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USGS2013

Sediment geochemistry of Corte Madera Marsh, San Francisco Bay, California: have local inputs changed, 1830-2010?

Large perturbations since the mid-1800s to the supply and source of sediment entering San Francisco Bay have disturbed natural processes for more than 150 years. Only recently have sediment inputs through the Sacramento-San Joaquin Delta (the Delta) decreased to what might be considered pre-disturbance levels. Declining sediment inputs to San Francisco Bay raise concern about continued tidal marsh accretion, particularly if sea level rise accelerates in the future. The aim of this study is to explore whether the relative amount of local-watershed sediment accumulating in a tidal marsh has changed as sediment supply from the Sacramento-San Joaquin Rivers has decreased. To address this question, sediment geochemical indicators, or signatures, in the fine fraction (silt and clay) of Sacramento River, San Joaquin River, San Francisco Bay, and Corte Madera Creek sediment were identified and applied in sediment recovered from Corte Madera Marsh, one of the few remaining natural marshes in San Francisco Bay. Total major, minor, trace, and rare earth element (REE) contents of fine sediment were determined by inductively coupled plasma mass and atomic emission spectroscopy. Fine sediment from potential source areas had the following geochemical signatures: Sacramento River sediment downstream of the confluence of the American River was characterized by enrichments in chromium, zirconium, and heavy REE; San Joaquin River sediment at Vernalis and Lathrop was characterized by enrichments in thorium and total REE content; Corte Madera Creek sediment had elevated nickel contents; and the composition of San Francisco Bay mud proximal to Corte Madera Marsh was intermediate between these sources. Most sediment geochemical signatures were relatively invariant for more than 150 years, suggesting that the composition of fine sediment in Corte Madera Marsh is not very sensitive to changes in the magnitude, timing, or source of sediment entering San Francisco Bay through the Delta. Nor does there appear to be a ubiquitous increase in the proportion of fine sediment from Corte Madera watershed accumulating in the marsh during the last 20 years when sediment inflows through the Delta have decreased to pre-disturbance levels. We conclude that a large, well-mixed reservoir, such as the transportable fine sediment pool in San Francisco Bay, is the primary source of sediment to Corte Madera Marsh, and this source buffers the marsh against changes in sediment supply from the Delta and local watersheds. This study also found that Corte Madera Marsh sediment between about 10-30 centimeters depth is highly contaminated with lead, likely a legacy of lead smelter operations near Carquinez Strait and leaded gasoline use.

California↗

USGS1990

Reconnaissance wadi-sediment geochemical survey of the Bi'r Jarbuah area, Kingdom of Saudi Arabia

A reconnaissance wadi-sediment geochemical survey for gold was conducted in the Bi'r Jarbuah Area (lat 20° 45' 00"-21 ° 00' 00" N., long 43° 30' 00"- 43° 41' 00" K). The area is located in the northern part of a regional concentration of gold occurrences, the Jabal Ishmas-Wadi Tathlith gold belt. Panned concentrates and minus-80-mesh fractions were obtained from 300 samples collected from a 320 km 2 area and analysed by atomic-absorption spectroscopy. Analyses of the pannedconcentrate samples proved to be more definitive than sieved samples in delineating areas of mineralization. Most of the anomalous gold-and arsenic-bearing wadi-sediment samples are located along an irregular contact between gneissic and dioritic rocks in the center of an area characterized by the presence of subparallel dacitic dike swarms. Most of the ancient gold mines are also located along this contact. Gold is associated with arsenic but not with silver. Five areas containing gold-anomalies areas and 6 areas containing tellurium anomalies and the contact zone between the diorite and the paragneiss are recommended for further investigation of precious-metals resources.

