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At least 163 records · Page 9

Results and Implications of Mineralogical Models for Chemical Sediments at Meridiani Planum

The Mars Exploration Rover (MER) "Opportunity" has explored chemically-enriched sedimentary outcrops at Meridiani Planum, Mars. In its first year, three different crater sites - Eagle, Fram and Endurance - have been explored. Nineteen high-interest outcrop rocks were investigated by first grinding a hole to reach the interior (using the Rock Abrasion Tool, RAT), and then conducting APXS (alpha particle x-ray spectrometry) analysis, MB (M ssbauer) analysis, and close up imaging (MI, microscopic imager). Sixteen elements and four Fe-bearing minerals were assayed to good accuracy in each sample, producing 380 compositional data points. The Miniature Thermal Emission Spectrometer (Mini- TES) obtained spectra on outcrop materials which provide direct indication of several mineral classes. Preliminary reports on Eagle crater and three RAT samples have been published. Chemical trends and a derived mineralogical model for all RAT d outcrop samples to date has been developed.

Clark, B. C.↗

A Systematic Interpretation of Subsurface Proppant Concentration from Drilling Mud Returns: Case Study from Hydraulic Fracturing Test Site (HFTS-2) in Delaware Basin

The aim of this study is generation and validation of a proppant log using analysis of drilling mud returns for child wells. Proppant log provides qualitative as well as quantitative insights into spatial distribution of proppant sand particles from prior stimulation of parent wells. While the basic methodology was developed and formalized during analysis of material collected from through fracture cores at Hydraulic Fracturing Test Site in Midland Basin (HFTS – 1), the test wells at HFTS – 2 in the neighboring Delaware Basin allowed the opportunity to validate the workflow on actual mud return samples from subsurface. As a child well is being drilled, periodic mud return samples are collected at the rig site and preserved for analysis. The workflow involves systematic cleaning of the samples including various steps such as washing, drying and segregation of samples into relevant size fractions of interest (< Mesh 20) based on specifications of pumped sand during stimulation of the parent well. Clean samples are imaged using high resolution transparency scanning. Scan images are then systematically analyzed for particles of interest using computer vision techniques. Sample counts are further validated using elemental analysis of smaller sub-samples at various depths of interest. This step is necessary to isolate proppant versus other naturally occurring minerals such as sulphates and carbonates which show similar optical properties. We successfully correlated proppant distribution against the existing parent well and validated propped versus relatively un-propped zones for a child well at the test site. The advantage of testing the proppant log concept at the HFTS – 2 site is the plethora of additional diagnostic data that is available to validate our primary observations. We can correlate spatial proppant distribution against variability in stimulation response based on independent observations such as image logs, microseismic attributes as well as DAS response, all of which tend to corroborate one another. One of our significant successes was being able to describe varying degrees of impact of the parent well along the lateral length of a stimulated child well. Our workflow represents a systematic and one-of-a-kind interpretation of spatial proppant distribution while drilling child wells. This provides unique opportunities to better understand the current state of the Downloaded from http://onepetro.org/URTECONF/proceedings-pdf/21URTC/2-21URTC/D021S031R003/2477415/urtec-2021-5189-ms.pdf/1 by Carol Worster on 28 February 2022 URTeC 5189 2 reservoir being targeted including zones which are likely more drained relative to others and how the planned completion of the child well can be improved. Lastly, this log can be useful is validating optimal well spacing in relatively new fields under development.

58 GEOSCIENCES↗

Analytical workflow dependence of experimental observables for uranium chemistries

In this work, we investigated how the sequencing of laboratory analytical methods used for chemical and morphological characterization influences analytical findings for particulate materials relevant to the nuclear fuel cycle, including UO2, U3O8, studtite (UO2O2·4H2O), and β-UO3, in the context of nuclear forensic analysis. Particles of each chemistry obtained from consistent production batches were exposed to Raman spectroscopy and scanning electron microscopy in varying orders to elucidate how the order in which the techniques are applied influences morphological and chemical observations as a function of particle size. The results indicate that particles from all four chemistries exposed to high-resolution electron imaging before Raman spectral analysis demonstrate optical vibrational spectral changes that reduce accurate interpretation of the underlying chemistry via Raman spectral analysis. We hypothesize that these changes are due to the thermal load of the electron beam imparted to the sample being unable to be dissipated by materials with poor thermal conduction properties. Results from this study will aid in determining best practices for forensic analysis procedures to reduce uncertainty in chemical determination of unknown particulate samples.

