Analysis of background residential dust for World Trade Center signature components using scanning electron microscopy and x-ray microanalysis
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Examination of Libby, Montana, Fill Material for Background Levels of Amphibole from the Rainy Creek Complex Using Scanning Electron Microscopy and X-Ray Microanalysis
Natural background levels of Libby-type amphibole in the sediment of the Libby valley in Montana have not, up to this point, been determined. The purpose of this report is to provide the preliminary findings of a study designed by both the U.S. Geological Survey and the U.S. Environmental Protection Agency and performed by the U.S. Geological Survey. The study worked to constrain the natural background levels of fibrous amphiboles potentially derived from the nearby Rainy Creek Complex. The material selected for this study was sampled from three localities, two of which are active open-pit sand and gravel mines. Seventy samples were collected in total and examined using a scanning electron microscope equipped with an energy dispersive x-ray spectrometer. All samples contained varying amounts of feldspars, ilmenite, magnetite, quartz, clay minerals, pyroxene minerals, and non-fibrous amphiboles such as tremolite, actinolite, and magnesiohornblende. Of the 70 samples collected, only three had detectable levels of fibrous amphiboles compatible with those found in the rainy creek complex. The maximum concentration, identified here, of the amphiboles potentially from the Rainy Creek Complex is 0.083 percent by weight.
Open-File Report↗
Microstructure and crystallographic preferred orientation of polycrystalline microgarnet aggregates developed during progressive creep, recovery, and grain boundary sliding
Optical microscopy, electron probe microanalysis, and electron backscatter diffraction methods have been used to examine a broad range of garnet microstructures within a high strain zone that marks the western margin of a major transpression zone in the southern New England Appalachians. Garnet accommodated variable states of finite strain, expressed as low strain porphyroclasts (Type 1), high strain polycrystalline aggregates (Type 2), and transitional morphologies (Type 3) that range between these end members. Type 1 behaved as rigid porphyroclasts and is characterized by four concentric Ca growth zones. Type 2 help define foliation and lineation, are characterized by three Ca zones, and possess a consistent bulk crystallographic preferred orientation of (100) symmetrical to the tectonic fabric. Type 3 show variable degrees of porphyroclast associated with aggregate, where porphyroclasts display complex compositional zoning that corresponds to lattice distortion, low-angle boundaries, and subgrains, and aggregate CPO mimics porphyroclast orientation. All aggregates accommodated a significant proportion of greenschist facies deformation through grain boundary sliding, grain rotation and impingement, and pressure solution, which lead to a cohesive behavior and overall strain hardening of the aggregates. The characteristic CPO could not have been developed in this manner, and was the result of an older phase of partitioned amphibolite facies dislocation creep, recovery including chemical segregation, and recrystallization of porphyroclasts. This study demonstrates the significance of strain accommodation within garnet and its affect on composition under a range of PT conditions, and emphasizes the importance of utilizing EBSD methods with studies that rely upon a sound understanding of garnet. ?? 2010 Elsevier Ltd.
Journal of Structural Geology↗
Transitioning laser ablation ICP-MS from research applications to routine trace element microanalysis: A look at quantitative trace element analyses and imaging
[No abstract available]
Microscopy and Microanalysis↗
Compositional and structural mapping of Northwest Africa 15507 angrite
Angrite meteorites represent interesting sampling of planetary crustal environments. Quench-textured angrites with strong crystal zoning originated from the shallow surface region, with evidence of reducing conditions during solidification. Plutonic angrites have more coarse-grained igneous and metamorphic textures with comparatively less zoning and are interpreted as having equilibrated at greater depth. Plutonic angrites contain the minerals magnetite Fe 3 O 4 comprised of Fe 2+ and Fe 3+ , and rhönite, where Fe 3+ is required by inspection of mineral stoichiometry. NWA 15507 is a plutonic angrite with a microgabbroic texture (mean grainsize ∼1.4 mm) composed of zoned Al-Ti-augite, Ca-bearing olivine, anorthite, with accessory kirschsteinite, rhönite, hercynite, low-Ni kamacite, merrillite, Ti-free magnetite and troilite [ 1 ]. Rhönite analyzed by electron-probe microanalysis (EPMA) has the formula Ca 2.04 (Mg 0.32 Fe 2+ 4.25 Fe 3+ 0.47 Ti 0.33 Al 0.61 )(Si 3.74 Al 2.26 )O 20 , where Fe 3+ was estimated by stoichiometric analysis. During preliminary cathodoluminescence (CL) analysis, complex subgrain and oscillatory zoning was observed in the anorthite. In this study we use a combined approach of electron probe microanalysis (EPMA), cathodoluminescence (CL), electron-backscatter diffraction (EBSD), and laser ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS) to further investigate the anorthite and distribution of Fe 3+ in NWA 15507.
