Geology Reports⌕ Search

SEARCH · Geology Reports

Results for “Spectroscopy”

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 613 records · Page 34Linked to original sources

Petrophysical and geomechanical properties of gas hydrate-bearing sediments recovered from Alaska North Slope 2018 Hydrate-01 Stratigraphic Test Well

Knowledge of petrophysical and geomechanical properties of gas hydrate-bearing sediments are essential for predicting reservoir responses to gas production. The same information is also needed for the designing of production well completions such as specifications for artificial lift, test site water storage capacity, and mesh size for the sand control systems. In December 2018, the Stratigraphic Test Well Hydrate-01 was drilled in the western part of the Prudhoe Bay Unit on the Alaska North Slope as part of the technical planning effort for a future long-term production test being planned and led by a collaborative team from the U.S. Department of Energy - National Energy Technology Laboratory (DOE-NETL), U.S. Geological Survey (USGS), and Japan’s Research and Development Consortium for Pore Filling Hydrate in Sand (MH21-S) (Boswell et al., 2020, Collett et al., 2020, Okinaka et al., 2020). Logging-while-drilling (LWD) data were acquired (Haines et al., 2020, Suzuki et al., 2019) and sidewall core sampling depths were selected from the LWD logs. Sidewall pressure coring was conducted to recover gas hydrate-bearing sediments from two reservoir sections named Unit B and Unit D. A total of 34 cores were successfully recovered by 5 runs of a wireline deployed pressure coring system (CoreVault® System - Halliburton). The core analysis plan for this project is shown in Figure 1. Upon recovery, the pressure core autoclaves were transported from the Alaska North Slope to the Stratum Reservoir laboratory in Anchorage Alaska. To access the cores, they were first quenched in liquid nitrogen while still at high pressure in the core system autoclaves (Figure 1a). The cores were next removed from the pressure corer autoclaves with temperature control support from dry ice and stored under liquid nitrogen at atmospheric pressure. A total of 19 disturbed low-quality cores were processed for index property measurements, which included grain size and grain density analysis. Another 4 core samples were depressurized, trimmed, and core plugs were cut from each core and used to measure intrinsic permeabilities of host sediments (Figure 1). Unsteady-state permeability measurements were conducted on two samples to obtain relative water permeability (Rel.-Perm.) to gas and core scale Nuclear Magnetic Resonance (NMR) transverse relaxation time (T2) distribution measurements were performed to evaluate pore size distribution (Figure 1b). A total of 13 remaining high-quality cores with significant gas hydrate concentrations were preserved for advanced laboratory analysis. The National Institute of Advanced Industrial Science and Technology, as a part of the Japanese National Hydrate Research Program (MH21-S, funded by Ministry of Economy, Trade and Industry), received the 13 remaining high-quality core samples at their laboratories in Sapporo, Japan for advanced core analysis. High-resolution X-ray computed tomography (CT) was used to analyze the physical characteristics of the samples, which showed for the most part undisturbed lithological layers. Cores were lathed into cylindrical shapes and prepared for multi property measurements (Figure 1c). As a result, sediment from Unit D was characterized as silty-sand at ~37% porosity with ~80% gas hydrate saturation. An average hydration number n = 6.16 was measured for the recovered gas hydrate samples by Raman spectroscopy. An average intrinsic permeability of ~400 mD and in situ effective permeability (with hydrate) on the order of ~10 mD was measured for a total of five core samples. The Unit B recovered cores consisted of well sorted sand at ~40% porosity with ~95% gas hydrate saturation. An average intrinsic permeability of ~1 Darcy and in situ effective permeability on the order of ~30 mD was measured for the Unit B cores. Additional laboratory measurements yielded small permeability reductions due to porosity loss with increasing effective stress that simulated sediment consolidation along with depressurization in the highly permeable sandy sediment. The apparent limited change in porosity and permeability may be caused by the low compressibility of quartz sand grains in the recovered cores. X-ray diffraction (XRD) and thermal conductivity analysis also indicated a high quartz content within the recovered cores. Completed triaxial compression tests established internal friction angles based on the Mohr-Coulomb's failure criterion, which were calculated at 40° for hydrate-bearing sediment and 29.8° for hydrate free sediment.