Manns, Rebecca [University of Nevada, Las Vegas]↗

The Distribution, Composition, and Particle Properties of Mars Mesospheric Aerosols: an Analysis of CRISM Visible/near-IR Limb Spectra with Context from Near-Coincident MCS and MARCI Observations

The Compact Reconnaissance Imaging Spectral Mapper (CRISM) onboard the Mars Reconnaissance Orbiter (MRO) obtains pole-to-pole observations (i.e., full MRO orbits) of vertical profiles for visible/near-IR spectra (λ=0.4–4.0 μm), which are ideally suited to identifying the composition and particle sizes of Mars ice and dust aerosols over 50–100 km altitudes in the Mars mesosphere. Within the coverage limitations of the CRISM limb data set, a distinct compositional dichotomy is found in Mars mesospheric ice aerosols. CO2 ice clouds appear during the aphelion period of Mars orbit (Solar Longitudes, Ls∼0–160°) at low latitudes (∼20S–10N) over specific longitude regions (Meridiani, Valles Marineris) and at typical altitudes of 55–75 km. Apart from faint water ice hazes below 55 km, mesospheric H2O ice clouds are primarily restricted to the perihelion orbital range (Ls∼160 – 350°) at northern and southern mid-to-low latitudes with less apparent longitudinal dependences. Mars mesospheric CO2 clouds are presented in CRISM spectra with a surprisingly large range of particle sizes (cross section weighted radii, Reff=0.3 to 2.2 μm). The smaller particle sizes (Reff ≤1 μm) appear concentrated near the spatial (latitude and altitude) boundaries of their global occurrences. CRISM spectra of mesospheric CO2 clouds also show evidence of iridescence, indicating very narrow particle size distributions (effective variance, Veff∼0.03) and so very abrupt CO2 cloud nucleation. Furthermore, these clouds are sometimes accompanied by altitude coincident peaks in 1.27 μm O2 dayglow, which indicates very dry, cold regions of formation. Mesospheric water ice clouds generally exhibit small particle sizes (Reff=0.1–0.3 μm), although larger particle sizes (Reff=0.4–0.7 μm) appear infrequently. On average, water ice cloud particle sizes decrease with altitude over 50–80 km in the perihelion mesosphere. Water ice mass appears similar in clouds over a large range of observed cloud particle sizes, with particle number densities increasing to ∼10 cm−3 for Reff=0.2 μm. Near coincident Mars Climate Sounder (MCS) temperature and aerosol profile measurements for a subset of CRISM mesospheric aerosol measurements indicate near saturation (H2O and CO2) conditions for ice clouds and distinct mesospheric temperature increases associated with mesospheric dust loading. Dayside (3 pm) mesospheric CO2 clouds with larger particle sizes (Reff ≥0.5 μm) scatter surface infrared emission in MCS limb infrared radiances, as well as solar irradiance in the MCS solar band channel. Scattering of surface infrared emission is most strikingly presented in nighttime (3 am) MCS observations at 55–60 km altitudes, indicating extensive mesospheric nighttime CO2 clouds with considerably larger particle sizes (Reff∼7 μm). Mesospheric CO2 ice clouds present cirrus-like waveforms over extensive latitude and longitude regions (10°×10°), as revealed in coincident Mars Color Imager (MARCI) nadir imaging. Solar tides, gravity waves, and the large orbital variation of the extended thermal structure of the Mars atmosphere influence all of these behaviors. Mesospheric dust aerosols appear infrequently over the non-global (planet encircling) dust storm era of the CRISM limb data set (2009–2016), and exhibit smaller particle sizes (Reff=0.2–0.7 μm) relative to dust in the lower atmosphere. One isolated case of an aphelion (Ls=96°) mesospheric dust layer with large dust particle sizes (Reff ∼2 μm) over Syria Planum may reflect high altitude, non-local transport of dust over elevated regions.

