Search USGS⌕ Search

SEARCH · Search USGS

Results for “Scanning”

Search indexed USGS publications on groundwater, aquifers, geologic maps, mineral resources and earthquakes. Explore source records by subject and place.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 73 records · Page 4Linked to original sources
USGS2022

Characterization of bituminite in Kimmeridge Clay by confocal laser scanning and atomic force microscopy

This work investigates bituminite (amorphous sedimentary organic matter) in Upper Jurassic Kimmeridge Clay source rock via confocal laser scanning microscopy (CLSM) and atomic force microscopy (AFM). These petrographic tools were used to provide better understanding of the nature of bituminite, which has been historically difficult to identify and differentiate from similar organic matter types in source rocks. As part of an International Committee for Coal and Organic Petrology (ICCP) working group, an immature (0.42% vitrinite reflectance), organic-rich (44.1 wt% total organic carbon content) sample of Kimmeridge Clay was distributed to multiple laboratories for CLSM characterization. The primary observations from CLSM imaging and spectroscopy include: 1) the interpreted presence of Botryococcus algae as a contributor to bituminite precursors; 2) color red-shift of sulfide reflectance and bituminite auto-fluorescence from below the sample surface; 3) positive alteration of bituminite from laser-induced photo-oxidation of the sample surface, including fluorescence blue-shift; 4) fluorescence blue-shift associated to higher fluorescence intensity regions in bituminite indicative of compositional (fluorophore) differences; 5) the need for fluorescence spectroscopy standardization as applied via CLSM; and 6) the suitability of CLSM fluorescence spectroscopy to predict solid bitumen reflectance from bituminite spectral emission via calibration to an extant dataset. Secondary CLSM observations include detection of reflected laser light from highly reflective inclusions in bituminite, including sulfides and fusinite, and radiolytic alteration of bituminite caused by substitution of U for Fe in sulfides. Findings from AFM include the observation that surface roughening or surface flattening of bituminite are induced by differential broad ion beam (BIB) milling and are dependent on the location and scale of AFM topology measurement. This result highlights our still limited understanding of the effects of BIB milling on sedimentary organic matter and indicates the need for further research before this technique can be advanced as a standard practice in petrographic sample preparation. Collectively, the results of this study illustrate the general applicability and versatility of AFM and CLSM as tools for organic petrology research, specifically for better understanding of the nature and properties of the bituminite maceral.

Kimmeridge↗
USGS2023

Scanning electron microscopic evaluation of broad ion beam milling effects to sedimentary organic matter: Sputter-induced artifacts or naturally occurring porosity?

Research examining organic-matter hosted porosity has significantly increased during the last decade due to greater focus on understanding hydrocarbon migration and storage in source-rock reservoirs, and technological advances in scanning electron microscopy (SEM) capabilities. The examination of nanometer-scale organic-matter hosted porosity by SEM requires the preparation of exceptionally flat geologic samples beyond the abilities of traditional mechanical polishing, which can deform or otherwise obscure organic surfaces. To meet this demand, broad ion beam (BIB) milling was introduced as a sample preparation technique for SEM petrographic analysis of geologic samples. As with any sample preparation technique, there can be unintended consequences. In this study, we examined the development of nanometer-scale sputter-induced voids caused by BIB milling of thermoset plastic binder material [poly(methyl methacrylate), PMMA] used for the mounting of geologic samples, and artifact sputter-induced voids in the organic matter of Green River Formation and Kimmeridge Clay Formation source rocks. Development of artifact sputter-induced voids was evaluated in relation to variations in the slope of the sample examination surface (0.0–4.9% slope), effectively varying the angle of ion incidence. The results indicate that only minor variations in the angle of ion incidence can generate sputter-induced voids in both PMMA (10.0–386.2 nm diameter sputter-induced voids) and sample sedimentary organic matter (solid bitumen; 12.2–103.6 nm diameter sputter-induced voids). Overall, average artifact pore diameters increased with increasing ion incidence angle within PMMA. Although sputter-induced voids within solid bitumen in the Green River Formation sample were only found in limited extent, the size of these void artifacts falls within the same size range as naturally occurring meso-macroporosity. That is, the pore-like artifacts could easily be misconstrued as naturally developed organic porosity, which is a major concern for SEM-based porosity evaluation methods. This study describes the factors that contribute to the creation of artifact sputter-induced voids, their distinguishing characteristics, and best practices for avoiding the creation of ion-induced artifacts.