Microscopy and Microanalysis↗
Mineralogy of mine waste at the Vermont Asbestos Group mine, Belvidere Mountain, Vermont
Samples from the surfaces of waste piles at the Vermont Asbestos Group mine in northern Vermont were studied to determine their mineralogy, particularly the presence and morphology of amphiboles. Analyses included powder X-ray diffraction (XRD), optical microscopy, scanning electron microscopy (SEM), electron probe microanalysis (EPMA), and Raman spectroscopy. Minerals identified by XRD were serpentine-group minerals, magnetite, chlorite, quartz, olivine, pyroxene, and brucite; locally, mica and carbonates were also present. Raman spectroscopy distinguished antigorite and chrysotile, which could not be differentiated using XRD. Long-count, short-range XRD scans of the (110) amphibole peak showed trace amounts of amphibole in most samples. Examination of amphiboles in tailings by optical microscopy, SEM, and EPMA revealed non-fibrous amphiboles compositionally classified as edenite, magnesiohornblende, magnesiokatophorite, and pargasite. No fibrous amphibole was found in the tailings, although fibrous tremolite was identified in a sample of host rock. Knowledge of the mineralogy at the site may lead to better understanding of potential implications for human health and aid in designing a remediation plan.
American Mineralogist↗
Not-so-routine electron probe microanalyses of jarosite
No abstract available.
Microscopy and Microanalysis↗
Approach for quantifying rare Earth elements at low keV
The challenges of analyzing bastnaesite (REECO3F) and hydroxylbastnaesite (REECO3OH) include beam sensitivity, quantification of light elements in a heavy element matrix, the presence of elements that cannot be analyzed with EPMA (H), and the use of x-ray lines whose physical constants are not well known. To overcome some of these challenges, Ca, La, Ce, Pr, Nd, and Sm were analyzed at 15 keV accelerating voltage and the light elements (C, O, F) were analyzed at 7 keV accelerating voltage. This approach is ideal for samples that are homogeneous within the volume analyzed. However, for the bastnaesite of interest, this solution is unsatisfactory as backscattered electron imaging reveals chemical variations at scales of less than 1 m (fig. 1). Monte Carlo simulations and wavescans of the REE M family of x-rays were evaluated to determine the best analytical approach. Monte Carlo simulations using Casino v2.42 were ran on a substrate of CeCO3F with a density of 5.00 g/cm3 at 15 keV and 7 kCV accelerating voltage. Depth distribution curves, φ(ρz), reveal x-ray generation at 15 keV for the Ce L shell x-rays approaches 1.0 m whereas the depth of Ce M shell x-ray generation at 7 keV is less than 0.4 m. Similarly, the K shell x-ray generation depth for C, O, and F at 7 keV is also less than 0.4 m. These simulations demonstrate an accelerating voltage of 7 keV or less and use of the REE M x-rays is necessary to acquire chemical information from the same volume of material for the light and heavy elements. Bastnaesite contains all REE and therefore one must consider the energy of the highest x-ray line of interest, namely the Lu M at 1.83 kV, to achieve an overvoltage (Eo/Ec) of over 2. Bastnaesite is also an insulator and requires a conductive coating, therefore 7 keV was used to avoid contributions of the coating material to the analysis given the above constraints. The USNM REE phosphate standards, Edinburgh REE glasses, CeO2, LaB6, and the metals of Sm, Dy, Gd, Er, and Yb were selected to evaluate the peak overlaps of the M family x-ray lines. The materials were coated with ~ 5nm iridium with a Leica ACE600 prior to analysis. Full spectrometer wavescans were collected at 7 keV accelerating voltage, 50 nA beam current, and 20 um beam diameter on a JEOL 8530F Plus using TAP and TAPL crystals. The step size was 0.109 mm along the length of the spectrometer with a dwell of 3 seconds at each step. M and M lines are broad and not individually resolved for the light REE but become more separated and sharper with increasing atomic number. M and M lines for each REE are also present across the spectrometer range further complicating peak interference corrections. The peak positions and overall shape for the Ce M and M lines vary with the coordination of the element. Significant shifts in position and shape were not observed when comparing the Ce M peaks of CeO2 and CePO4. Similar results were seen when comparing the available REE metal to the phosphate (Sm, Dy, Gd, Er, Yb). These wavescans suggest the use of the M or M lines if matrix matched standards are not available.