Open-File Report↗

USGS1998

Analytical results for forty-two fluvial tailings cores and seven stream sediment samples from High Ore Creek, northern Jefferson County, Montana

Metal-mining related wastes in the Boulder River basin study area in northern Jefferson County, Montana have been implicated in their detrimental effects on water quality with regard to acid-generation and toxic-metal solubility. Sediments, fluvial tailings and water from High Ore Creek have been identified as significant contributors to water quality degradation of the Boulder River below Basin, Montana. A study of 42 fluvial tailings cores and 7 stream sediments from High Ore Creek was undertaken to determine the concentrations of environmentally sensitive elements (i.e. Ag, As, Cd, Cu, Pb, Zn) present in these materials, and the mineral phases containing those elements. Two sites of fluvial deposition of mine-waste contaminated sediment on upper High Ore Creek were sampled using a one-inch soil probe. Forty-two core samples were taken producing 247 subsamples. The samples were analyzed by ICP-AES (inductively coupled-plasma atomic emission spectroscopy) using a total mixed-acid digestion. Results of the core analyses show that the elements described above are present at very high concentrations (to 22,000 ppm As, to 460 ppm Ag, to 900 ppm Cd, 4,300 ppm Cu, 46,000ppm Pb, and 50,000 ppm Zn). Seven stream-sediment samples were also analyzed by ICP-AES for total element content and for leachable element content. Results show that the sediment of High Ore Creek has elevated levels of ore-related metals throughout its length, down to the confluence with the Boulder River, and that the metals are, to a significant degree, contained in the leachable phase, namely the hydrous amorphous iron- and manganese-hydroxide coatings on detrital sediment particles.

Montana↗

USGS1999

Elemental analyses of modern dust in southern Nevada and California

Selected samples of modern dust collected in marble traps at sites in southern Nevada and California (Reheis and Kihl, 1995; Reheis, 1997) have been analyzed for elemental composition using instrumental neutron activation analysis (INAA) and inductively coupled plasma atomic emission spectroscopy (ICP-AES) and inductively coupled plasma mass spectroscopy (ICP-MS). For information on these analytical techniques and their levels of precision and accuracy, refer to Baedecker and McKown (1987) for INAA, to Briggs (1996) for ICP-AES, and to Briggs and Meier (1999) for ICP-MS. This report presents the elemental compositions obtained using these techniques on dust samples collected from 1991 through 1997. The dust-trap sites were established at varying times; some have been maintained since 1984, others since 1991. For details on site location, dust-trap construction, and collection techniques, see Reheis and Kihl (1995) and Reheis (1997). Briefly, the trap consists of a coated angel-food cake pan painted black on the outside and mounted on a post about 2 m above the ground. Glass marbles rest on a circular piece of galvanized hardware cloth (now replaced by stainless-steel mesh), which is fitted into the pan so that it rests 3-4 cm below the rim. The 2-m height eliminates most saltating sand-sized particles. The marbles simulate the effect of a gravelly fan surface and prevent dust that has filtered or washed into the bottom of the pan from being blown back out. The dust traps are fitted with two metal straps looped in an inverted basket shape; the top surfaces of the straps are coated with a sticky material that effectively discourages birds from roosting.

California, Nevada↗

USGS1999

Analytical results for 35 mine-waste tailings cores and six bed sediment samples, and an estimate of the volume of contaminated materials at Buckeye meadow on upper Basin Creek, northern Jefferson County, Montana

Metal-mining related wastes in the Boulder River basin study area in northern Jefferson County, Montana have been implicated in their detrimental effects on water quality with regard to acid-generation and toxic-metal solubilization. Flotation-mill tailings in the meadow below the Buckeye mine, hereafter referred to as the Buckeye mill-tailings site, have been identified as significant contributors to water quality degradation of Basin Creek, Montana. Basin Creek is one of three tributaries to the Boulder River in the study area; bed sediments and waters draining from the Buckeye mine have also been implicated. Geochemical analysis of 35 tailings cores and six bed-sediment samples was undertaken to determine the concentrations of Ag, As, Cd, Cu, Pb,and Zn present in these materials. These elements are environmentally significant, in that they can be toxic to fish and/or the invertebrate organisms that constitute their food. A suite of one-inch cores of dispersed flotation-mill tailings and underlying premining material was taken from a large, flat area north of Basin Creek near the site of the Buckeye mine. Thirty-five core samples were taken and divided into 204 subsamples. The samples were analyzed by ICP-AES (inductively coupled plasma-atomic emission spectroscopy) using a mixed-acid digestion. Results of the core analyses show that the elements listed above are present at moderate to very high concentrations (arsenic to 63,000 ppm, silver to 290 ppm, cadmium to 370 ppm, copper to 4,800 ppm, lead to 93,000 ppm, and zinc to 23,000 ppm). Volume calculations indicate that an estimated 8,400 metric tons of contaminated material are present at the site. Six bed-sediment samples were also subjected to the mixed-acid total digestion, and a warm (50°C) 2M HCl-1% H 2 O 2 leach and analyzed by ICP-AES. Results indicate that bed sediments of Basin Creek are only slightly impacted by past mining above the Buckeye-Enterprise complex, moderately impacted at the upper (eastern) end of the tailings area, and heavily impacted at the lower (western) end of the area and downstream. The metals are mostly contained in the 2M HCl-1% H 2 O 2 leachable phase, which are the hydrous amorphous iron- and manganese-hydroxide coatings on detrital sediment particles.