International Journal of Coal Geology↗
USGS2025

Confocal laser-scanning microscopy (CLSM)-based thermal maturity of Tasmanites and progress in standardization of fluorescence microspectrometry

Evaluation of thermal maturity in vitrinite-free or vitrinite-deficient sediments via fluorescence microspectrometry can provide relevant information related to petroleum exploration and thermal history assessment. However, variation in spectral fluorescence properties of alginite macerals with increasing thermal maturity is largely underexplored. Here, authors of this study have applied confocal laser-scanning microscopy (CLSM) in conjunction with fluorescence microspectrometry to a maturity series of marine Upper Devonian Tasmanites algae from the Ohio Shale (Huron Member) and a single sample from the Marcellus Formation of the Appalachian Basin. Spectral fluorescence properties of Tasmanites were evaluated in relation to orientation, measurement location, and the number of measurements per sample, and were compared to published literature. Emission spectra of Tasmanites from continuous wave laser excitation (405 nm) were acquired from sections perpendicular and parallel to bedding and at different positions within individual Tasmanites bodies. The results showed a progressive red-shift in emission maxima (λ max ) in a large sample sized maturity series ( N = 19), e.g., 493 to 578 nm for the perpendicular section at middle position. Further, blue-shifted apex and mineral-adjacent positions within sections perpendicular to bedding were observed, with the latter being reported here for the first time. While blue-shift at apex positions can be attributed to mechanical deformation-induced reorientation of photoselected fluorophores, the blue-shifted mineral-adjacent positions could result from strain loading and development of a plastic deformation region at the mineral contact zone with Tasmanites . A decrease in standard deviation with increasing number of measured emission maxima is well-observed, and 15 to 20 individual measurements per sample appears sufficient for low standard deviation and coefficient of variance. CLSM-derived thermal maturity parameters indicated that a moderate positive correlation of red/green quotient (Q 650/500 ; R 2 = 0.67) with solid bitumen reflectance (BR o in %) exists. For reproducible results, the determination of λ max and Q 650/500 should be conducted exclusively in the middle position at perpendicular and parallel sections of the polished whole-rock pellets, where the lowest standard deviation in measurement was observed. These results strengthen the suitability and relevance of the CLSM technique in thermal maturity studies of dispersed organic matter (DOM) and contribute to the standardization of fluorescence microspectrometry methods in organic petrology investigation.

Kentucky, Ohio, Virginia, West Virginia↗
USGS2015

Thermal maturity of Tasmanites microfossils from confocal laser scanning fluorescence microscopy

We report here, for the first time, spectral properties of Tasmanites microfossils determined by confocal laser scanning fluorescence microscopy (CLSM, using Ar 458 nm excitation). The Tasmanites occur in a well-characterized natural maturation sequence ( R o 0.48–0.74%) of Devonian shale ( n = 3 samples) from the Appalachian Basin. Spectral property λ max shows excellent agreement ( r 2 = 0.99) with extant spectra from interlaboratory studies which used conventional fluorescence microscopy techniques. This result suggests spectral measurements from CLSM can be used to infer thermal maturity of fluorescent organic materials in geologic samples. Spectra of regions with high fluorescence intensity at fold apices and flanks in individual Tasmanites are blue-shifted relative to less-deformed areas in the same body that have lower fluorescence intensity. This is interpreted to result from decreased quenching moiety concentration at these locations, and indicates caution is needed in the selection of measurement regions in conventional fluorescence microscopy, where it is common practice to select high intensity regions for improved signal intensity and better signal to noise ratios. This study also documents application of CLSM to microstructural characterization of Tasmanites microfossils. Finally, based on an extant empirical relation between conventional λ max values and bitumen reflectance, λ max values from CLSM of Tasmanites microfossils can be used to calculate a bitumen reflectance equivalent value. The results presented herein can be used as a basis to broaden the future application of CLSM in the geological sciences into hydrocarbon prospecting and basin analysis.

