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At least 91 records · Page 5

INL CRMO XRF Report 2025-04: Provenance Determinations for 116 Obsidian Artifacts from Upper Snake U.S. Bureau of Reclamation Archaeological Collections

This report presents provenance determinations for 116 obsidian artifacts from Upper Snake U.S. Bureau of Reclamation collections. Provenance determinations were made using energy dispersive X-ray fluorescence (ED-XRF) spectrometry at the Idaho National Laboratory (INL) Cultural Resource Management Office (CRMO) under the direction of Dr. Kyle Freund.

99 - GENERAL AND MISCELLANEOUS↗

INL CRMO XRF Report 2025-05: Provenance Determinations for 23 Folsom and Midland Projectile Points from Eastern Idaho

This report presents provenance determinations for 23 obsidian and fine-grained volcanic Folsom and Midland projectile points from eastern Idaho. Provenance determinations were made using energy dispersive X-ray fluorescence (ED-XRF) spectrometry at the Idaho National Laboratory (INL) Cultural Resource Management Office (CRMO) under the direction of Dr. Kyle Freund.

58 GEOSCIENCES↗

INL CRMO XRF Report 2025-03: Provenance Determinations for 854 Projectile Points from Idaho Falls District Bureau of Land Management Archaeological Collections

This report presents provenance determinations for 854 obsidian and fine-grained volcanic projectile points from Idaho Falls District Bureau of Land Management collections. Provenance determinations were made using energy dispersive X-ray fluorescence (ED-XRF) spectrometry at the Idaho National Laboratory (INL) Cultural Resource Management Office (CRMO) under the direction of Dr. Kyle Freund.

99 - GENERAL AND MISCELLANEOUS↗

INL CRMO XRF Report 2025-06: Provenance Determinations for 246 Obsidian and Fine-grained Volcanic Artifacts from Folsom-era Sites in Eastern Idaho

This report presents provenance determinations for 246 obsidian and fine-grained volcanic artifacts from Folsom-era sites in eastern Idaho. Provenance determinations were made using energy dispersive X-ray fluorescence (ED-XRF) spectrometry at the Idaho National Laboratory (INL) Cultural Resource Management Office (CRMO) under the direction of Dr. Kyle Freund.

58 GEOSCIENCES↗

INL CRMO XRF Report 2025-02: Provenance Determinations for 1,124 Projectile Points from Lands and Collections Managed by the U.S. Department of Energy-Idaho Operations Office (DOE-ID)

This report presents provenance determinations for 1,124 obsidian and fine-grained volcanic (FGV) projectile points from lands and collections managed by the U.S. Department of Energy-Idaho Operations Office (DOE-ID). These determinations were made using energy-dispersive X-ray fluorescence (ED-XRF) spectrometry at the Idaho National Laboratory (INL) Cultural Resource Management Office (CRMO) under the direction of Dr. Kyle Freund.

58 GEOSCIENCES↗

Spatially resolved nanostructural analysis of disordered phases in carbonated alkali-activated slag

Alkali-activated slag (AAS) is a promising low-CO 2 alternative cement consisting of several disordered phases of similar composition. Although their local atomic arrangements are known to influence macroscopic behavior, determination of structural changes in response to external stimuli remains a challenge. Here, X-ray diffraction-computed tomography (XRD-CT), pair distribution function-CT (PDF-CT), and nanoprobe X-ray fluorescence (nano-XRF) have been used to uncover how an increase of magnesium in AAS affects the atomic structure and spatial arrangement of phases after aggressive carbonation (100% dry CO 2 ), conditions experienced in applications such as oil and gas wells and geological storage of CO 2 . From PDF-CT it is found that a higher magnesium content decreases the average nanoscale crystallite size of disordered calcium carbonate. At the same time, higher magnesium content is correlated with a less decalcified C-(N)-A-S-H gel, as determined via analysis of Ca-Si atom-atom correlations from PDF-CT and Ca/Si ratios from nano-XRF. Finally, nano-XRF reveals that the disordered (i.e., amorphous) calcium carbonate is stabilized by the presence of silicates.