Montana↗

USGS2023

Groundwater chemistry and hexavalent chromium

Water samples collected by the U.S. Geological Survey from more than 100 wells between March 2015 and November 2017 in Hinkley and Water Valleys, in the Mojave Desert 80 miles northeast of Los Angeles, California, were analyzed for field parameters, major ions, nutrients, and selected trace elements, including hexavalent chromium, Cr(VI). Water from most wells was alkaline and oxic. The pH ranged from 6.9 in water-table wells near recharge areas along the Mojave River to 9.4 in deeper wells farther downgradient in the northern subarea. Hexavalent chromium concentrations measured by ion chromatography using U.S. Environmental Protection Agency Method 218.6 and a version of that method used for detection of Cr(VI) concentrations as low as 0.06 micrograms per liter (μg/L), produced results comparable to field speciation with subsequent analyses by graphite furnace atomic absorption spectroscopy (coefficient of determination, R 2 , of 0.97). Hexavalent chromium concentrations ranged from less than the study reporting level of 0.10 to 2,500 μg/L. The highest concentrations were within the October–December 2015 (Q4 2015) regulatory Cr(VI) plume downgradient from the Hinkley compressor station. Hexavalent chromium concentrations outside the Q4 2015 regulatory Cr(VI) plume were as high as 11 μg/L. Hexavalent chromium concentrations in water from most wells were distributed in a narrow redox potential and pH band within the overlapping chromate ion, CrO 4 2− (aqueous) , and manganese-3, Mn(III) (solid) , stability fields. The redox potential of water from some wells completed in carbonate-rich mudflat/playa deposits approached the more oxic manganese-4, Mn(IV) (solid) , stability field. However, Cr(VI) concentrations in porewater pressure-extracted from Mn(IV)-containing deposits in the eastern subarea did not exceed 3.3 μg/L, and porewater does not appear to be a source of Cr(VI) concentrations greater than this concentration in water from wells in the eastern subarea. On the basis of comparison with California-wide data, Cr(VI) concentrations at the measured pH were higher than expected for uncontaminated water from wells (1) within the Q4 2015 regulatory Cr(VI) plume, (2) within the eastern subarea nominally crossgradient from the Hinkley compressor station and upgradient from the Q4 2015 regulatory Cr(VI) plume, and (3) from shallow wells in the northern subarea downgradient from the leading edge of the Q4 2015 regulatory Cr(VI) plume. Hexavalent chromium concentrations in alkaline water from wells in the northern subarea of Hinkley Valley and in Water Valley were within ranges expected for uncontaminated water elsewhere in California given their pH and trace-element composition. Hexavalent chromium concentrations were higher than expected on the basis of selected trace-element concentrations that co-occur with Cr(VI) in water from wells within the Q4 2015 regulatory Cr(VI) plume and from wells in the eastern and northern subareas near the plume margins. Hexavalent chromium concentrations did not exceed 4 μg/L in water from domestic wells sampled in Hinkley and Water Valleys and were generally within ranges expected for uncontaminated groundwater given their pH and trace-element composition. Interpretations derived from Cr(VI) and pH, and from Cr(VI) and selected trace-element concentrations collected between March 2015 and November 2017 were used within a summative-scale analysis to determine the Cr(VI) plume extent (chapter G). However, Cr(VI) background concentrations (chapter G) were calculated from regulatory data collected from selected wells between April 2017 and January 2018.