Microscopy and Microanalysis↗
Correlating quantified cathodoluminescence spectra in jadeite with micro-scale color measurements in visible-near infrared reflectance spectrometry
Cultures throughout history have valued jadeite jade (hereinafter jade), a natural material assemblage composed predominately of the NaAl endmember pyroxene, jadeite (NaAlSi 2 O 6 ) that is prized for its mechanical properties and enticing coloration [ 1 , 2 ]. The geological setting for the formation of jadeite-rich rocks and associated complex geochemical phenomena is well documented in the literature [ 3-5 ]. Unlike single crystal gems, jade often contains a mixture of colors, but the stone is perhaps best known for exhibiting a range of green hues from pale green to blue green, and to deep green [ 1 , 6 ]. Efforts to classify jade color include qualitative matching to a set of reference color tiles, and less commonly, use of a more quantitative set of color perception values first established by International Commission on Illumination’s (CIE 1931) color space, which includes values for light-dark luminance level (L*), a green-red vector (a*), and a blue-yellow vector (b*) [ 7 , 8 ]. Two principal mechanisms have been identified as the cause of green coloration in jadeite: 1) the chemical state of impurity Fe, either 2+ or 3+, and 2) minor to trace Cr in the crystal structure [ 9 , 10 ]. Previous studies have associated Cr 3+ with cathodoluminescence (CL) spectral features in jadeite using point spectrometry, with more recent connections made via 2D CL spectrum imaging [ 11-13 ]. In this effort, we are seeking to establish whether Cr impurities are correlated with green coloration in jadeite using micro-scale (≤110 μm) visible-near infrared (VIS-NIR) reflectance spectrometry.
Microscopy and Microanalysis↗
Cathodoluminescence imaging and spectrometry of a jadeite microbeam reference crystal: Detection of Ce3+
Options for selecting a high Na concentration mineral for instrument calibration that are suitably stable under the electron beam are limited [ 1 ]. NaCl (approximately a mass fraction of 39 % Na) is not practical for use alongside other embedded and polished materials in a mounted block of standards. While albite (NaAlSi 3 O 8 ; approximately a mass fraction of 8 % Na) represents a typical choice for some microanalysts, it may be subject to time dependent signal intensity issues, such as those observed for Na and other cations during analysis of hydrous glasses [ 2 ]. Near endmember jadeite pyroxene (NaAlSi 2 O 6 ; approximately mass fraction of 11 % Na) represents a desirable option for calibration given its relatively large concentration of Na and insensitivity to electron beam radiation with respect to X-ray output. Despite these desirable characteristics, jadeites have been shown to contain complex microstructures as the result of intracrystalline zoning [ 3 , 4 ], and the impact of chemical inhomogeneity within mineral standards and natural glasses has been documented [ 5-7 ]. In this study, a commercially obtained jadeite crystal (source location “China”) was studied to assess its microscale uniformity using a suite of microbeam methods, including dispersive red-green-blue multispectral cathodoluminescence imaging (CL RGB ), hyperspectral CL imaging spectrometry, energy dispersive X-ray spectrometry (EDS), SEM-based micro-X-ray fluorescence (μXRF), and wavelength dispersive X-ray spectrometry (WDS).