McCaslin, Eric R. [Princeton Univ., NJ (United Sta↗

Effect of glutathione-coated Mn-doped ZnS quantum dots on nutrient delivery in basil ( Ocimum basilicum ) plants

Ensuring efficient nutrient delivery while minimizing environmental impacts remains a significant challenge for modern agriculture. Nanotechnology-based fertilizers offer promising strategies to improve nutrient uptake and bioavailability in plants. This research aims to evaluate the use of Glutathione-coated Manganese-doped Zinc Sulfide quantum dots (GSH-ZnS-Mn QDs) as a potential nano fertilizer for basil (Ocimum basilicum). QDs' physicochemical properties were characterized using UV–Vis spectroscopy, photoluminescence, FTIR, and energy-dispersive X-ray spectroscopy, confirming successful Mn doping and glutathione surface functionalization. Basil plants were exposed to different concentrations of GSH-ZnS-Mn QDs under soil and hydroponic conditions. Plant growth parameters, oxidative stress responses, photosynthetic pigments, and macro- and micronutrient uptake were assessed using biochemical assays and inductively coupled plasma optical emission spectrometry (ICP-OES). Elemental uptake, spatial distribution, and zinc speciation were further investigated using synchrotron-based micro-X-ray fluorescence (μ-XRF) imaging and X-ray absorption near-edge structure (XANES) spectroscopy. Results show that exposure to GSH-ZnS-Mn QDs resulted in a concentration-dependent increase in leaf and stem biomass, accompanied by enhanced Zn accumulation in plant tissues. Catalase activity decreased across all tested concentrations, suggesting a shift toward glutathione-dependent antioxidant pathways rather than oxidative damage. Chlorophyll levels exhibited moderate reductions at higher concentrations. The higher increase in macronutrient (K, Ca, and Mg) uptake was reported in plants exposed to 200 ppm of QDs. μ-XRF imaging indicated a selective accumulation of Zn in roots and stems, with partial translocation to leaves. XANES analyses revealed that Zn from QDs was mainly converted into organic Zn species, such as Zn-phytate, Zn-acetate, and Zn-cysteine, indicating transformation and complexation within the plant. The findings demonstrate that a glutathione coating on GSH-ZnS-Mn QDs improves biocompatibility and nutrient delivery efficiency. These results highlight the relevance of surface functionalization in regulating nanoparticle fate, transformation, and nutrient bioavailability, supporting the potential application of GSH–ZnS–Mn QDs as modern nano fertilizers.