Fuel↗
USGS2014

Characterizing the primary material sources and dominant erosional processes for post-fire debris-flow initiation in a headwater basin using multi-temporal terrestrial laser scanning data

Wildfire dramatically alters the hydrologic response of a watershed such that even modest rainstorms can produce hazardous debris flows. Relative to shallow landslides, the primary sources of material and dominant erosional processes that contribute to post-fire debris-flow initiation are poorly constrained. Improving our understanding of how and where material is eroded from a watershed during a post-fire debris-flow requires (1) precise measurements of topographic change to calculate volumetric measurements of erosion and deposition, and (2) the identification of relevant morphometrically defined process domains to spatially constrain these measurements of erosion and deposition. In this study, we combine the morphometric analysis of a steep, small (0.01 km 2 ) headwater drainage basin with measurements of topographic change using high-resolution (2.5 cm) multi-temporal terrestrial laser scanning data made before and after a post-fire debris flow. The results of the morphometric analysis are used to define four process domains: hillslope-divergent, hillslope-convergent, transitional, and channelized incision. We determine that hillslope-divergent and hillslope-convergent process domains represent the primary sources of material over the period of analysis in the study basin. From these results we conclude that raindrop-impact induced erosion, ravel, surface wash, and rilling are the primary erosional processes contributing to post-fire debris-flow initiation in the small, steep headwater basin. Further work is needed to determine (1) how these results vary with increasing drainage basin size, (2) how these data might scale upward for use with coarser resolution measurements of topography, and (3) how these results change with evolving sediment supply conditions and vegetation recovery.

California↗
USGS2020

Quantifying 40 years of rockfall activity in Yosemite Valley with historical Structure-from-Motion photogrammetry and terrestrial laser scanning

Rockfalls and rockslides are often dominant geomorphic processes in steep bedrock landscapes, but documenting their occurrence can be challenging, requiring frequent monitoring and well resolved spatial data. Repeat application of remote sensing methods such as Terrestrial Laser Scanning (TLS) and Structure-from-Motion (SfM) photogrammetry can detect even very small rockfalls, but typically these acquisitions span only years and may not record rockfall activity representative of longer-term rates of cliff erosion. Inventory databases can extend rockfall records, but are commonly incomplete and prone to observation bias. We employed TLS and SfM on two adjacent cliffs (El Capitan and Middle Brother) in Yosemite Valley, integrating semi-annual data collections from 2010 to 2017 with “historical” (archival) SfM models derived from oblique photographs taken in 1976. Comparing the 1976 SfM models against more recent data allows for more accurate and precise rockfall detection and volume measurement over a 40-year period. Change detection indicates that 235 rockfalls occurred from the two cliffs, more than twice as many events as are recorded in Yosemite's inventory database. Although individual rockfall volumes reported in the inventory database vary from those measured by SfM-TLS, reported cumulative volumes are similar to measured volumes, likely because the large-volume events that account for most of the cumulative volume tend to be widely observed and well-documented. Volume-frequency relationships indicate that the cliffs erode predominantly by less frequent, larger-volume rockfalls, at rates of 0.9 to 1.7 mm/yr. Our study demonstrates how integrated SfM and TLS measurements, especially utilizing SfM models derived from historical imagery, allow detection and quantification of rockfalls spanning several decades, complementing and improving inventory databases, informing rockfall hazard assessment, and providing longer-term rates of cliff erosion.

California↗
USGS2020

Estimating wildfire fuel consumption with multitemporal airborne laser scanning data and demonstrating linkage with MODIS-derived fire radiative energy