Alaska↗

Micrometer-scale characterization of solid mine waste aids in closure due diligence

Precious- and base-metal mining often occurs in deposits with high acid-generating potential, resulting in mine waste that contains metals in forms of varying bioavailability, and therefore toxicity. The solids that host these metals are often noncrystalline, nanometer to micrometer in size, or undetectable by readily available analytical techniques (e.g., X-ray diffraction). This analytical shortcoming can pose a challenge when attempting to characterize sources and natural attenuation of metals at a given site, which is a best practice to satisfy closure due diligence. Numerous case studies have shown that efforts to characterize mine waste at multiple scales, particularly the micrometer scale, often lead to a better understanding of metal distribution and potential contamination risks. This paper presents a case study that compares the use of both traditional and non-traditional techniques to identify and quantify metal hosts in sediments downstream of the abandoned mine waste piles at the Ely Copper Mine Superfund site in Vermont (USA). The contaminant present in the highest concentration in the sediments is copper, yet not all copper-bearing solids were detected with bulk X-ray diffraction (XRD). At the micrometer scale, a combination of synchrotron-based X-ray absorption spectroscopy (XAS) and an automated mineralogy (AM) system were used to identify the most abundant copper-bearing solids. Bulk XAS and AM also provided semi-quantitative abundances of these solids in the sediment. At the Ely Copper Mine, copper in stream sediments was found to be predominantly hosted in sulphide minerals downstream of a major mine waste pile, whereas upstream copper was predominantly hosted in secondary iron and manganese (oxyhydr)oxides. These copper-bearing hosts were consistent with the expected bioavailability of copper in the sediments based on laboratory toxicity tests with aquatic organisms. When the bulk of copper was present in sulphides, aquatic organisms experienced greater survival than when copper was mostly associated with secondary iron and manganese (oxyhydr)oxides. The information gained from probing the sediments at multiple scales can now be used to prioritize containment and remediation strategies. While synchrotron-based analytical techniques have proven to be invaluable in many studies of mine waste, access to these techniques is limited. In contrast, access to a scanning electron microscope that can perform AM is becoming more common, primarily for the application in mining design and mineral processing operations. More recently, the successful use of AM to characterize mine waste suggests that this technique can be equally as valuable for mine closure plans. The resolution of information obtained may go beyond what is required from a regulatory perspective, but given that the results have the potential to be more conclusive than many traditional techniques, this level of characterization may save time and money in the long run.

Vermont↗

Finalization of the Confocal Laser Scanning Microscopy (CLSM) working group

A working group in Commission II to investigate applications of confocal laser scanning microscopy (CLSM) for organic petrology investigations has finalized with publication of the manuscript “Characterization of bituminite in Kimmeridge Clay by confocal laser scanning and atomic force microscopy” in the International Journal of Coal Geology. The manuscript is available via Open Access from https://doi.org/10.1016/j.coal.2022.103927 and also from the Commission II working group (WG) webpage https://www.iccop.org/workinggroup/confocal-laser-scanning-microscopy-clsm/. A report detailing the full history and results from the WG also is available from the Commission II WG webpage. The working group investigated the application of CLSM to an organic-rich (44 wt.% TOC), thermally immature sample (VRo 0.42%) of the Kimmeridge Clay Formation. CLSM imaging and spectroscopy and atomic force microscopy (AFM) were used to characterize bituminite.

ICCP News↗

Exploring Martian geothermal and liquid water potential with basin modeling

Assessing the potential for geothermal energy and liquid water presence in the Martian subsurface is crucial for future exploration and habitability studies. In this work, we employed comprehensive finite element model simulations adapted specifically for Martian conditions to estimate subsurface temperatures and the potential for liquid water at depth within Martian crater basins. Rock and fluid property values for basin fill were carefully adjusted to match Martian gravity, radiogenic heat generation, and compositional characteristics derived from rover analyses, Martian meteorite samples, and orbital spectroscopy data. Multiple modeling scenarios were explored to systematically evaluate end-member cases across critical variables such as heat flow, lithological composition, and average surface temperature. Sensitivity testing revealed that heat flow and average annual surface temperatures are the most important variables. Results were used in calculations based on a database of Martian craters to estimate the temperature of crater fill at depth. Our model results indicate significant potential for sustained liquid water in the subsurface within sedimentary deposits across a range of crater sizes and latitudes. They further suggest that viable geothermal reservoirs likely exist and are potentially accessible for future Martian missions seeking energy sources or exploring astrobiological hypotheses. This study provides a methodological framework for geothermal and hydrological assessments for the subsurface of Mars, contributing to ongoing planetary exploration strategies.