California↗

USGS1998

A table of polyatomic interferences in ICP-MS

Spectroscopic interferences are probably the largest class of interferences in ICP-MS and are caused by atomic or molecular ions that have the same mass-to-charge as analytes of interest. Current ICP-MS instrumental software corrects for all known atomic “isobaric” interferences, or those caused by overlapping isotopes of different elements, but does not correct for most polyatomic interferences. Such interferences are caused by polyatomic ions that are formed from precursors having numerous sources, such as the sample matrix, reagents used for preparation, plasma gases, and entrained atmospheric gases.

Atomic Spectroscopy↗

USGS1999

A lead isotope distribution study in swine tissue using ICP-MS

In the United States lead is an ubiquitous environmental pollutant that is a serious human health hazard, especially for women of childbearing age, developing fetuses, and young children. Information concerning the uptake and distribution of lead to maternal and fetal tissues during pregnancy is poorly documented. A study was designed using domestic swine and lead isotope enrichment methodology to focus on maternal absorption and distribution of lead into bone and soft tissues, including the fetal compartment, under varying conditions of oral lead exposure and during altered physiological states (pregnant vs unbred). Total lead levels and Pb207/Pb206 ratios in bone (femur and vertebra), blood, and soft tissues (liver, kidney, brain) were determined by ICP-MS. Lead in fetal tissues derived from maternal bone could be differentiated from that derived from exogenous dosing. Unbred swine absorbed much less lead than pregnant females receiving the same dose. The accuracy and precision of ICP-MS at the instrumental level and for the entire method (sample collection, digestion, and analysis) were evaluated for both Pb207/Pb206 ratios and total lead. Several changes were suggested in method design to improve both instrumental and total method precision.

Atomic Spectroscopy↗

USGS2020

Examination of inertinite within immature Eagle Ford Shale at the nanometer-scale using atomic force microscopy-based infrared spectroscopy

The nanoscale molecular composition of sedimentary organic matter is challenging to characterize in situ given the limited tools available that can adequately interrogate its complex chemical structure. This is a particularly relevant issue in source rocks, as kerogen composition will strongly impact its reactivity and so is critical to understanding petroleum generation processes during catagenesis. The recent advent of tip-enhanced analytical methods, such as atomic force microscopy-based infrared spectroscopy (AFM-IR), has allowed for the major compositional features of kerogen and other types of in situ organic matter to be elucidated at spatial resolutions at or below 50 nm. Here AFM-IR was applied to examine inertinite, an important organic matter type, present in a thermally immature Eagle Ford calcareous mudstone. The data show that the nanoscale molecular composition of the examined inertinite is (i) less heterogeneous than solid bitumen in more thermally mature Eagle Ford samples and (ii) more hydrogen- and oxygen-rich than inertinite examined in the New Albany Shale.

Texas↗

USGS2018

Quantitative evaluation of vitrinite reflectance and atomic O/C in coal using Raman spectroscopy and multivariate analysis

Vitrinite reflectance (VRo) is a standard petrographic method for assessing thermal maturity (rank) of coal. The vitrinite reflectance technique, however, requires significant petrographic experience, can be time-consuming, and may be biased by analyst subjectivity. Correlations between coal rank and Raman spectral properties are a promising alternative that can supplant some of the limitations inherent in the VRo protocol. The traditional peak-fitting methodologies for quantifying metrics from Raman spectra, however, also suffer from analyst subjectivity that can affect correlations between analyte and spectral properties. This research combines high-throughput Raman spectroscopy with multivariate analysis (MVA) to create calibration models for the prediction of coal rank though VRo and atomic O/C ratio. MVA techniques eliminate the ambiguous subjectivity prevalent in peak-fitting methods by evaluating the full Raman spectrum, then identifying the integral vibrational modes for constructing accurate models. Partial least squares (PLS) regression models were developed using Raman spectra and VRo values (0.23–5.23%) for 68 geographically diverse coal samples. The calibration set was validated using one-half of the samples to rigorously assess the model’s predictive accuracy. The root mean standard error of prediction was 0.19 for the VRo model and 0.014 for the atomic O/C model. Both models exhibited linear correlations, with coefficients of determination ( R 2 ) for the validation set of 0.99 (VRo) and 0.93 (atomic O/C), despite the geographic and rank diversity of the samples. This study demonstrates the applicability and power of using PLS models for the prediction of both the VRo and atomic O/C ratio from Raman spectra. The quantitative MVA protocol contained herein provides a Raman alternative to the VRo industry benchmark for coal rank that is not subject to the limitations and subjectivity of peak-fitting methods.