Microscopy and Microanalysis↗
Complex carbonate ore mineralogy in the Mountain Pass carbonatite rare earth element deposit, USA
Economic concentrations of rare earth element (REE) minerals are uncommon in the Earth’s crust, with most occurring in carbonatites. Unlike most igneous rocks composed of silicate minerals, carbonatites are dominated by carbonate minerals, some of which can incorporate significant light REEs (LREEs; La, Ce, Pr, Nd). Technological applications of REEs are numerous and they have been identified as some of the most critical mineral commodities to the global economy. The Mountain Pass carbonatite stock in the Mojave Desert of California is the most economically significant REE deposit in the USA and contains a few to tens of percent (by volume) of the carbonate REE ore mineral bastnäsite. Despite the economic significance of the Mountain Pass deposit, studies of its ore mineralogy are limited. Here we present new carbonate ore mineralogy data for a compositionally diverse suite of carbonatitic rocks from the Mountain Pass stock and related dikes. Whole-rock geochemical data are integrated with mineral-scale textural and chemical data obtained by scanning electron microscopy (SEM), electron probe microanalysis (EPMA), and microRaman spectroscopy. Our results document a complex spectrum of REE-bearing carbonate minerals and intermediate mixed-layer structures. Mineral species include bastnäsite [REE(CO 3 )F], hydroxylbastnäsite [REE(CO 3 )OH], parisite [Ca(REE) 2 (CO 3 ) 3 F 2 ], synchysite [Ca(REE)(CO 3 ) 2 F], röntgenite [Ca 2 (Ce,La) 3 (CO 3 ) 5 F 3 ], and sahamalite [(Mg,Fe 2+ )(REE) 2 (CO 3 ) 4 ]. Carbonate ore mineralogy is heterogeneous within and between samples, including at the intracrystal scale. Complexly zoned crystals exhibit as many as five to six different compositional domains and syntaxial intergrowths, commonly with the more Ca-rich varieties (parisite, synchysite) forming crystal rims that surround relict bastnäsite cores. We attribute the phenocryst variability to changes in the chemistry and temperature of primary carbonatite magmas and evolved/exsolved fluids. Cross-cutting vein textures of calcite, celestine and various REE carbonate minerals, interstitial bastnäsite crystallization, breccia blocks lined by fine-grained bastnäsite, and the presence of hydroxylbastnäsite and partially hydroxylated bastnäsite point to the role of secondary hydrothermal processes in REE mineralization. Fluorcarbonate mineral compositions demonstrate that La and Ce are more structurally abundant in bastnäsite, whereas the more Ca-rich species (parisite, synchysite) contain a greater proportion of REE heavier than Pr (Nd, Sm, Eu, Gd) and Y. Atomic ratios of Pr/(Nd + Pr) are likewise variable, with the highest average value for bastnäsite (0.25) compared to parisite (0.22) and sychysite (0.21). This finding has geometallurgical implications, given that current mining operations are focused on recovery of Nd and Pr for high field strength permanent magnets and the Nd/Pr ratios are a critical factor in ore processing and magnet manufacture.