Conference Paper↗

USGS addresses needs for lithium calibration and quality control materials for pLIBS analysis

Lithium (Li) is a globally important commodity used for energy storage, national defense, human health, and advanced technologies. Lithium resource development requires identifying deposits with elevated concentrations and optimal mineralogy, typically associated with select clays and pegmatites. Lithium is a light, highly reactive alkali metal with low atomic mass that is difficult to detect and quantify using conventional portable geochemical techniques such as X-ray fluorescence (XRF). However, portable laser-induced breakdown spectroscopy (pLIBS) is a powerful analytical technique for lithium exploration due to its ability to analyze solids quickly with minimal preparation. The expanded utility of pLIBS is hampered by the lack of matrix-matched calibration and quality control (QC) materials. The United States Geological Survey (USGS) has developed in-house lithium calibration and QC materials for lithium in clay and pegmatite matrices to address this limitation. We present the workflow and implementation of a custom-built matrix specific calibration on a SciAps Z-300 pLIBS, using proprietary Profile Builder software. The implementation of the custom calibration and quality control standards enables us to collect semiquantitative results directly from the pLIBS while in the field. Ultimately, this calibration has improved confidence in sample selection and collection in the field, providing more efficient site characterization.

Conference Paper↗

Raman spectroscopic characterization of CH4 density over a wide range of temperature and pressure

The positions of the CH 4 Raman ν 1 symmetric stretching bands were measured in a wide range of temperature (from −180 °C to 350 °C) and density (up to 0.45 g/cm 3 ) using high-pressure optical cell and fused silica capillary capsule. The results show that the Raman band shift is a function of both methane density and temperature; the band shifts to lower wavenumbers as the density increases and the temperature decreases. An equation representing the observed relationship among the CH 4 ν 1 band position, temperature, and density can be used to calculate the density in natural or synthetic CH 4 -bearing inclusions.

Journal of Raman Spectroscopy↗

Shift in the Raman symmetric stretching band of N2, CO2, and CH4 as a function of temperature, pressure, and density

The Raman spectra of pure N 2 , CO 2 , and CH 4 were analyzed over the range 10 to 500 bars and from −160°C to 200°C (N 2 ), 22°C to 350°C (CO 2 ), and −100°C to 450°C (CH 4 ). At constant temperature, Raman peak position, including the more intense CO 2 peak ( ν +), decreases (shifts to lower wave number) with increasing pressure for all three gases over the entire pressure and temperature ( PT ) range studied. At constant pressure, the peak position for CO 2 and CH 4 increases (shifts to higher wave number) with increasing temperature over the entire PT range studied. In contrast, N 2 first shows an increase in peak position with increasing temperature at constant pressure, followed by a decrease in peak position with increasing temperature. The inflection temperature at which the trend reverses for N 2 is located between 0°C and 50°C at pressures above ~50 bars and is pressure dependent. Below ~50 bars, the inflection temperature was observed as low as −120°C. The shifts in Raman peak positions with PT are related to relative density changes, which reflect changes in intermolecular attraction and repulsion. A conceptual model relating the Raman spectral properties of N 2 , CO 2 , and CH 4 to relative density (volume) changes and attractive and repulsive forces is presented here. Additionally, reduced temperature-dependent densimeters and barometers are presented for each pure component over the respective PT ranges. The Raman spectral behavior of the pure gases as a function of temperature and pressure is assessed to provide a framework for understanding the behavior of each component in multicomponent N 2 -CO 2 -CH 4 gas systems in a future study.

Journal of Raman Spectroscopy↗

Emission spectra of the cations of some fluoro-substituted phenols in the gaseous phase

Emission spectra of the cations of 2,5- and 3,5-difluorophenol, of 2,3,4- and 2,4,5-trifluorophenol, of 2,3,5,6-tetrafluorophenol and of 2,3,4,5,6-pentafluorophenol have been obtained in the gas phase using low-energy electron beam excitation. The band systems are assigned to the B̃ (π −1 ) → X̃ (π −1 ) electronic transitions of these cations by reference to photoelectron spectroscopic data. The He(Iα) photoelectron spectra and the ionisation energies of ten fluoro-substituted phenols are reported. The symmetries of the four lowest electronic states of these cations are inferred from the radiative decay studies. The lifetimes of the lowest vibrational levels of the B̃ (π −1 ) state of the six fluoro-substituted phenol cations above have also been measured.