Fuel↗

USGS2020

Nanoscale molecular composition of solid bitumen from the Eagle Ford Group across a natural thermal maturity gradient

Microscopic solid bitumen is a petrographically defined secondary organic matter residue produced during petroleum generation and subsequent oil transformation. The presence of solid bitumen impacts many reservoir properties including porosity, permeability, and hydrocarbon generation and storage, among others. Furthermore, solid bitumen reflectance is an important parameter for assessing the thermal maturity of formations with little to no vitrinite. While the molecular composition of solid bitumen will strongly impact associated parameters such as the development of organic matter porosity, hydrocarbon generation, and optical reflectance, assessing the molecular composition of solid bitumen in situ within shale reservoirs can be challenging due to the small grain sizes (often ≤1 μm in diameter) and the inherent heterogeneity of shale formations. Here we employ the recently developed atomic force microscopy based infrared spectroscopy (AFM-IR) technique to investigate solid bitumen molecular composition in situ within shale samples from the Late Cretaceous Eagle Ford Group. These samples possess sulfur-rich type II kerogens that span a natural thermal maturity gradient from early oil generation to the dry gas window. The application of AFM-IR allows for the rapid collection of thousands of compositional measurements from solid bitumen with ∼50 nm resolution. Our results indicate that (i) solid bitumen from the lower Eagle Ford displays both intra- and intergranular variation in the relative abundance of CH 2 , C═C, and C═O moieties present; (ii) this molecular variation tends to, but does not always, decrease with an increase in thermal maturity; and (iii) the solid bitumen composition between samples, from an atomic ratio perspective, is more similar than analysis of bulk kerogen isolates would indicate. These findings are discussed with perspective toward understanding the impact of thermal stress on the composition of secondary organic matter within the Eagle Ford Shale and highlight the growing awareness that organic matter heterogeneity within petroliferous mudrocks extends down to the nanoscale regime.

Energy and Fuels↗

USGS2019

Nanoscale molecular fractionation of organic matter within unconventional petroleum source beds

Fractionation of petroleum during migration through sedimentary rock matrices has been observed across lengths of meters to kilometers. Selective adsorption of specific chemical moieties at mineral surfaces and/or the phase behavior of petroleum during pressure changes typically are invoked to explain this behavior. Such phenomena are of interest as they impact both the quality and recoverability of petroleum resources. Given the current emphasis on unconventional (continuous) resources, there is a need to understand petroleum fractionation occurring during expulsion and migration at the nanometer to micron scale, due to the fine-grained nature of petroliferous mudrocks. Here, organic matter compositional differences observed within kukersites (petroleum source beds containing acritarch Gloeocapsomorpha prisca) and the overlying carbonate reservoir layer from the Ordovician Stonewall Formation are explored using a suite of spectroscopic methods, primarily through atomic force microscopy based infrared spectroscopy (AFM-IR). AFM-IR is capable of providing spatial resolutions approaching 50 nm and allows for assessment of the molecular fingerprint of kukersite organic matter across transition zones from organic-rich ‘source’ layers into neighboring carbonate ‘reservoir’ layers ~150 μm away. Results indicate that organic matter composition begins to vary immediately following expulsion from source layers, with loss of carbonyl groups and a concomitant decrease in alkyl chain-length, as migration distance increases. These chemical transitions correlate with a decrease in fluorescence intensity, increase in solid bitumen reflectance, and increase in Raman aromaticity proxies (D-G band separation) in the organic matter. Our findings are consistent with the retention of polar compounds onto mineral grains during expulsion and migration, following primary cracking and bituminization of the Gloeocapsomorpha prisca kerogen.