Clancy, Todd R.↗

The distribution, composition, and particle properties of Mars mesospheric aerosols: An analysis of CRISM visible/near-IR limb spectra with context from near-coincident MCS and MARCI observations

The Compact Reconnaissance Imaging Spectral Mapper (CRISM) onboard the Mars Reconnaissance Orbiter (MRO) obtains pole-to-pole observations (i.e., full MRO orbits) of vertical profiles for visible/near-IR spectra (λ= 0.4–4.0 μm), which are ideally suited to identifying the composition and particle sizes of Mars ice and dust aerosols over 50–100 km altitudes in the Mars mesosphere. Within the coverage limitations of the CRISM limb data set, a distinct compositional dichotomy is found in Mars mesospheric ice aerosols. CO2 ice clouds appear during the aphelion period of Mars orbit (Solar Longitudes, L(s )∼ 0–160°) at low latitudes (∼20S–10N) over specific longitude regions (Meridiani, Valles Marineris) and at typical altitudes of 55–75 km. Apart from faint water ice hazes below 55 km, mesospheric H2O ice clouds are primarily restricted to the perihelion orbital range (L(s)∼160 – 350°) at northern and southern mid-to-low latitudes with less apparent longitudinal dependences. Mars mesospheric CO2 clouds are presented in CRISM spectra with a surprisingly large range of particle sizes (cross section weighted radii, R(eff) = 0.3 to 2.2 μm). The smaller particle sizes (R(eff) ≤1 μm) appear concentrated near the spatial (latitude and altitude) boundaries of their global occurrences. CRISM spectra of mesospheric CO2 clouds also show evidence of iridescence, indicating very narrow particle size distributions (effective variance, V(eff) ∼ 0.03) and so very abrupt CO2 cloud nucleation. Furthermore, these clouds are sometimes accompanied by altitude coincident peaks in 1.27 μm O2 dayglow, which indicates very dry, cold regions of formation. Mesospheric water ice clouds generally exhibit small particle sizes (R(eff) = 0.1–0.3 μm), although larger particle sizes (R(eff) = 0.4–0.7 μm) appear infrequently. On average, water ice cloud particle sizes decrease with altitude over 50–80 km in the perihelion mesosphere. Water ice mass appears similar in clouds over a large range of observed cloud particle sizes, with particle number densities increasing to ∼10 per cu. cm for R(eff) = 0.2 μm. Near coincident Mars Climate Sounder (MCS) temperature and aerosol profile measurements for a subset of CRISM mesospheric aerosol measurements indicate near saturation (H2O and CO2) conditions for ice clouds and distinct mesospheric temperature increases associated with mesospheric dust loading. Dayside (3 pm) mesospheric CO2 clouds with larger particle sizes (R(eff) ≥0.5 μm) scatter surface infrared emission in MCS limb infrared radiances, as well as solar irradiance in the MCS solar band channel. Scattering of surface infrared emission is most strikingly presented in nighttime (3 am) MCS observations at 55–60 km altitudes, indicating extensive mesospheric nighttime CO2 clouds with considerably larger particle sizes (R(eff)∼7 μm). Mesospheric CO2 ice clouds present cirrus-like waveforms over extensive latitude and longitude regions (10°×10°), as revealed in coincident Mars Color Imager (MARCI) nadir imaging. Solar tides, gravity waves, and the large orbital variation of the extended thermal structure of the Mars atmosphere influence all of these behaviors. Mesospheric dust aerosols appear infrequently over the non-global (planet encircling) dust storm era of the CRISM limb data set (2009–2016), and exhibit smaller particle sizes (R(eff) = 0.2–0.7 μm) relative to dust in the lower atmosphere. One isolated case of an aphelion (L(s) = 96°) mesospheric dust layer with large dust particle sizes (R(eff) ∼2 μm) over Syria Planum may reflect high altitude, non-local transport of dust over elevated regions.