California↗
Characterizing the source of potentially asbestos-bearing commercial vermiculite insulation using in situ IR spectroscopy
Commercially produced vermiculite insulation from Libby, Montana, contains trace levels of asbestiform amphibole, which is known to cause asbestos-related diseases. When vermiculite insulation is found in a building, evaluation for its potential asbestos content traditionally involves collecting a sample from an attic or wall and submitting it for time-consuming analyses at an off-site laboratory. The goal of this study was to determine if in situ near-infrared reflectance measurements could be used to reliably identify the source of vermiculite ore and therefore its potential to contain asbestos. Spectra of 52 expanded ore samples, including attic insulation, commercial packing materials, and horticultural products from Libby, Montana; Louisa, Virginia; Enoree, South Carolina; Palabora, South Africa; and Jiangsu, China, were measured with a portable spectrometer. The mine sources for these vermiculite ores were identified based on collection location, when known, and on differences in elemental composition as measured by electron probe microanalysis. Reflectance spectra of the insulation samples show vibrational overtone and combination absorptions that vary in wavelength position and relative intensity depending on elemental composition and proportions of their constituent micas (i.e., vermiculite ore usually consists of a mixture of hydrobiotite and vermiculite mineral flakes). Band depth ratios of the 1.38/2.32, 1.40/1.42, and 2.24/2.38 μm absorptions allow determination of a vermiculite insulation's source and detection of its potential to contain amphibole, talc, and/or serpentine impurities. Spectroscopy cannot distinguish asbestiform vs. non-asbestiform amphiboles. However, if the spectrally determined mica composition and mineralogy of an insulation sample is consistent with ore from Libby, then it is likely that some portion of the sodic-calcic amphibole it contains is asbestiform, given that all of the nearly two dozen Libby vermiculite insulation samples examined with scanning electron microscopy in this study contain amphiboles. One sample of expanded vermiculite ore from multiple sources was recognized as a limitation of the spectral method, therefore an additional test (i.e., 2.24 μm absorption position vs. 2.24/2.38 μm band depth ratio) was incorporated into the spectral method to eliminate misclassification caused by such mixtures. With portable field spectrometers, the methodology developed can be used to determine vermiculite insulation's source and estimate its potential amphibole content, thereby providing low-cost analysis with onsite reporting to property owners.
American Mineralogist↗
Manganese-enhanced magnetic resonance microscopy of mineralization
Paramagnetic manganese (II) can be employed as a calcium surrogate to sensitize magnetic resonance microscopy (MRM) to the processing of calcium during bone formation. At high doses, osteoblasts can take up sufficient quantities of manganese, resulting in marked changes in water proton T1, T2 and magnetization transfer ratio values compared to those for untreated cells. Accordingly, inductively coupled plasma mass spectrometry (ICP-MS) results confirm that the manganese content of treated cell pellets was 10-fold higher than that for untreated cell pellets. To establish that manganese is processed like calcium and deposited as bone, calvaria from the skull of embryonic chicks were grown in culture medium supplemented with 1 mM MnCl2 and 3 mM CaCl2. A banding pattern of high and low T2 values, consistent with mineral deposits with high and low levels of manganese, was observed radiating from the calvarial ridge. The results of ICP-MS studies confirm that manganese-treated calvaria take up increasing amounts of manganese with time in culture. Finally, elemental mapping studies with electron probe microanalysis confirmed local variations in the manganese content of bone newly deposited on the calvarial surface. This is the first reported use of manganese-enhanced MRM to study the process whereby calcium is taken up by osteoblasts cells and deposited as bone. ?? 2007 Elsevier Inc. All rights reserved.
