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To test if reflectance increases to sedimentary organic matter (vitrinite) caused by broad ion beam (BIB) milling were related to molecular aromatization and condensation, we used Raman and Fourier transform infrared (FTIR) spectroscopies 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 expressed by the areal root-mean-square roughness parameter Rq). Samples consisted of four medium volatile bituminous coals. We used a non-aggressive BIB milling approach with conditions of [(5 min, 4 keV, 15°incline, 360° rotation at 25 rpm and 100%...
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Solid organic matter (OM) in sedimentary rocks produces petroleum and solid bitumen when it undergoes thermal maturation. The solid OM is a 'geomacromolecule', usually representing a mixture of various organisms with distinct biogenic origins, and can have high heterogeneity in composition. Programmed pyrolysis is a common conventional method to reveal bulk geochemical characteristics of the dominant OM while detailed organic petrography is required to reveal information about the biogenic origin of contributing macerals. Despite advantages of programmed pyrolysis, it cannot provide information about the heterogeneity of chemical compositions present in the individual OM types. Therefore, other analytical techniques...
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The refractory nature of zircon to temperature and pressure allows even a single zircon grain to preserve a rich history of magmatic, metamorphic, and hydrothermal processes. Isotopic dating of micro-domains exposed in cross-sections of zircon grains allows us to interrogate this history. Unfortunately, our ability to select the zircon grains in a heavy mineral concentrate that records the most geochronologic information is limited by our inability to predict internal zonation from observations of whole zircon grains. Here we document the use of a petrographic microscope to observe and image the photoluminescence (PL) response of whole zircon grains excited under ultraviolet (UV) light, and the utility of this PL...
Geological models for petroleum generation suggest thermal conversion of oil-prone sedimentary organic matter in the presence of water promotes increased liquid saturate yield, whereas absence of water causes formation of an aromatic, cross-linked solid bitumen residue. To test the influence of exchangeable hydrogen from water, organic-rich (22 wt.% total organic carbon, TOC) mudrock samples from the Eocene lacustrine Green River Mahogany zone oil shale were pyrolyzed under hydrous and anhydrous conditions at temperatures between 300 and 370°C for 72 hrs. Petrographic approaches including optical microscopy, reflectance, Raman spectroscopy, and scanning electron and transmission electron microscopy, supplemented...
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This data release contains reflectance measurements for eight samples submitted to the USGS Organic Petrology Laboratory in Reston. Samples include two artificial rock samples made from cement with organic matter added (samples 001-002), a coal and shale sample (samples 003-004, respectively), and hydrous pyrolysis residues for samples 001-004. The hydrous pyrolysis experiments were conducted at 330°C for 72 hours at the United States Geological Survey's (USGS) Denver Federal Center. Samples were mounted into 1-inch circular briquettes in USGS-Reston according to ASTM D2797 for organic petrographic analysis. Cement plugs (samples 001-002, and pyrolysis residues 005-006) were crushed to approximately 1 mm top-size...
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This study presents Raman spectroscopic data paired with scanning electron microscopy (SEM) to assess solid bitumen composition and porosity development as a function of solid bitumen texture and association with minerals. A series of hydrous pyrolysis experiments (1-103 days, 300-370°C) using a low maturity (0.25% solid bitumen reflectance, BRo), high total organic carbon [(TOC), 14.0 wt. %] New Albany Shale sample as the starting material yielded pyrolysis residues designed to evaluate the evolution of TOC, solid bitumen aromaticity, and organic porosity development with increasing temperature and heating duration. Solid bitumen was analyzed by Raman spectroscopy wherein point data was collected from accumulations...
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Research examining organic-matter hosted porosity has significantly increased during the last ten years 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. But like with any sample preparation technique,...
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For nearly two and a half decades following World War II, production wastes from the world’s largest manufacturer of technical DDT were discharged into sewers of Los Angeles County. Following treatment, the wastes were released via a submarine outfall system to nearshore coastal waters where a portion accumulated in shallow sediments of the Palos Verdes Shelf (PVS). An investigation of the pore-water geochemistry of DDT-related compounds (DDX) was undertaken in an effort to understand factors controlling the rate of reductive dechlorination (RDC) of the major DDT degradate, 4,4’-DDE. Equilibrium matrix-solid phase microextraction (matrix-SPMEeq) combined with automated thermal desorption-gas chromatography/mass...
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Recent production of light sweet oil from shallow (~2,000 ft) horizontal wells in the Upper Devonian Berea Sandstone of eastern Kentucky and historical oil production from conventional wells in the Berea of adjoining southern Ohio has prompted re-evaluation of Devonian petroleum systems in the central Appalachian Basin. Herein, we examined Upper Devonian Ohio Shale (lower Huron Member) and Middle Devonian Marcellus Shale organic-rich source rocks from eastern Ohio and nearby areas using organic petrography and geochemical analyses of solvent extracts. The data indicate the organic matter in the Ohio and Marcellus Shales was primarily derived from marine algae and its degradation products including bacterial biomass....