R. Todd Clancy↗

An Initial Analysis of the Pixel-Level Uncertainties in Global MODIS Cloud Optical Thickness and Effective Particle Size Retrievals

Moderate Resolution Imaging Spectroradiometer (MODIS) retrievals of cloud optical thickness and effective particle radius employ well-known solar reflectance techniques using pre-calculated reflectance look-up tables. We evaluate the quantitative uncertainty in simultaneous retrievals of cloud optical thickness and particle size for this type of algorithm. The technique uses sensitivity calculations derived from the reflectance look-up tables, coupled with estimates for the effect of various error terms on the uncertainty in inferring the actual cloud-top reflectance. The error terms include the effects of instrument calibration, surface spectral albedo, and atmospheric corrections on both water and ice cloud retrievals. Because particle shapes in ice clouds are highly variable, the effect of particle shape is analyzed separately with a more approximate method. Results will deal exclusively with pixel-level uncertainties associated with plane-parallel clouds; real-world radiative departures from a plane-parallel model are an additional consideration. While we demonstrate the uncertainty technique with operational 1 km MODIS retrievals from the Terra and Aqua satellite platforms, the technique is applicable to any reflectance-based satellite- or air-borne sensor retrieval using similar spectral channels.

Platnick, S.↗

The characterization of wear-causing particles and silica sand in particular

Erodants and abradants are two types of wear-causing particles (WCP). Despite their effects on the severity and rate of wear, WCP are inadequately characterized in a surprising number of publications, especially those involving impingement erosion and three-body abrasion. That shortfall makes it difficult to correlate features of WCP with the details of worn surfaces, or to develop wear models that account for those features. It is argued that the documentation of WCP should go beyond simply reporting their composition and mean particle size. In late 1985, ASTM Committee G2 on Wear and Erosion established a task group on the characterization of WCP. At that time, image analysis was slower and less sophisticated than it is today. While that ASTM task group failed to produce a consensus standard, computerized particle characterization methods were developing in fields other than tribology, fields like geoscience, heavy sand mining, materials processing, and pharmaceuticals. A notable exception to this is ferrography, which is a widely-used diagnostic for lubricated tribosystems. In the context of dry wear, it is useful to identify which features of WCP would be beneficial to document, and to identify some techniques and scales of detail appropriate to particular tribosystems. In this paper, examples are presented for the morphological and mechanical characterization of silica sand grains, as prompted by a triboanalysis of the abrasive and erosive wear of biomass pre-processing equipment. The authors propose a minimum level of documentation for WCP, one that can enrich tribosystem analysis both in laboratory tests and field studies.

36 MATERIALS SCIENCE↗

The influence of cooling rate on condensation of iron, aluminum, and uranium oxide nanoparticles

Fundamental observations of particle size distributions are needed to develop models that predict the fate and transport of radioactive materials in the atmosphere following a nuclear incident. The extent of material transport is influenced by the time scales of particle formation processes (e.g., condensation, coagulation). In this study, we investigated the influence of cooling time scales on size distributions of uranium, aluminum, and iron oxide particles that are synthesized separately under identical run conditions inside the controlled environment of an argon plasma flow reactor. Two distinct temperature distributions are imposed along the flow reactor by varying the argon flow rate downstream of the plasma torch. The vaporized reactants of uranium, aluminum, and iron are cooled from about 5000K to 1000K before they are collected on silicon wafers for ex situ scanning electron microscope analysis. The microscope images show that the sizes of the largest aluminum and iron oxide particles heavily depend on the cooling time scales, whereas significant size variation with cooling rate is not observed for uranium oxide particles. In addition, the size distribution of aluminum oxide particles exhibits the broadest range among all three metal oxides studied. We performed simulations of particle size distributions using a kinetic model that couples gas phase oxidation chemistry with particle formation processes, including nucleation, condensation, and coagulation. The model results demonstrate the strong sensitivity of particle size distribution to different cooling histories (i.e., temperature vs residence time) along the flow reactor. In conclusion, the kinetic model also helps identify directions for future research to improve the predictions.

36 MATERIALS SCIENCE↗

Examples of Optical Assessment of Surface Cleanliness of Genesis Samples

Optical microscope assessment of Genesis solar wind collector surfaces is a coordinated part of the effort to obtain an assessed clean subset of flown wafer material for the scientific community. Microscopic survey is typically done at 50X magnification at selected approximately 1 square millimeter areas on the fragment surface. This survey is performed each time a principle investigator (PI) returns a sample to JSC for documentation as part of the established cleaning plan. The cleaning plan encompasses sample handling and analysis by Genesis science team members, and optical survey is done at each step in the process. Sample surface cleaning is performed at JSC (ultrapure water [1] and UV ozone cleaning [2]) and experimentally by other science team members (acid etch [3], acetate replica peels [4], CO2 snow [5], etc.). The documentation of each cleaning method can potentially be assessed with optical observation utilizing Image Pro Plus software [6]. Differences in particle counts can be studied and discussed within analysis groups. Approximately 25 samples have been identified as part of the cleaning matrix effort to date.