Characterizing pre- and post-fire fuels remains a key challenge for estimating biomass consumption and carbon emissions from wildfires. Airborne laser scanning (ALS) data have demonstrated effectiveness for estimating canopy, and to a lesser degree, surface fuel components at fine-scale (i.e., 30 m) across landscapes. Using pre- and post-fire ALS data and corresponding field data, this study estimated consumption of canopy fuel (ΔCF), understory fuel (ΔUF), total fuel (ΔTF), and canopy bulk density (ΔCBD) for the 2012 Pole Creek fire in Oregon, USA (10,760 ha), and portions of the 2011 Las Conchas fire in New Mexico, USA (4,934 ha). Additionally, the feasibility of predicting fuel consumption was tested using separate pre- and post-fire models (PrePost), models combining all pre- and post-fire data (Pooled), and models using all data from both fires (Global). Estimates of ΔTF were then compared to fire radiative energy (FRE, units: MJ) derived from Fire Radiative Power (FRP, units: MW) observations from the Moderate Resolution Imaging Spectroradiometer (MODIS) sensor onboard NASA Terra and Aqua satellites to mechanistically derive a biomass combustion coefficient (BCC, units: kg MJ −1 ). The PrePost and Pooled approaches yielded similar results at Las Conchas, but at Pole Creek insufficient pre-fire field data resulted in erroneous fuel consumption estimates outside the fire perimeter using the PrePost models. These results demonstrated that pre-fire field data were less important for these models than having field data which represent the full range of fuel conditions likely to exist across the landscape. Estimated total biomass consumed for the PrePost, Pooled, and Global models were 226 Gg, 224 Gg, and 224 Gg at Las Conchas, and 581 Gg, 713 Gg, and 552 Gg at Pole Creek. Comparisons between estimated ΔTF and FRE yielded an average BCC for both fires of 0.367 (s.d. ± 0.049) kg MJ −1 based on pixels with at least five MODIS observations. Both higher MODIS observations per pixel and accounting for canopy occlusion of FRE improved the relationship between ΔTF and MODIS-FRE. This study suggested a practical modelling approach for future efforts using only post-fire field observations and quantified a landscape-scale relationship between MODIS-derived FRE and fine-scale fuel consumption consistent with prior experiments.

New Mexico, Oregon↗
USGS2009

Method development for analysis of urban dust using scanning electron microscopy with energy dispersive x-ray spectrometry to detect the possible presence of world trade center dust constituents

The collapse of the World Trade Center Towers on September 11, 2001, sent dust and debris across much of Manhattan and in the surrounding areas. Indoor and outdoor dust samples were collected and characterized by U.S. Geological Survey (USGS) scientists using scanning electron microscopy with energy-dispersive spectrometry (SEM/EDS). From this characterization, the U.S. Environmental Protection Agency and USGS developed a particulate screening method to determine the presence of residual World Trade Center dust in the indoor environment using slag wool as a primary "signature". The method describes a procedure that includes splitting, ashing, and sieving of collected dust. From one split, a 10 mg/mL dust/ isopropanol suspension was prepared and 10-30 ??L aliquots of the suspension placed on an SEM substrate. Analyses were performed using SEM/EDS manual point counting for slag wool fibers. Poisson regression was used to identify some of the sources of uncertainty, which are directly related to the small number of fibers present on each sample stub. Preliminary results indicate that the procedure is promising for screening urban background dust for the presence of WTC dust. Consistent sample preparation of reference materials and samples must be performed by each laboratory wishing to use this method to obtain meaningful and accurate results. ?? 2009 American Chemical Society.

Environmental Science & Technology↗
USGS2000

Snow crystal imaging using scanning electron microscopy: III. Glacier ice, snow and biota