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For sample mounting, organic petrology laboratories typically use cold-setting epoxy-resin (e.g., 40°C, used by Oklahoma Geological Survey, OGS) or heat-setting plastic (e.g., 180°C, used by U.S. Geological Survey, USGS). Previous workers have suggested a systematic vitrinite reflectance (VRo) increase was associated with the thermoplastic preparation process, relative to epoxy mounting, which was attributed to moisture loss from the transient high temperatures of plastic mounting. In this study, we evaluated thermal effects to low maturity organic matter from transient exposure to elevated temperatures. A subbituminous coal sample was subjected to long-term (4 to 38 weeks) exposure to temperatures of 85 to 120°C...
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As part of a larger study, organic petrographic features of Leonardian Wolfcamp A repetitive siliceous and calcareous mudrock and fine-grained carbonate lithofacies cycles occurring in the R. Ricker #1 core from Reagan County, Midland Basin, Texas were evaluated. The objectives of the petrographic investigation were to estimate thermal maturity, identify organic matter types and abundances, and identify the presence or absence of migrated hydrocarbons. An integrated analytical program included geochemical screening [total organic carbon (TOC) content by LECO, programmed pyrolysis by HAWK, including from solvent-extracted samples], X-ray diffraction mineralogy, organic petrography, SEM-EDS including correlative light...
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The U.S. Geological Survey assessed undiscovered unconventional hydrocarbon resources reservoired in the Upper Cretaceous Tuscaloosa marine shale (TMS) of southern Mississippi and adjacent Louisiana in 2018. As part of the assessment, oil- source rock correlations were examined in the study area where operators produce light (38-45° API), sweet oil from horizontal, hydraulically-fractured wells in an overpressured ‘high-resistivity’ (>5 ohm-m) zone (HRZ) at the base of the TMS. Our initial characterization of TMS samples indicated overall low organic carbon (avg. TOC ~1.0%) and dominance of a gas-prone Type III or mixed Type II/III kerogen, potentially inconsistent with a self-sourced petroleum system model for...
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This data release contains the boundaries of assessment units and input data for the assessment of undiscovered continuous oil and gas in the Upper Cretaceous Tuscaloosa Marine shale of the U.S. Gulf Coast. The Assessment Unit is the fundamental unit used in the National Assessment Project for the assessment of undiscovered oil and gas resources. The Assessment Unit is defined within the context of the higher-level Total Petroleum System. The Assessment Unit is shown herein as a geographic boundary interpreted, defined, and mapped by the geologist responsible for the province and incorporates a set of known or postulated oil and (or) gas accumulations sharing similar geologic, geographic, and temporal properties...
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Pollen morphology and pollen morphology in conjunction with other characteristics have elucidated the origin and evolution of various plant groups. Many studies of fossil pollen rarely discuss the effects of diagenesis and sample preparation on pollen characteristics. This paper examines the relationship of diagenesis, sample preparation (e.g., acetolysis), and staining techniques on the preservation and interpretation of pollen characteristics viewed with light, scanning and transmission electron microscopy. Based on empirical studies, different species under similar experimental conditions have different reflectance values, indicating the individual species respond differently to diagenetic events. The quantitative...
The nanoscale molecular composition of kerogen is a challenging parameter to characterize given the chemical and structural complexity exhibited by this important biopolymer. However, kerogen composition will strongly impact its reactivity and so is a critical parameter to understand petroleum generation processes during kerogen 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 to be elucidated at spatial resolutions at or below 50 nm. Here we apply AFM-IR to examine inertinite, an important kerogen maceral type, from an immature Eagle Ford Shale sample. Our data show...
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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 shale reservoir properties including porosity, permeability, and hydrocarbon generation and storage, amongst 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...
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Fluorescence spectroscopy via confocal laser scanning microscopy (CLSM) was used to analyze ancient sedimentary organic matter, including Tasmanites microfossils in Devonian shale and Gloecapsomorpha prisca (G. prisca) in Ordovician kukersite from North American basins. We examined fluorescence emission as a function of excitation laser wavelength, sample orientation, and with respect to location within individual organic entities and along organic matter chemical transects. Results from spectral scans of the same field of view in Tasmanites with different laser lines showed progressive red-shift in emission maxima with longer excitation wavelengths. This result indicates steady-state Tasmanites fluorescence emission...
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The dataset covers X-ray diffraction (XRD) applied for mineral determination in shales from the Utica, Excello, Niobrara, and Monterey formations. The XRD was performed prior to modified Rock-Eval pyrolysis, reflectance, organic petrology, and Fourier-transform infrared spectroscopy (FTIR) being employed to analyze geochemical properties; gas adsorption (CO2 and N2) was used to characterize pore structures.