Rodriquez, Melissa C.↗

RAPID: The imaging energetic particle spectrometer on Cluster

The RAPID spectrometer for the Cluster mission, an advanced particle detector for the analysis of suprathermal plasma distributions in the energy range from 20 to 400 keV and from 2 keV/nuc to 1500 keV for electrons and ions, respectively, is presented. Novel detector concepts in combination with pinhole acceptance permit the measurement of angular distributions over a range of 180 deg in polar angle for either species. The detection principle for the ionic component is based on a two dimensional analysis of a particle's velocity and energy. Electrons are identified by the well known energy range relationship. The detection techniques are described and selected areas in geospace are used to highlight the scientific objectives of this investigation.

Wilken, B.↗

Automated Track Recognition and Event Reconstruction in Nuclear Emulsion

The major advantages of nuclear emulsion for detecting charged particles are its submicron position resolution and sensitivity to minimum ionizing particles. These must be balanced, however, against the difficult manual microscope measurement by skilled observers required for the analysis. We have developed an automated system to acquire and analyze the microscope images from emulsion chambers. Each emulsion plate is analyzed independently, allowing coincidence techniques to be used in order to reject back- ground and estimate error rates. The system has been used to analyze a sample of high-multiplicity Pb-Pb interactions (charged particle multiplicities approx. 1100) produced by the 158 GeV/c per nucleon Pb-208 beam at CERN. Automatically reconstructed track lists agree with our best manual measurements to 3%. We describe the image analysis and track reconstruction techniques, and discuss the measurement and reconstruction uncertainties.

Deines-Jones, P.↗

Development of techniques for gantryless associated-particle imaging

To move fast-neutron radiography using the associated-particle imaging technique from the laboratory to the field, the development of new analysis techniques is required. In particular, the relative positions of the source and detectors need to be determined when they have been placed by hand, the normalization for a particular source–detector geometry needs to be determined without a measurement in the same geometry with no object present, and accurate image stitching is required when multiple detector positions are necessary to image an object. The present work describes methods that employ transmission neutron data to localize a fast-neutron imaging panel with respect to the neutron source, calculate a normalization for a given source–detector geometry, stitch images together, and describes the required system calibrations. The reported techniques enable in-field neutron radiography for cases in which the source–detector geometry is not well known a priori and where operational constraints preclude a normalization measurement.

Heath, Matthew↗

Ultra-Microtome for the Preparation of TEM Samples from Battery Cathodes

An ultra-microtome method is developed for the preparation of transmission electron microscopy (TEM) specimens from the cathodes of Li-ion battery. Results indicate that the samples prepared with the ultra-microtome method yield atomic resolution imaging from the core area of particles of hundreds to thousands of nanometers. Analysis of the TEM samples prepared with ultra-microtome indicates that no observable structural damage, such as microcracking, is introduced during the cutting process, and the cathodes cut by ultra-microtome exhibit unchanged micro-morphologies compared with the uncut ones. These results demonstrate that ultra-microtome is a promising method for the preparation of TEM specimens and revealing in-depth microstructures of fragile materials such as battery cathodes.

transmission electron microscopy, Sample Preparati↗

Impact of Controlled Storage Conditions on the Hydrolysis and Surface Morphology of Amorphous-UO 3

The hydration and morphological effects of amorphous (A)-UO 3 following storage under varying temperature and relative humidity have been investigated. This study provides valuable insight into U-oxide speciation following aging, the U-oxide quantitative morphological data set, and, overall, the characterization of nuclear material provenance. A-UO 3 was synthesized via the washed uranyl peroxide synthetic route and aged based on a 3-factor circumscribed central composite design of experiment. Target aging times include 2.57, 7.00, 14.0, 21.0, and 25.4 days, temperatures of 5.51, 15.0, 30.0, 45.0, and 54.5 °C, and relative humidities of 14.2, 30.0, 55.0, 80.0, and 95.8% were examined. Following aging, crystallographic changes were quantified via powder X-ray diffraction and an internal standard Rietveld refinement method was used to confirm the hydration of A-UO 3 to crystalline schoepite phases. The particle morphology from scanning electron microscopy images was quantified using both the Morphological Analysis of MAterials software and machine learning. Results from the machine learning were processed via agglomerative hierarchical clustering analysis to distinguish trends in morphological attributes from the aging study. Significantly hydrated samples were found to have a much larger, plate-like morphology in comparison to the unaged controls. Predictive modeling via a response surface methodology determined that while aging time, temperature, and relative humidity all have a quantifiable effect on A-UO 3 crystallographic and morphological changes, relative humidity has the most significant impact.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Detecting and characterizing special nuclear material for nuclear nonproliferation applications