Low-temperature scanning electron microscopy (SEM) was used to observe metamorphosed snow, glacial firn, and glacial ice obtained from South Cascade Glacier in Washington State, USA. Biotic samples consisting of algae ( Chlamydomonas nivalis ) and ice worms (a species of oligochaetes) were also collected and imaged. In the field, the snow and biological samples were mounted on copper plates, cooled in liquid nitrogen, and stored in dry shipping containers which maintain a temperature of-196°C. The firn and glacier ice samples were obtained by extracting horizontal ice cores, 8 mm in diameter, at different levels from larger standard glaciological (vertical) ice cores 7.5 cm in diameter. These samples were cooled in liquid nitrogen and placed in cryotubes, were stored in the same dry shipping container, and sent to the SEM facility. In the laboratory, the samples were sputter coated with platinum and imaged by a low-temperature SEM. To image the firn and glacier ice samples, the cores were fractured in liquid nitrogen, attached to a specimen holder, and then imaged. While light microscope images of snow and ice are difficult to interpret because of internal reflection and refraction, the SEM images provide a clear and unique view of the surface of the samples because they are generated from electrons emitted or reflected only from the surface of the sample. In addition, the SEM has a great depth of field with a wide range of magnifying capabilities. The resulting images clearly show the individual grains of the seasonal snowpack and the bonding between the snow grains. Images of firn show individual ice crystals, the bonding between the crystals, and connected air spaces. Images of glacier ice show a crystal structure on a scale of 1–2 mm which is considerably smaller than the expected crystal size. Microscopic air bubbles, less than 15 μm in diameter, clearly marked the boundaries between these crystal-like features. The life forms associated with the glacier were easily imaged and studied. The low-temperature SEM sample collecting and handling methods proved to be operable in the field; the SEM analysis is applicable to glaciological studies and reveals details unattainable by conventional light microscopic methods.

Washington↗
USGS2018

Method to characterize inorganic particulates in lung tissue biopsies using field emission scanning electron microscopy

Humans accumulate large numbers of inorganic particles in their lungs over a lifetime. Whether this causes or contributes to debilitating disease over a normal lifespan depends on the type and concentration of the particles. We developed and tested a protocol for in situ characterization of the types and distribution of inorganic particles in biopsied lung tissue from three human groups using field emission scanning electron microscopy (FE-SEM) combined with energy dispersive spectroscopy (EDS). Many distinct particle types were recognized among the 13 000 particles analyzed. Silica, feldspars, clays, titanium dioxides, iron oxides and phosphates were the most common constituents in all samples. Particles were classified into three general groups: endogenous , which form naturally in the body; exogenic particles, natural earth materials; and anthropogenic particles, attributed to industrial sources. These in situ results were compared with those using conventional sodium hypochlorite tissue digestion and particle filtration. With the exception of clays and phosphates, the relative abundances of most common particle types were similar in both approaches. Nonetheless, the digestion/filtration method was determined to alter the texture and relative abundances of some particle types. SEM/EDS analysis of digestion filters could be automated in contrast to the more time intensive in situ analyses.

Toxicology Mechanisms and Methods↗
USGS2015

Estimating sturgeon abundance in the Carolinas using side-scan sonar

Sturgeons (Acipenseridae) are one of the most threatened taxa worldwide, including species in North Carolina and South Carolina. Populations of Atlantic Sturgeon Acipenser oxyrinchus in the Carolinas have been significantly reduced from historical levels by a combination of intense fishing and habitat loss. There is a need for estimates of current abundance, to describe status, and for estimates of historical abundance in order to provide realistic recovery goals. In this study we used N -mixture and distance models with data acquired from side-scan sonar surveys to estimate abundance of sturgeon in six major sturgeon rivers in North Carolina and South Carolina. Estimated abundances of sturgeon greater than 1 m TL in the Carolina distinct population segment (DPS) were 2,031 using the count model and 1,912 via the distance model. The Pee Dee River had the highest overall abundance of any river at 1,944 (count model) or 1,823 (distance model). These estimates do not account for sturgeon less than 1 m TL or occurring in riverine reaches not surveyed or in marine waters. Comparing the two models, the N -mixture model produced similar estimates using less data than the distance model with only a slight reduction of estimated precision.

Marine and Coastal Fisheries: Dynamics, Management↗
USGS1984

Side-scan sonar assessment of gray whale feeding in the Bering Sea

Side-scan sonar was used to map and measure feeding pits of the California gray whale over 22,000 square kilometers of the northeastern Bering Sea floor. The distribution of pits, feeding whales, ampeliscid amphipods (whale prey), and a fine-sand substrate bearing the amphipods were all closely correlated. The central Chirikov Basin and nearshore areas of Saint Lawrence Island supply at least 6.5 percent of the total gray whale food resource in summer. While feeding, the whales resuspend at least 1.2 × 10 8 cubic meters of sediment annually; this significantly affects the geology and biology of the region.