Basil↗

Strategies and Technologies for In Situ Mineralogical Investigations on Mars

Surface landers on Mars (Viking and Pathfinder) have not revealed satisfying answers to the mineralogy and lithology of the planet's surface. In part, this results from their prime directives: Viking focused on exobiology, Pathfinder focused on technology demonstration. The analytical instruments on board the landers made admirable attempts to extract the mineralogy and geology of Mars, as did countless modeling efforts after the missions. Here we suggest a framework for elucidating martian, or any other planetary geology, through an approach that defines (a) type of information required, (b) explorational strategy harmonious with acquisition of these data, (c) interpretation approach to the data, (d) compatible mission architecture, (e) instrumentation for interrogating rocks and soil. (a) Data required: The composition of a planet is ordered at scales ranging from molecules to minerals to rocks, and from geological units to provinces to planetary-scale systems. The largest ordering that in situ compositional instruments can attempt to interrogate is rock type "aggregate" information. This is what the geologist attempts to identify first. From this, mineralogy can be either directly seen or inferred. From mineralogy can be determined elemental abundances and perhaps the state of the compounds as being crystalline or amorphous. Knowledge of rock type and mineralogy is critical for elucidating geologic process. Mars landers acquired extremely valuable elemental data, but attempted to move from elements to aggregates, but this can only be done by making many assumptions and sometimes giant leaps of faith. Data we believe essential are elements, minerals, degree of ordering of compounds, and the aggregate or rock type that these materials compose. (b) Explorational strategy: A lander should function as a surrogate geologist. Of the total landscape, a geologist sees much, but gives detailed attention to an infinitesimally small amount of what is seen. To acquire samples worth detailed scrutiny, as many samples as possible need examining at a cursory or reconnaissance level. A representative, statistically-meaningful sample number cannot be overemphasized. This maxim still applies to geological exploration of our own planet of which we have abundant knowledge. Analysis of many samples mandates low-power consumption per sample. (c) Data interpretation: No single instrument can analyze the full spectrum of the x-axis. An instrument is optimized for detecting certain material characteristics and must therefore affix itself to some point on the x-axis. Any conclusions drawn about data to the left or right of the instrument's position on this axis must necessarily be derived by inference. Hence, it seems logical to include on a mission, instruments that are not closely spaced in their x-axis-position, and if only two analytical methods are used, as shown, they should start at opposite ends of the axis and work towards the center. As examples, we depict a high-resolution camera to evaluate rock type ("aggregate" state) and mineralogy, and an x-ray diffractometer-fluorescence spectrometer (XRD-XRF) to determine elements, minerals, and the degree of order of materials. (d) Mission architecture: No instrument or suite of instruments can be relied upon to always give truly unequivocal analyses. The suite of instruments should therefore permit conclusions of one instrument to be checked against those of another through closed analytical loops. These "loops" can be structured by a combination of orbital imagery, descent imagery, broad-band site viewing/analysis, and data that cover both x and y axes. For example, the detection of a basaltic-looking rock with a microscope should be checked against the elements detected, the appearance of the rock as a lava flow from descent imagery, and so forth. (e) Instrumentation: To satisfy the above criteria, it is necessary to: (i) See the rock or soil with high resolution + magnification, (ii) Examine many samples, (iii) Consume little power per analysis, (iv) Determine elemental species, (v) Determine mineralogy directly (not inferentially) and the degree of ordering of compounds, (vi) Start analyzing from both ends of the x-axis. Every geologist wants to see the hand sample first, and apply a hand lens to its surface. This has not been the starting point for missions to Mars. Thus, our technology satisfies all these criteria . This XRD-XRF-Optical instrument currently being developed, analyses rock or soil surfaces without the need for sample acquisition or preparation; this satisfies the power criterion, and enables many analyses. The device acquires direct mineralogy and determines elemental species. The embedded endoscopic camera satisfies the critical criterion of close inspection of samples; the fiber optic cable can also be used for IR, LTV, or laser sample analysis. Additional information is contained in the original (Figures).

Marshall, J. R.↗

Utilization of independent solar flux measurements to eliminate nongeochemical variation in X-ray fluorescence data

It is shown that the direct method of solar activity correction for lunar XRF data produces XRF data with better statistics than uncorrected data. Direct measurements of the solar flux made by Solrad 10 are converted to emissions of the sun from two assumed temperature regions. These emissions are ratioed to produce emission measure ratios, sensitive indicators of shifts in solar activity. The Tucker-Koren model (1971) of the solar flux is used in the calculation of EMRs and in the calculation of theoretical lunar Si, Al, and Mg fluorescence of maria and highland soils. Al/Si(Mg/Si) ratios calculated at a 'normal' EMR of 0.030 are divided by Al/Si(Mg/Si) ratios at particular EMRs. The relationship between EMR and the quotients of this division, called 'correction factors', is well explained by empirically derived power law functions.

Clark, P. E.↗

A new color correlation method applied to XRF Al/Si ratios and other lunar remote sensing data

Orbital X-ray fluorescence Al/Si intensity ratios, corrected for variations in solar activity, are correlated with normal albedo, elevation measurements from laser altimetry data, and gamma ray data in the 2.75-8.60 MeV range. Each of these data sets is placed into a digital array consisting of 1/4 deg latitude by 1/4 deg longitude pixels. Information relative to the correlation of Al/Si ratios with each of the other data sets is presented in the following forms: (1) histograms are given for each data set to show the frequency distribution within the areas of common coverage; (2) density plots are produced from the plot of a two-dimensional array consisting of the Al/Si ratio vs the other parameter value for each pixel; and (3) color correlation maps are produced by placing the two-dimensional array into a 3 x 3 matrix consisting of nine equal subarrays containing an equal number of data points.