Abstract There is an urgent need for new, better instrumentation and techniques for detecting and characterizing special nuclear material (SNM), i.e., highly enriched uranium and plutonium. The development of improved instruments and techniques requires experiments performed with the SNM itself, which is of limited availability. This paper describes the findings of experiments performed at the National Criticality Experiments Research Center conducted using new instruments and techniques on unclassified, kg-quantity SNM objects. These experiments, performed in the framework of the Department of Energy, National Nuclear Security Administration Consortium for Monitoring, Technology, and Verification, focused on detecting, characterizing, and localizing SNM samples with masses ranging from 3.3 to 13.8 kg, including plutonium and highly enriched uranium using prototype detectors and techniques. The work demonstrates SNM detection and characterization using recently-developed prototype detection systems. Specifically, we present new results in passive detection and imaging of plutonium and uranium objects using gamma-ray and dual particle (fast neutron and gamma-ray) imaging. We also present a new analysis of the delayed neutron emissions during active interrogation of uranium using a neutron generator.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

An approach for automated analysis of particle holograms

A simple method for analyzing droplet holograms is proposed that is readily adaptable to automation using modern image digitizers and analyzers for determination of the number, location, and size distributions of spherical or nearly spherical droplets. The method determines these parameters by finding the spatial location of best focus of the droplet images. With this location known, the particle size may be determined by direct measurement of image area in the focal plane. Particle velocity and trajectory may be determined by comparison of image locations at different instants in time. The method is tested by analyzing digitized images from a reconstructed in-line hologram, and the results show that the method is more accurate than a time-consuming plane-by-plane search for sharpest focus.

Stanton, A. C.↗

The Stardust: A Successful Encounter with the Remarkable Comet Wild 2

On January 2, 2004 the Stardust spacecraft completed a close flyby of comet Wild2 (P81). Flying at a relative speed of 6.1 km/s within 237km of the 5 km nucleus, the spacecraft took 72 close-in images, measured the flux of impacting particles and did in-situ compositional analysis of freshly released dust with a time-of-flight mass spectrometer. The primary goal of the mission is to collect >500 particles >15 m diameter and return them to Earth on January 15, 2006. The cometary particles ranging in size from a micron to approx.100 microns were collected in low density silica aerogel. After returning over a hundred 2x4x3 cm aerogel collection cells will be processed at the curatorial facility at the NASA Johnson Space Center and 5 to 100 micron size extracted cometary particles will be distributed to analysts by a system that will be based on the allocation procedures for cosmic dust, Antarctic meteorites and lunar samples.

Brownlee, D. E.↗

Using Image Pro Plus Software to Develop Particle Mapping on Genesis Solar Wind Collector Surfaces

The continued success of the Genesis mission science team in analyzing solar wind collector array samples is partially based on close collaboration of the JSC curation team with science team members who develop cleaning techniques and those who assess elemental cleanliness at the levels of detection. The goal of this collaboration is to develop a reservoir of solar wind collectors of known cleanliness to be available to investigators. The heart and driving force behind this effort is Genesis mission PI Don Burnett. While JSC contributes characterization, safe clean storage, and benign collector cleaning with ultrapure water (UPW) and UV ozone, Burnett has coordinated more exotic and rigorous cleaning which is contributed by science team members. He also coordinates cleanliness assessment requiring expertise and instruments not available in curation, such as XPS, TRXRF [1,2] and synchrotron TRXRF. JSC participates by optically documenting the particle distributions as cleaning steps progress. Thus, optical document supplements SEM imaging and analysis, and elemental assessment by TRXRF.

Rodriquez, Melissa C.↗