Journal of Electron Spectroscopy and Related Pheno↗

Sets of spectral lines for spectrographic thermometry and manometry in d.c. arcs of geologic materials

Sets of 5 Fe(I) lines and 3 Ti(I) Ti(II) line pairs have been characterized for precise spectrographic thermometry and manometry, respectively, in d.c. arcs of geologic materials. The recommended lines are free of spectral interferences, exhibit minimal self absorption within defined concentration intervals, and are useful for chemically-unaltered silicate rocks, arced in an argon—oxygen stream. The functional character of these lines in thermometry and manometry of d.c. arcs for evaluations of electrical parameter effects, for temporal studies, and for matrix-effect investigations on real samples is illustrated.

Spectrochimica Acta Part B: Atomic Spectroscopy↗

Reduction of matrix interferences in furnace atomic absorption with the L'vov Platform

Use of a modified L'vov Platform and ammonium phosphate as a matrix modifier greatly reduced matrix interferences in a commercial Massmann-type atomic absorption furnace. Platforms were readily fabricated from furnace tubes and, once positioned in the furnace, caused no inconvenience in operation. Two volatile elements (Pb, Cd), two of intermediate volatility (Co, Cr) and two which form stable oxides (Al, Sn) were tested in natural water and selected synthetic matrices. In every case for which there was a significant matrix effect during atomization from the tube wall, the platform and platform plus modifier gave improved performance. With lead, for example, an average ratio of 0.48 ± 0.11 was found when the slope of the standard additions plot for six different natural water samples was compared to the slope of the standard working curve in dilute acid. The average slope ratio between the natural water matrices and the dilute acid matrix was 0.94 ± 0.03 with the L'vov Platform and 0.96 ± 0.03 with the platform and matrix modifier. In none of the cases studied did the use of the platform or platform plus modifier cause an interference problem where none existed while atomizing from the tube wall. An additional benefit of the platform was a factor of about two improvement in peak height precision.

Spectrochimica Acta Part B: Atomic Spectroscopy↗

Heating rates in furnace atomic absorption using the L'vov platform

Heating rate profiles for the furnace tube wall, the furnace atmosphere, and a L'vov platform were established for a range of conditions in a cyclically heated graphite atomizer. The tube wall profile was made by direct observation with a recording optical pyrometer. The sodium line reversal method was used to establish the heating rate of the furnace atmosphere, and appearance temperatures for a series metals of differing volatility was used to establish platform profiles. The tube wall heating rate was nearly linear at 2240°C s − until the desired temperature was reached after which the temperature remained constant. The furnace atmosphere reached a given temperature 0.2–0.4 s later than the tube wall through most of the atomize cycle. The platform lagged the tube wall 0.5–0.8 s. Under typical operating conditions the furnace atmosphere was 100–200°C cooler than the tube wall and at nearly constant temperature when the analyte vaporized from the platform. The L'vov platform causes the cyclically heated commercial furnace to approximate the behavior of a constant temperature furnace during atomization.

Spectrochimica Acta Part B: Atomic Spectroscopy↗

The investigation of chemical structure of coal macerals via transmitted-light FT-IR microscopy by X. Sun

A recent paper by Sun [X. Sun, Spectrochim. Acta A 62 (1-3) (2005) 557] attempts to characterize a variety of liptinite, termed "barkinite", from Chinese Permian coals. The component identified does not appear to fundamentally differ from previously-described liptinite macerals included in the International Committee for Coal and Organic Petrology's system of maceral nomenclature. Further, chemical comparisons made with macerals from coals of different rank and age are flawed because the author did not account for changes in chemistry with rank or for the chemical changes associated with botanical changes through geologic time. The author has not satisfactorily proved his hypothesis that the component differs morphologically or chemically from known liptinite-group macerals. ?? 2006 Elsevier B.V. All rights reserved.