Magnetic Resonance Imaging↗
Organic petrology and micro-spectroscopy of Tasmanites microfossils: Applications to kerogen transformations in the early oil window
The transformation of kerogen to hydrocarbons in the early stages of oil generation is critical for understanding the resource potential of liquid-rich shale plays. Organic petrology commonly is used for visual evaluation of type, quality, and thermal maturity of organic matter, but the relationship of visual petrographic changes to chemical transformations is not well characterized. To improve understanding of these processes, organic-walled microfossils of the unicellular green alga Tasmanites (composed of algaenan) in Upper Devonian Ohio Shale (Huron Member, Appalachian Basin) were analyzed by micro-spectroscopy techniques including micro-Fourier transform infrared (micro-FTIR), X-ray photoelectron (XPS), electron probe microanalysis (EPMA), and fluorescence. Immature to mid-oil window maturation sequences of core and outcrop samples with solid bitumen reflectance (BR) and vitrinite reflectance (VR) values ranging from 0.45 to 0.80 %Ro were used. Hydrous pyrolysis was applied to low-maturity (BR: 0.25–0.39 %Ro) Huron and time-correlative New Albany shale samples to create similar artificial maturation sequences for comparison. Micro-FTIR spectroscopy revealed a decrease in the CH 2 /CH 3 ratio with increasing maturity, indicating Tasmanites aliphatic chains become shorter and more branched. Oxygenated functional groups decreased relative to aliphatic stretching bands and increased aromaticity was noted at the highest maturities. In samples that were pyrolyzed for 72 h at temperatures of 300–320 °C (BR: 0.56–0.68 %Ro), Tasmanites showed similar trends, whereas at pyrolysis temperatures of 340 °C and higher (BR > 1.0 %Ro), Tasmanites was pseudomorphed by accumulations of solid bitumen, carbonate and sulfide. Replacement of Tasmanites by these phases in hydrous pyrolysis experiments ≥340 °C and its absence at higher maturities (peak oil, VR and BR ≥ 0.9 %Ro) in naturally matured samples, as documented in a previous study, implies that a large fraction of the algaenan component of original organic carbon is converted to petroleum during thermal maturation. XPS analysis indicated the molar proportion of aliphatic carbon increases with increasing thermal maturity, accompanied by decreases in oxygenated functional groups and olefinic carbon. EPMA of Tasmanites showed highest concentrations of S, with concentrations of redox-sensitive trace elements U, Mo, Ni and V generally at or below detection limits. Decrease in organic S with increasing thermal maturity may be related to cleavage of Tasmanites at C S linkages; however, this relationship was inconsistent and presence of adjacent or entrained nanoscale silicate or sulfide phases may impact measured trace element concentrations. Fluorescence microscopy and spectroscopy showed a red shift in spectral maxima and decreased emission intensities with increasing maturity, interpreted as due to non-radiative energy loss possibly because of increased aromaticity. Collectively, these results provide new insights into the in situ chemical transformations that accompany petrographic changes as oil-prone kerogen converts to petroleum with thermal advance from immature conditions into the mid-oil window.
Organic Geochemistry↗
A new basaltic glass microanalytical reference material for multiple techniques
The U.S. Geological Survey (USGS) has been producing reference materials since the 1950s. Over 50 materials have been developed to cover bulk rock, sediment, and soils for the geological community. These materials are used globally in geochemistry, environmental, and analytical laboratories that perform bulk chemistry and/or microanalysis for instrument calibration and quality assurance testing. To answer the growing demand for higher spatial resolution and sensitivity, there is a need to create a new generation of microanalytical reference materials suitable for a variety of techniques, such as scanning electron microscopy/X-ray spectrometry (SEM/EDS), electron probe microanalysis (EPMA), laser ablation inductively coupled mass spectrometry (LA-ICP-MS), and secondary ion mass spectrometry (SIMS). As such, the microanalytical reference material (MRM) needs to be stable under the beam, be homogeneous at scales of better than 10–25 micrometers for the major to ultra-trace element level, and contain all of the analytes (elements or isotopes) of interest. Previous development of basaltic glasses intended for LA-ICP-MS has resulted in a synthetic basaltic matrix series of glasses (USGS GS-series) and a natural basalt series of glasses (BCR-1G, BHVO-2G, and NKT-1G). These materials have been useful for the LA-ICP-MS community but were not originally intended for use by the electron or ion beam community. A material developed from start to finish with intended use in multiple microanalytical instruments would be useful for inter-laboratory and inter-instrument platform comparisons. This article summarizes the experiments undertaken to produce a basalt glass reference material suitable for distribution as a multiple-technique round robin material. The goal of the analytical work presented here is to demonstrate that the elemental homogeneity of the new glass is acceptable for its use as a reference material. Because the round robin exercise is still underway, only nominal compositional ranges for each element are given in the article.
Microscopy Today↗