Clark, P. E.↗

X-ray fluorescence analysis of alloy and stainless steels using a mercuric iodide detector

A mercuric iodide detector was used for the XRF analysis of a number of NBS standard steels, applying a specially developed correction method for interelemental effects. It is shown that, using this method and a good peak-deconvolution technique, the HgI2 detector is capable of achieving resolutions and count rates needed in the XRF anlysis of multielement samples. The freedom from cryogenic cooling and from power supplies necessary for an electrically cooled device makes this detector a very good candidate for a portable instrument.

Kelliher, Warren C.↗

Methods for identification and verification using vacuum XRF system

Apparatus and methods in which one or more elemental taggants that are intrinsically located in an object are detected by x-ray fluorescence analysis under vacuum conditions to identify or verify the object's elemental content for elements with lower atomic numbers. By using x-ray fluorescence analysis, the apparatus and methods of the invention are simple and easy to use, as well as provide detection by a non line-of-sight method to establish the origin of objects, as well as their point of manufacture, authenticity, verification, security, and the presence of impurities. The invention is extremely advantageous because it provides the capability to measure lower atomic number elements in the field with a portable instrument.

Schramm, Fred↗

Molecular and Elemental Dust Analyzer (MEDA) for the comet rendezvous asteroid flyby mission

Comets are some to the most primitive bodies in the solar system and therefore should contain elemental, chemical, and isotopic records of the early history of the solar system. An opportunity to perform in situ analyses of a comet nucleus exists with the Comet Rendezvous Asteroid Flyby (CRAF) mission. An integrated gas chromatograph/X-ray fluorescence instrument (MEDA), being proposed for inclusion onboard the CRAF spacecraft, will measure the molecular and elemental constituents of collected dust grains and ices. The gas chromatograph, employing helium ionization detectors and three columns designed to separate light gases, polar gases, and hydrocarbons will measure the volatile compounds of the biogenic elements thermally released from collected dust grains. The sensitivity of the GC for compounds of interest is at the picogram level. X-ray fluorescence utilized cryogenically cooled Si(Li) solid state detectors of nominal 150 eV resolution at 5.9 keV. Based on laboratory work with carbonaceous meteorites, both the GC and XRF can perform meaningful analyses with a few micrograms of collected comet dust.

Ohara, B. J.↗

INL CRMO XRF Special Report No. 3: INL CRMO XRF Calibration Methods for the Analysis of Ceramics and Brick

This report details the analytical methods used by the Idaho National Laboratory Cultural Resource Management Office to characterize ceramic and brick artifacts using X-ray fluorescence spectrometry. More specifically, this report provides details on instrumentation, analysis times, and matrix-specific calibration protocols for ceramic materials. Calibration curves were developed to adjust raw instrumental output for 13 elements using a suite of reference standards made from historic brick borrowed from the Yale Peabody Museum. Calibration curves were validated by plotting predicted values against published reference values for the calibration set as well as a certified soil reference standard (SRM 2711a).

36 MATERIALS SCIENCE↗

Elemental composition of the Martian surface

The Viking landers carried X-ray fluorescence spectrometers (XRFS) to the surface of Mars for direct in-situ measurements of the elemental composition of samples that could be acquired by the surface sampler scoops. A total of 21 samples at two landing sites were acquired and analyzed. In this review, the constraints imposed on the design and operation of the XRFS; the accuracy and precision limitations of XRF; and the interpretation of the results are discussed. The latter includes relevance of the investigation to Martian geological processes, SNC meteorites, the formation and history of Mars, and future mission objectives/capabilities.