Spectrochimica Acta - Part A: Molecular and Biomol↗

Aqueous infrared carboxylate absorbances: Aliphatic di-acids

Aqueous attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectra of 18 aliphatic di-carboxylic acids are reported as a function of pH. The spectra show isosbestic points and intensity changes which indicate that Beer's law is obeyed, and peak frequencies lie within previously reported ranges for aqueous carboxylates and pure carboxylic acids. Intensity sharing from the symmetric carboxylate stretch is evident in many cases, so that bands which are nominally due to alkyl groups show increased intensity at higher pH. The asymmetric stretch of the HA − species is linearly related to the microscopic acidity constantof the H 2 A species, with σ p K <0.25 log units; this relationship falls on the same line as previously observed for mono-carboxylic acids. The linear relationship applies to the acidity constant of the HA − species only when the two acid groups are well separated (>2 intervening atoms). The results suggest that aqueous ATR-FTIR may be able to estimate `intrinsic' p K a values of carboxylic acids, in addition to providing quantitative estimates of ionization.

Spectrochimica Acta - Part A: Molecular and Biomol↗

Determination of provenance soil type using inductively coupled plasma mass spectrometry (ICP-MS) analyses of Pinus ponderosa ash

This study demonstrates the feasibility of determining soil provenance from tree ash composition using elemental analysis and chemometric techniques. To date, no published studies have applied chemometric approaches to classify ash for provenance determination following forest fires. In this work, Pinus ponderosa ash was analyzed to distinguish samples based on soil type and geographic location. Pinus ponderosa , a widely distributed pine species in the western United States where wildfires are prevalent, was selected as a model system. Needles were collected from trees grown in five distinct soil types across northern Arizona and Colorado, then dry-ashed under controlled conditions. Classification was performed using three preprocessing techniques and five machine learning algorithms, including hierarchical modeling structures to optimize separation. Partial least squares discriminant analysis (PLS-DA) following a Box-Cox transformation yielded the highest classification accuracy, achieving a prediction kappa value of 0.98 for soil type identification. However, classification performance decreased when distinguishing both soil type and geographic location, indicating that additional variability may influence predictive accuracy in broader applications. These findings highlight the potential of inductively coupled plasma mass spectrometry (ICP-MS) and machine learning for post-wildfire forensic analysis and environmental monitoring.

Applied Spectroscopy↗

Near infrared spectroscopic examination of charred pine wood, bark, cellulose and lignin: Implications for the quantitative determination of charcoal in soils

The objective of this research was to investigate the effect of charring on near infrared spectra of materials likely to be present in forest fires in order to determine the feasibility of determining charred carbon in soils. Four materials (cellulose, lignin, pine bark and pine wood) and char from these materials created by charring for various durations (1 to 168 h) and at various temperatures (200 to 450??C) were studied. Near infrared spectra and measures of acidity (total acids, carboxylic acids, lactones and phenols as determined by titration) were available for 56 different samples (Not all samples charred at all temperatures/durations). Results showed spectral changes that varied with the material, temperature and duration of charring. Examination of spectra and correlation plots indicated that changes in the constituents of the materials in question, such as loss of OH groups in carbohydrates, rather than direct determination of typical products produced by charring, such as carboxylic acids, lactones and phenols, were the basis for the spectral changes. Finally, while the spectral changes resulting from charring appeared to be relatively unique to each material, PLS calibrations for total acids, carboxylic acids, lactones and phenols were successfully created (with R2 of 0.991, 0.943, 0.931 and 0.944, respectively) indicating that there is a sufficient commonality in the changes to develop calibrations without the need for unique calibrations for each specific set of charring conditions (i.e. material, temperature and time of heating).

Journal of Near Infrared Spectroscopy↗

Analysis of barium and strontium in sediments by dc plasma emission spectrometry

The dc plasma arc is suited to analysis of barium and strontium in a wide range of sedimentary rock matrices, from sands, shales, and carbonates, to ferromanganese nodules. Samples containing 10 ppm to more than 3000 ppm barium and strontium were studied. Both alkali (3500 ppm lithium borate, from a preliminary fusion) and lanthanum salts (1%) in the final solution are needed to achieve freedom from systematic effects due to extreme variation in matrix. In the absence of La, neither Li, Na, K, nor Cs totally eliminated effects of Al and other constituents on emission. Silica addition to the fusion helps achieve proper flux viscosity to aid removal of fused beads from graphite crucibles. The effect of refractory-substance formers such as aluminum with calcium can be reduced or removed by selection of a portion of the arc for emission measurement. However, it was decided not to pursue this approach because of loss in analytical sensitivity and need for greater precision in optical adjustment. Analysis of standard rock samples showed generally satisfactory agreement with precision methods of analysis, and some new standard rock data are reported.

Applied Spectroscopy↗