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USGS2006

Major- and Trace-Element Concentrations in Rock Samples Collected in 2005 from the Taylor Mountains 1:250,000-scale Quadrangle, Alaska

The data consist of major- and minor-element concentrations for rock samples collected during 2005 by the U.S. Geological Survey. Samples were analyzed by fire assay (Au, Pd, Pt), cold vapor atomic absorption spectroscopy (Hg), and the inductively coupled plasma mass spectrometry (ICPMS) 10 and 42 element methods. For details of sample preparation and analytical techniques see USGS Open File Report 02-0223 (Analytical methods for chemical analysis of geologic and other materials, U.S. Geological Survey), available at .

Open-File Report↗

USGS2007

Determination of total mercury in whole-body fish and fish muscle plugs collected from the South Fork of the Humboldt River, Nevada, September 2005

This report presents the results of a study by the U.S. Geological Survey, done in cooperation with the U.S. Bureau of Reclamation, to determine mercury concentrations in whole-body fish and fish muscle plugs from the South Fork of the Humboldt River near Elko in the Te-Moak Indian Reservation. A single muscle plug was collected from beneath the dorsal fin area in each of the three whole-body fish samples. After homogenization and lyophilization of the muscle plugs and whole-body fish samples, mercury concentrations were determined with a direct mercury analyzer utilizing the process of thermal combustion-gold amalgamation atomic absorption spectroscopy. Mercury concentrations in whole-body fish ranged from 0.048 to 0.061 microgram per gram wet weight, and 0.061 to 0.082 microgram per gram wet weight in muscle plugs. All sample mercury concentrations were well below the U.S. Environmental Protection Agency's fish consumption advisory of 0.30 microgram per gram wet weight.

Open-File Report↗

USGS2007

Determination of total mercury in fillets of sport fishes collected from Folsom and New Melones Reservoirs, California, 2004

This report presents the results of a study by the U.S. Geological Survey, done in cooperation with the U.S. Bureau of Reclamation, to determine mercury concentrations in selected sport fishes from Folsom and New Melones Reservoirs in California. Fillets were collected from each fish sample, and after homogenization and lyophilization of fish fillets, mercury concentrations were determined with a direct mercury analyzer utilizing the process of thermal combustion-gold amalgamation atomic absorption spectroscopy. Mercury concentrations in fish fillets from Folsom Reservoir ranged from 0.09 to 1.16 micrograms per gram wet weight, and from New Melones Reservoir ranged from 0.03 to 0.94 microgram per gram wet weight. Most of the fish fillets from Folsom Reservoir (87 percent) and 27 percent of the fillets from New Melones Reservoir exceeded the U.S. Environmental Protection Agency's fish consumption advisory of 0.30 microgram per gram wet weight.

Open-File Report↗

USGS2007

Determination of total mercury in fillets of sport fishes collected from Folsom Reservoir, California, 2006

This report presents the results of a study by the U.S. Geological Survey, done in cooperation with the U.S. Bureau of Reclamation, to determine mercury concentrations in selected sport fishes from Folsom Reservoir in California. Fillets were collected from each fish sample, and after homogenization and lyophilization of fish fillets, mercury concentrations were determined with a direct mercury analyzer utilizing the process of thermal combustion-gold amalgamation atomic absorption spectroscopy. Mercury concentrations in fillets ranged from 0.031 to 0.20 micrograms per gram wet weight in rainbow trout (Oncorhynchus mykiss) samples and 0.071 to 0.16 micrograms per gram wet weight in bluegill (Lepomis macrochirus) samples. Mercury concentration was 0.98 microgram per gram wet weight in a single spotted bass (Micropterus punctulatus) sample, which was the only one in the sample set which exceeded the U.S. Environmental Protection Agency's fish consumption advisory of 0.30 microgram per gram wet weight.

Open-File Report↗

USGS2008

Chemical data for precipitate samples

During studies of sulfide oxidation in coastal areas of Prince William Sound in 2005, precipitate samples were collected from onshore and intertidal locations near the Ellamar, Threeman, and Beatson mine sites (chapter A, fig. 1; table 7). The precipitates include jarosite and amorphous Fe oxyhydroxide from Ellamar, amorphous Fe oxyhydroxide from Threeman, and amorphous Fe oxyhydroxide, ferrihydrite, and schwertmannite from Beatson. Precipitates occurring in the form of loose, flocculant coatings were harvested using a syringe and concentrated in the field by repetitive decanting. Thicker accumulations were either scraped gently from rocks using a stainless steel spatula or were scooped directly into receptacles (polyethylene jars or plastic heavy-duty zippered bags). Most precipitate samples contain small amounts of sedimentary detritus. With three jarosite-bearing samples from Ellamar, an attempt was made to separate the precipitate from the heavy-mineral fraction of the sediment. In this procedure, the sample was stirred in a graduated cylinder containing deionized water. The jarosite-rich suspension was decanted onto analytical filter paper and air dried before analysis. Eleven precipitate samples from the three mine sites were analyzed in laboratories of the U.S. Geological Survey (USGS) in Denver, Colorado (table 8). Major and trace elements were determined by inductively coupled plasma-mass spectrometry following multiacid (HCl-HNO3-HClO4-HF) digestion (Briggs and Meier, 2002), except for mercury, which was analyzed by cold-vapor atomic absorption spectroscopy (Brown and others, 2002a). X-ray diffraction (XRD) analyses were performed on powdered samples (<200 mesh) by S. Sutley of the USGS. Additional details regarding sample preparation and detection limits are found in Taggert (2002). Discussions of the precipitate chemistry and associated microbial communities are presented in Koski and others (2008) and Foster and others (2008), respectively.

