.

Szakas, Sarah E. [Oak Ridge National Laboratory (O