Alaska↗
USGS1968

Aquilapollenites: Fossil pollen as seen under the scanning electron microscope

Photographs of a Late Cretaceous species of Aquilapollenites illustrate the usefulness of the scanning electron microscope (SEM) for the study of fossil pollen . The SEM has the advantages of great depth of focus and wide range of magnification; using present techniques, its use for the study of unsectioned specimens is limited to the observation of surface detail.

Geological Society of America Bulletin↗
USGS2025

Combining acoustic telemetry and side-scan sonar to estimate abundance of endangered shortnose sturgeon in the Hudson River, New York

For endangered shortnose sturgeon (Acipenser brevirostrum), the ability to estimate and monitor population size is critical for tracking species’ recovery. Yet, contemporary abundance estimates have not been completed for many shortnose sturgeon populations, largely owing to the difficulty in using traditional abundance estimators for sturgeons. Here, we estimate the adult shortnose sturgeon population size of the Hudson River, NY by integrating data from two largely passive sampling methods – acoustic telemetry and side-scan sonar – into a Bayesian hierarchical model of abundance. We estimated the adult abundance to be 69,798 individuals (95% CI = 9,207-185,666), making the Hudson River the largest extant shortnose sturgeon population. Despite this, the population remains vulnerable to localized disturbances, as over 40% of the population congregated in a small overwintering habitat that coincides with an area of high anthropogenic activity. Accordingly, recurrent demographic surveys may be beneficial for gaining insight into the relative effects of anthropogenic and naturally stochastic processes shaping shortnose sturgeon demography. Our modeling framework provides a relatively low-cost alternative for future demographic monitoring of species of conservation concern.

New York↗
USGS2006

An exploratory method to detect tephras from quantitative XRD scans: Examples from Iceland and east Greenland marine sediments

Tephras, mainly from Iceland, are becoming increasingly important in interpreting leads and lags in the Holocene climate system across NW Europe. Here we demonstrate that Quantitative Phase Analysis of x-ray diffractograms of the < 2 mm of marine sediment fraction (ie, sand, silt and clay) from Iceland and East Greenland can detect peaks in volcanic glass concentrations (weight%) even though discrete tephra layers are not visible; thus it provides a rapid overview of the probable location of volcanic glass within sediment sequences. Experiments in spiking samples from Baffin Bay and an artificial mixture of minerals with known weight% fractions of an Icelandic tephra (Hekla 4) demonstrate a significant correlation (r2 = 0.92 and 0.97) between known and estimated weight percentages, although the slope of the measured to observed weight% is around 0.65 and not 1.0 as expected. In core B997-321PC off North Iceland we identify tephras from point counting in the > 150 um fraction and identify these same peaks in XRD scans - two of these correlate geochemically and chronologically with Hekla 1104 and 3. At a distal site to the WNW of Iceland, on the East Greenland margin (core MD99-2317), the weight% of volcanic glass reaches values of 11% at about the time of the Saksunarvatn tephra. The XRD method identifies the presence of volcanic glass but not its elemental composition; hence it will assist in focusing attention on specific sections of sediment cores for subsequent geochemical fingerprinting of tephras. ?? 2006 SAGE Publications.

Holocene↗
USGS1987

Sedimentary processes on the northwestern Iberian continental margin viewed by long-range side-scan sonar and seismic data

The effects of an eastern boundary current in the North Atlantic have been mapped from about 39° north latitude along the Iberian margin to as far north as 43°30 north latitude at the western margin of Galicia Bank. The geostrophic current has produced sediment drifts that are covered with bedforms. The sediment drifts are difficult to detect on Gloria long-range side-scan sonar data but are easily resolved on seismic-reflection records as anomalously thick accumulations of sediment banked against either buried or outcropping basement highs. The bedforms ornamenting the drift surfaces were subdivided into 1,000-m water-depth intervals, and their dimensions were tabulated. There are few bedforms in water depths less han 2,000 m, but from depths between 2,000 and 4,000 m they are numerous and have a mean wavelength of 695 m. Bedforms from depths greater than 4,000 m have a mean wavelength of 999 m. The different wavelengths from different water depths suggest two distinct and separated boundary flows. The wave heights of all bedforms found in water depths greater than 2,000 m are less than 10 m. In order to investigate the continuity of sediment drifting through geological time, the stratigraphic section drilled at DSDP Site 398 was reinterpreted and, using seismic-reflection profiles, was traced throughout the northern Iberian margin. Together, the lithostratigraphic and seismic data indicate that sediment drifting developed along this margin in the Eocene. The lithofacies of the Eocene section is t e oldest to have numerous layers of sand and silt. An unconformity separates the Eocene section from the latest Miocene-Pliocene section. The unconformity is interpreted to be the result of the initial pulses of Mediterranean outflow that followed the Messinian desiccation events. A second period of sediment drifting commenced during the Pliocene once the Mediterranean basin filled and the flow out of the Strait of Gibraltar resumed.