Alaska↗

USGS2012

Concentrations of mercury and other metals in black bass (Micropterus spp.) from Whiskeytown Lake, Shasta County, California, 2005

This report presents the results of a reconnaissance study conducted by the U.S. Geological Survey (USGS) to determine mercury (Hg) and other selected metal concentrations in Black bass ( Micropterus spp. ) from Whiskeytown Lake, Shasta County, California. Total mercury concentrations were determined by cold-vapor atomic absorption spectroscopy (CVAAS) in fillets and whole bodies of each sampled fish. Selected metals scans were performed on whole bodies (less the fillets) by inductively coupled plasma–mass spectroscopy (ICP-MS) and inductively coupled plasma–optical emission spectroscopy (ICP-OES). Mercury concentrations in fillet samples ranged from 0.06 to 0.52 micrograms per gram (μg/g) wet weight (ww). Total mercury (HgT) in the same fish whole-body samples ranged from 0.04 to 0.37 (μg/g, ww). Mercury concentrations in 17 percent of "legal catch size" (≥305 millimeters in length) were above the U.S. Environmental Protection Agency water-quality criterion for the protection of human health of 0.30 μg/g (ww). These data will serve as a baseline for future monitoring efforts within Whiskeytown Lake.

California↗

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↗

USGS2015

Database creation, data quality assessment, and geochemical maps (phase V, deliverable 59)—Final report on compilation and validation of geochemical data

Under the World Bank-funded Second Projet de Renforcement Institutionnel du Secteur Minier de la Republique Islamique de Mauritanie (PRISM-II), this Phase V geochemistry report follows earlier Phase I and Phase II summary reports on geochemical data (U.S. Geological Survey, 2007 and Eppinger, 2007; respectively). All the reports are based on evaluations of geochemical data collected in 1999-2004 under an earlier World Bank program (PRISM-I) by the British Geological Survey (BGS) and the Bureau de Recherches Géologiques et Minières (BRGM) for the Government of Mauritania. There are no associated Phase III or IV reports. The geochemical sample media collected by the BGS and BRGM under the PRISM-I contract included rock, sediment, regolith, and soil samples. Details on sample collection procedures are in unpublished reports available from PRISM. These samples were analyzed under PRISM-I contract by ALS Chemex Laboratories using various combinations of modern methods including fire-assay inductively coupled plasma-atomic emission spectrometry (ICPAES) and ICP-mass spectrometry (ICP-MS) for Au; multi-acid digestion, atomic absorption spectroscopy (AAS) for Ag and As; 47-element, four-acid digestion, ICP-MS; 27-element, fouracid digestion, ICP-AES; special four-acid ICP-MS techniques for Pt and B; fire assay followed by ICP-AES for platinum-group elements; whole-rock analyses by wavelength dispersive X-ray fluorescence (XRF); special techniques for loss-on-ignition, inorganic C, and total S; and special ore-grade AAS techniques for Ag, Au, Cu, Ni, Pb, and Zn. Around 30,000 samples were analyzed by at least one technique. However, it is stressed here that: (1) there was no common sample medium collected at all sites, likely due to the vast geological and geomorphologic differences across the country, (2) the sample site distribution is very irregular, likely due in part to access constraints and sand dune cover, and (3) there was no common across-the-board trace element analytical package used for all samples. These three aspects fundamentally affect the ability to produce country-wide geochemical maps of Mauritania. Gold (Au), silver (Ag), and arsenic (As) were the three elements that were most commonly analyzed.

Open-File Report↗

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

The CETAC ADX-500 Autodiluter System: A Study of Dilution Performance with the ELAN 6000 ICP-MS and ELAN Software

The CETAC ADX-500 autodiluter system was tested with ELAN?? v 2.1 software and the ELAN 6000 ICP-MS instrument to determine on-line automated dilution performance during analysis of standard solutions containing nine analytes representative of the mass spectral range (mass 9 to mass 238). Two or more dilution schemes were tested for each of 5 test tube designs. Dilution performance was determined by comparison of analyte concentration means of diluted and non-diluted standards. Accurate dilutions resulted with one syringe pump addition of diluent in small diameter round-bottomed (13 mm OD) or conical-tipped (18 mm OD) tubes and one or more syringe pump additions in large diameter (28 mm OD) conical-tipped tubes. Inadequate dilution mixing which produced high analyte concentration means was observed for all dilutions conducted in flat-bottomed tubes, and for dilutions requiring multiple syringe additions of diluent in small diameter round-bottomed and conical tipped tubes. Effective mixing of diluted solutions was found to depend largely upon tube diameter and liquid depth: smaller tube diameters and greater liquid depth resulted in ineffective mixing, whereas greater tube diameter and shallower liquid depth facilitated effective mixing. Two design changes for the autodiluter were suggested that would allow effective mixing to occur using any dilution scheme and tube design.

Atomic Spectroscopy↗

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↗