Clark, Benton C.↗

CHEMIN: A Mineralogical Dust Analyzer for the Odyssey Mission to Comet Kopff

The Odyssey spacecraft will be launched in June 2006 and will rendezvous with periodic Comet Kopff in September 2009. Odyssey will initially perform slow flybys of the active Kopff nucleus at distances between 500 and 100 km, and will then be placed in orbit around the nucleus at altitudes between 200 and 50 km. Odyssey's scientific payload of seven instruments includes CHEMIN, a mineralogical dust analyzer, which will make the first direct measurements of the crystal structure and elemental composition of cometary dust. CHEMIN will simultaneously perform X-ray Diffraction and X-ray Fluorescence (XRD/XRF) of individual 1-100 micron dust particles collected passively as the spacecraft is immersed in the comet's coma. The instrument has the geometry of a microfocus X-ray camera, with a postage stamp-sized energy-discriminating CCD in place of the film, and a miniature Cu target X-ray tube as the X-ray source. The CHEMIN flight instrument will weigh less than 2 kg., will have a total volume of about 1 liter, and will operate on 3 watts of power. Individual analyses will require 1-2 hours. XRD maxima from 5 to 65 degrees two-theta will be collected, encompassing definitive peaks for all known minerals. XRF data will be simultaneously collected for elements C through U. The instrument has sufficient resolution to allow Rietveld refinement of the diffraction data. Rock types as complex as basalt have been quantitatively analyzed using a CHEMIN laboratory prototype. Selected examples of diffraction experiments performed on more than 30 minerals and rock types by the CHEMIN laboratory prototype will be discussed.

Blake, David↗

Probing the Mechanism of Selective Phosphate Adsorption from Wastewater Using Aqueous and Synchrotron X-ray Characterization

Ion exchange shows promise for recovering phosphate from wastewater as value-added products, but requires high phosphate selectivity to compete with conventional treatment. Hybrid anion exchange (HAIX) resins, which contain non-selective basic functional groups and selective iron oxide nanoparticles (FeOnp), can effectively remove phosphate from wastewater. However, knowledge gaps remain regarding the mechanisms of phosphate selectivity and influence of competing ions, hindering needed efforts to model adsorption dynamics and design scalable adsorption processes for varying wastewaters. To address these gaps, we integrated aqueous-phase adsorption analysis with solid-phase, synchrotron-based X-ray characterization; this integration facilitated elucidation of the distribution and speciation of iron, phosphate, and competing anions on HAIX resins. We compared a quaternary ammonium-functionalized HAIX resin (SBA) to a tertiary amine version (WBA) to determine the role of functional groups. X-ray radiography revealed differences in FeOnp speciation (goethite vs. ferrihydrite) and distribution (peripheral vs. homogeneous) between the resins, resulting in varied phosphate affinity and intraparticle diffusion resistance. Using micro-X-ray fluorescence (μ-XRF) and micro-X-ray absorption near-edge structure (μ-XANES) spectroscopy, we identified differences in where and how phosphate binds across resin types and wastewaters. Across wastewater compositions, FeOnp sites in WBA contribute more to phosphate adsorption than in SBA, possibly due to variations in Fe distribution and speciation. Phosphate adsorption densities calculated from quantitative μ-XRF maps matched those from aqueous analysis, demonstrating the effectiveness of this integrated approach. Altogether, results demonstrate the use of synchrotron-based X-ray characterization for investigating adsorption mechanisms and advance HAIX as a phosphate recovery technology from complex wastewaters.

Nutrient recovery↗

Combined Backscatter Moessbauer Spectrometer and X Ray Fluorescence analyzer (BaMS/XRF) for planetary surface materials

A backscatter Moessbauer spectrometer (BaMS) with included x ray fluorescence (XRF) capability for the Mars Environment Survey (MESUR) Mission, which has been proposed by NASA for 1998, is being developed. The instrument will also be suitable for other planetary missions such as those to the Moon, asteroids, and other solid solar-system objects. The BaMS would be unique for MESUR in providing information about iron mineralogy in rocks, clays, and other surface materials, including relative proportions of iron-bearing minerals. It requires no sample preparation and can identify all the normal oxidation states of iron (3+, 2+, 0). Thus, BaMS is diagnostic for weathering and other soil-forming processes. Backscatter design allows the addition of XRF elemental analysis with little or no modification. The BaMS/XRF instrument complements the thermal analyzer with evolved gas analyzer (TA-EGA) and the alpha-proton x-ray spectrometer (APXS) proposed (along with BaMS) for geochemical analysis on MESUR.

Agresti, D. G.↗