Journal of Sedimentary Petrology↗
USGS2024

Scanning electron microscopy of clays and clay minerals

The scanning electron microscope (SEM) proves to be ideally suited for studying the configuration, texture, and fabric of clay samples. Growth mechanics of crystalline units—interpenetration and interlocking of crystallites, crystal habits, twinning, helical growth, and topotaxis—also are uniquely revealed by the SEM. Authigenic kaolins make up the bulk of the examples because their larger crystallite size, better crystallinity, and open texture make them more suited to examination by the SEM than most other clay mineral types.

Clays and Clay Minerals↗
USGS2017

Analysis of artificially matured shales with confocal laser scanning raman microscopy: Applications to organic matter characterization

Raman spectroscopy has been suggested as a method for characterizing the thermal maturity of rocks. The literature contains many empirical correlations between thermal maturity proxies, such as vitrinite reflectance (V Ro ) and pyrolysis-T max , with spectral metrics such as Raman peak-widths, peak-center positions, peak-areas and all manner of differences and ratios of these parameters. However, while these correlations may be convincing for small data sets from limited sample series, broader application of these metrics to disparate and heterogeneous samples proves difficult and there remains no consensus. In this extended abstract, Raman spectroscopy is introduced and the history of Raman analysis of carbonaceous material is briefly outlined, highlighting some of the latent difficulties and potential sources of bias. We suggest the organization of a community working group to establish terminology, guidelines, procedures and standards necessary for the successful development of this technique to characterize organic matter in an accessible, unbiased, and reproducible manner. For the present multi-phase study, immature shale samples from the Bakken and Duvernay formations were subjected to hydrous pyrolysis for 72 hours at temperatures from 280°C to 360°C. Rock residues were mounted and polished for analysis via confocal laser-scanning Raman microscopy and reflectance. The maturation series from the Bakken was randomized for the Phase-I single-blind study to be presented at this conference. For the Phase-II study, solid bitumen reflectance (B Ro ) values for the Duvernay series will be known. Multiple hyperspectral maps were collected from each Bakken sample, with each map consisting of a single diffraction-limited spot-size spectrum per 1 µm 2 in rectangular areas several hundred micrometers on a side. Initial attempts at using basic spectral metrics on small numbers of hand-selected spectra to sort the blind series produced inconclusive results: any number of possible correlations could be found. In an improved approach, the statistics of the full spectral datasets were leveraged to: 1) objectively identify organic carbon types (OCTs) in a given map based on Raman and fluorescence spectral characteristics, 2) identify those OCTs in other maps from the same sample and determine if the heterogeneity of the sample has been adequately characterized, and 3) identify the same OCTs in maps from other samples in the maturation series. In ongoing work, our goals are to: 1) use these analyses of the blind series to develop a hypothesis for a correlation to maturation, 2) test the hypothesis by applying the same analyses to the known Duvernay series (in Phase-II), 3) if necessary refine the hypothesis based on observations from the Duvernay analysis, and 4) finally reveal the true order of the Bakken series to verify if the hypothesized correlation accurately predicts the maturity order of the samples. In this document, we share progress to date. The analysis of one area of interest is detailed showing the differentiation of two OCTs based on Raman and fluorescence spectral features, including the use of 2-factor histograms, Principle Components Analysis (PCA), and Nonlinear Iterative Peak Fitting (NIPF).

Conference Paper↗