Energy and Fuels↗

USGS2017

Nanoscale geochemical and geomechanical characterization of dispersed organic matter in shale by infrared nanoscopy

Solid organic matter (OM) plays an essential role in the generation, migration, storage, and production of hydrocarbons from economically important shale rock formations. Electron microscopy images have documented spatial heterogeneity in the porosity of OM at nanoscale, and bulk spectroscopy measurements have documented large variation in the chemical composition of OM during petroleum generation. However, information regarding the heterogeneity of OM chemical composition at the nanoscale has been lacking. Here we demonstrate the first application of atomic force microscopy-based infrared spectroscopy (AFM-IR) to measure the chemical and mechanical heterogeneity of OM in shale at the nanoscale, orders of magnitude finer than achievable by traditional chemical imaging tools such as infrared microscopy. We present a combination of optical microscopy and AFM-IR imaging to characterize OM heterogeneity in an artificially matured series of New Albany Shales. The results document the evolution of individual organic macerals with maturation, providing a microscopic picture of the heterogeneous process of petroleum generation.

Nature Communications↗

USGS2000

Formation evaluation of gas hydrate-bearing marine sediments on the Blake Ridge with downhole geochemical log measurements

The analyses of downhole log data from Ocean Drilling Program (ODP) boreholes on the Blake Ridge at Sites 994, 995, and 997 indicate that the Schlumberger geochemical logging tool (GLT) may yield useful gas hydrate reservoir data. In neutron spectroscopy downhole logging, each element has a characteristic gamma ray that is emitted from a given neutron-element interaction. Specific elements can be identified by their characteristic gamma-ray signature, with the intensity of emission related to the atomic elemental concentration. By combining elemental yields from neutron spectroscopy logs, reservoir parameters including porosities, lithologies, formation fluid salinities, and hydrocarbon saturations (including gas hydrate) can be calculated. Carbon and oxygen elemental data from the GLT was used to determine gas hydrate saturations at all three sites (Sites 994, 995, and 997) drilled on the Blake Ridge during Leg 164. Detailed analyses of the carbon and oxygen content of various sediments and formation fluids were used to construct specialized carbon/oxygen ratio (COR) fan charts for a series of hypothetical gas hydrate accumulations. For more complex geologic systems, a modified version of the standard three-component COR hydrocarbon saturation equation was developed and used to calculate gas hydrate saturations on the Blake Ridge. The COR-calculated gas hydrate saturations (ranging from about 2% to 14% bulk volume gas hydrate) from the Blake Ridge compare favorably to the gas hydrate saturations derived from electrical resistivity log measurements.

Conference Paper↗

USGS1999

Effects of humic substances on the bioconcentration of polycyclic aromatic hydrocarbons: Correlations with spectroscopic and chemical properties of humic substances

The presence of dissolved humic substances (HS, fulvic and humic acids) generally reduces the up take of hydrophobic organic compounds into aquatic organisms. The extent of this effect depends both on the concentration and on the origin of the HS. The aim of this study was to investigate the role of qualitative differences between HS from different origins. The effects of seven different HS on the bioconcentration of pyrene and benzo[ a ]pyrene (B a P) in the nematode Caenorhabditis elegans were related to the spectroscopic and chemical properties of the HS. The effect of each humic material on the bioconcentration of pyrene or B a P was quantified as a “biologically determined” partition coefficient K DOC . We observed significant linear relationships between K DOC and the atomic H/C ratio, the specific absorptivity at 254 nm, the content of aromatic carbons (as determined by 13 C nuclear magnetic resonance spectroscopy, the copper-complexing capacity, the content of phenolic OH groups, and the molecular weight of the HS. There was no discernible relationship of K DOC with the atomic (N + O)/C ratio, an indicator of the polarity of HS. Taken together, our results show that the variability in the effects of HS from different origins could be related to variations in bulk properties of the HS. Parameters describing the aromaticity of the humic materials seemed to be most useful for estimating effects of HS on the bioconcentration of pyrene and B a P.