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Imaging of Niobrara Formation and Mowry Shale samples from a range of thermal maturities provided observations and data on pore systems, organic matter (OM) types and associations with mineralogy and fabric, wettability, and microporosity associated with both diagenetic and detrital clays. Imaging techniques included scanning electron microscopy, organic petrography and correlative scanning electron microscopy, and mapping of mineralogy through energy dispersive spectroscopy.
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The dataset covers Attenuated Total Reflectance (ATR) measurements taken from altered kerogen in shales from the Woodford formation. The ATR measurements were taken after the samples were run through supercritical CO2 alteration experiments in a brine solution.


map background search result map search result map DDT and Related Compounds in Pore Water of Shallow Sediments on the Palos Verdes Shelf, CA Data release for Organic geochemistry and petrology of Devonian shale in eastern Ohio: implications for petroleum systems assessment (2018) Analyzing Heterogeneity in Artificially Matured Samples of Bakken Shales (2018) Organic Petrography and Diagenesis of Leonardian Mudrocks and Carbonates, Midland Basin, Texas (2018) XRD data from study on the impact of thermal maturity on shale microstructures using hydrous pyrolysis (2018) USGS Gulf Coast Petroleum Systems and National and Global Oil and Gas Assessment Projects-Louisiana-Mississippi Salt Basins and Western Gulf Provinces, Upper Cretaceous Tuscaloosa Marine Shale Assessment Unit Boundaries and Assessment Input Data Forms ATR data from interaction of kerogen with brine-saturated supercritical carbon dioxide (CO2) and its implications to geologic carbon sequestration and enhanced oil/gas recovery (2018) Oil-source rock correlation studies in the unconventional Upper Cretaceous Tuscaloosa marine shale petroleum system, Mississippi and Louisiana, USA (2019) Sample mounting for organic petrology: no thermal effects from transient exposure to elevated temperatures (2019) Fluorescence spectroscopy of ancient sedimentary organic matter via confocal laser scanning microscopy (CLSM) Investigating the effects of broad ion beam milling to sedimentary organic matter Nanoscale Molecular Composition of Solid Bitumen from the Eagle Ford Group Across a Natural Thermal Maturity Gradient Atomic Force Microscopy-based Infrared Spectroscopy Data within Immature Eagle Ford Shale at the Nanometer-scale Photoluminescence Imaging of Whole Zircon Grains on a Petrographic Microscope—An Underused Aide for Geochronologic Studies TOC, Reflectance and Raman Data from Eocene Green River Mahogany zone Reflectance and spectral fluorescence data from the effect of diagenesis on the preservation of morphology and ultrastructural features of pollen Textural occurrence and organic porosity of solid bitumen in shales Organic petrology of Cretaceous Mowry and Niobrara source-rock reservoirs, Powder River Basin, Wyoming, USA Reflectance measurements for eight samples submitted to the USGS Organic Petrology Laboratory in Reston Evaluation of pore-like features in sedimentary organic matter Organic Petrography and Diagenesis of Leonardian Mudrocks and Carbonates, Midland Basin, Texas (2018) DDT and Related Compounds in Pore Water of Shallow Sediments on the Palos Verdes Shelf, CA Oil-source rock correlation studies in the unconventional Upper Cretaceous Tuscaloosa marine shale petroleum system, Mississippi and Louisiana, USA (2019) TOC, Reflectance and Raman Data from Eocene Green River Mahogany zone ATR data from interaction of kerogen with brine-saturated supercritical carbon dioxide (CO2) and its implications to geologic carbon sequestration and enhanced oil/gas recovery (2018) Data release for Organic geochemistry and petrology of Devonian shale in eastern Ohio: implications for petroleum systems assessment (2018) Textural occurrence and organic porosity of solid bitumen in shales Reflectance measurements for eight samples submitted to the USGS Organic Petrology Laboratory in Reston USGS Gulf Coast Petroleum Systems and National and Global Oil and Gas Assessment Projects-Louisiana-Mississippi Salt Basins and Western Gulf Provinces, Upper Cretaceous Tuscaloosa Marine Shale Assessment Unit Boundaries and Assessment Input Data Forms Atomic Force Microscopy-based Infrared Spectroscopy Data within Immature Eagle Ford Shale at the Nanometer-scale Analyzing Heterogeneity in Artificially Matured Samples of Bakken Shales (2018) Organic petrology of Cretaceous Mowry and Niobrara source-rock reservoirs, Powder River Basin, Wyoming, USA Investigating the effects of broad ion beam milling to sedimentary organic matter Photoluminescence Imaging of Whole Zircon Grains on a Petrographic Microscope—An Underused Aide for Geochronologic Studies Fluorescence spectroscopy of ancient sedimentary organic matter via confocal laser scanning microscopy (CLSM) XRD data from study on the impact of thermal maturity on shale microstructures using hydrous pyrolysis (2018) Evaluation of pore-like features in sedimentary organic matter Sample mounting for organic petrology: no thermal effects from transient exposure to elevated temperatures (2019) Reflectance and spectral fluorescence data from the effect of diagenesis on the preservation of morphology and ultrastructural features of pollen