Environmental Toxicology and Chemistry↗

USGS2021

The Confocal Laser Scanning Microscopy Working Group of the ICCP: Final report 2021

This report summarizes the activities and results of the Confocal Laser Scanning Microscopy (CLSM) working group (WG) of the International Committee for Coal and Organic Petrology (ICCP), from its inception in September, 2015, to the present day (September, 2021). The purpose of this report is to document the history of the working group and to compile and evaluate its results. The CLSM WG examined an immature, organic-rich sample of Kimmeridge Clay, which was characterized via CLSM imaging and spectroscopy. In addition, mechanically polished and broad ion beam (BIB) milled sample preparations were characterized via atomic force microscopy. Highlights of findings from the CLSM WG include: the interpreted presence of Botryococcus; incomplete blocking of laser light from highly reflective materials; surface roughening and surface flattening induced by differential BIB milling dependent on location and scale of measurement; substitution of uranium for iron in sulfides; red-shift of reflectance and auto-fluorescence from below the sample surface; positive alteration from laser-induced photo-oxidation of the sample surface including fluorescence blue-shift; blueshift associated to higher fluorescence intensity regions in amorphous organic matter; need for fluorescence spectroscopy standardization as applied via CLSM; and the suitability of CLSM to predict solid bitumen reflectance via calibration to an extant data set. Due to the inability of WG members to continue participating in a WG format, the CLSM WG is hereby finalized. This report represents the final product of WG activity, with the aim to summarize the information included herein for a future peer-reviewed manuscript.

Final Report↗

USGS2020

Investigating the effects of broad ion beam milling to sedimentary organic matter: Surface flattening or heat-induced aromatization and condensation?

Previous work has proposed transfer of kinetic heat energy from low-energy broad ion beam (BIB) milling causes thermal alteration of sedimentary organic matter, resulting in increases of organic matter reflectance. Whereas, other studies have suggested the organic matter reflectance increase from BIB milling is due to decreased surface roughness. To test if reflectance increases to sedimentary organic matter (vitrinite) caused by BIB milling were related to molecular aromatization and condensation, Raman and Fourier transform infrared (FTIR) spectroscopies were used to evaluate potential compositional changes in the same vitrinite locations pre- and post-BIB milling. The same locations also were examined by atomic force microscopy (AFM) to determine topographic changes caused by BIB milling (as quantified by the areal root-mean-square roughness parameter S q ). Samples consisted of four medium volatile bituminous coals. A non-aggressive BIB milling approach was used with conditions of 5 min, 4 keV, 15°incline, 360° rotation at 25 rpm and 100% focus (1.5 kV discharge; ∼100 μA). This gentle BIB milling caused vitrinite reflectance (VR o ) increases of 12 to 36% of the original values determined optically before milling (average 26% increase). When molecular proxies from FTIR (A- and C-factor, branching ratio) were plotted against each other for the same vitrinite locations pre- and post-milling, mean data points for each sample generally lie within error of a 1:1 line. Likewise, mean Raman thermal proxy [full-width half maximum of G-band (G-FWHM), Raman band separation (RBS) and D1/G band intensity ratio] values were similar for pre- and post-milled locations, also plotting within error of a 1:1 line. AFM confirms the majority (24 of 36) of pre- and post-ion milled surface pairs were smoother (lower S q values) after BIB milling. These results are interpreted to indicate VR o increase induced by the gentle BIB milling conditions used in this study is an effect of decreased diffuse reflectance due to flatter surfaces, causing more photons to reflect directly back to the detector. Little evidence was observed for molecular aromatization and condensation of vitrinite molecules following BIB milling (with the conditions used). The presence of milling-induced artifacts, including differential milling effects dependent on location and the development of self-organized patterned structures, indicate much work remains in standardization of BIB milling before its promulgation as a routine sample preparation technique for organic petrography. These results provide better understanding of anthropogenic-induced changes to geological samples caused by the now widespread adoption of BIB milling as a disruptive innovation in sample preparation.

Fuel↗

USGS2025

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↗