Thermal Indices Innovation Active
Thermal indices innovation focuses on the utilization of correlative microscopy and spectroscopy techniques for innovative approaches to advance the understanding of thermal indices development. These techniques include correlative light and electron microscopy (CLEM), confocal laser scanning microscopy (CLSM), and atomic force microscopy and infrared microscopy (AFM-IR), among others. Use of these instruments can help to differentiate sedimentary organic matter (SOM) types and reveal the spatial evolution of their properties during thermal maturity advancement, allowing for the development and application of innovative instrument tests to measure thermal indices. Thermal indices innovation research has led to pioneering results in organic petrology, including the first applications of AFM-IR, optical photothermal infrared spectroscopy, fluorescence spectroscopy via confocal laser scanning microscopy, integrated correlative light and electron microscopy, and application of cathodoluminescence as a tool to identify organic matter types.
Objectives:
An important control on reservoir permeability and hydrocarbon storage space in shale petroleum systems is an interconnected nano-porosity network. The consensus is that porosity in SOM consequently forms due to increasing thermal maturity and the generation of petroleum from SOM. There are inconsistencies, however, regarding the thermal regime with respect to its preservation in different matrices, its development in different SOM types, and timing of the onset of organic porosity development. The advancement of understanding these inconsistencies requires the ability to differentiate SOM and observe porosity at the nanoscale. Because electron microscopy is unable to differentiate SOM types, CLEM, CLSM, and AFM-IR techniques are used in this research. Prior innovation research focused on these issues yielded pioneering results on hydrocarbon generation and migration fractionation of petroleum, which led to distribution of these advancements at invited international presentations and in an invited synthesis manuscript.
Continuation of these efforts involves three main objectives to advance the understanding of thermal indices development. The first is to use CLEM techniques to document organic porosity development in different thermal regimes and SOM type at a range of scales. Another goal is to better characterize petroleum formation, expulsion, and migration processes at the microscale. The third overarching goal is to continue to innovate applications of correlative microscopy and spectroscopy techniques to characterize physical and chemical properties of SOM across a range of thermal maturities in both naturally and artificially matured sample series.
Listed below are other science projects or tasks associated with this project.
Petrographic Thermal Indices Research
Vitrinite Reflectance Service
Standardization of Petrographic Thermal Indices
Hydrous Pyrolysis and Kerogen Conversion
Listed below are data products associated with this project.
Data from Cretaceous formations of the Babouri-Figuil Sedimentary Basin, northern Cameroon
Evaluation of pore-like features in sedimentary organic matter
Thermal evolution of graptolite and solid bitumen properties at high maturity under natural and artificial conditions
Strain induced molecular heterogeneity in ancient sedimentary organic matter mapped at nanoscales using optical photothermal infrared spectroscopy
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
Atomic Force Microscopy-based Infrared Spectroscopy Data within Immature Eagle Ford Shale at the Nanometer-scale
Nanoscale Molecular Composition of Solid Bitumen from the Eagle Ford Group Across a Natural Thermal Maturity Gradient
Data from Nanoscale Molecular Fractionation of Organic Matter within Unconventional Petroleum Source Beds (2019)
High Microscale Variability in Raman Thermal Maturity Estimates from Shale Organic Matter - Data Release
Listed below are publications associated with this project.
Cathodoluminescence differentiates sedimentary organic matter types
Scanning electron microscopic evaluation of broad ion beam milling effects to sedimentary organic matter: Sputter-induced artifacts or naturally occurring porosity?
Mapping ancient sedimentary organic matter molecular structure at nanoscales using optical photothermal infrared spectroscopy
Relating systematic compositional variability to the textural occurrence of solid bitumen in shales
Evaluating aromatization of solid bitumen generated in the presence and absence of water: Implications for solid bitumen reflectance as a thermal proxy
Characterization of bituminite in Kimmeridge Clay by confocal laser scanning and atomic force microscopy
The Confocal Laser Scanning Microscopy Working Group of the ICCP: Final report 2021
Hydrous pyrolysis of New Albany Shale: A study examining maturation changes and porosity development
Compositional evolution of organic matter in Boquillas Shale across a thermal gradient at the single particle level
Investigating the effects of broad ion beam milling to sedimentary organic matter: Surface flattening or heat-induced aromatization and condensation?
Examination of inertinite within immature Eagle Ford Shale at the nanometer-scale using atomic force microscopy-based infrared spectroscopy
Nanoscale molecular composition of solid bitumen from the Eagle Ford Group across a natural thermal maturity gradient
- Overview
Thermal indices innovation focuses on the utilization of correlative microscopy and spectroscopy techniques for innovative approaches to advance the understanding of thermal indices development. These techniques include correlative light and electron microscopy (CLEM), confocal laser scanning microscopy (CLSM), and atomic force microscopy and infrared microscopy (AFM-IR), among others. Use of these instruments can help to differentiate sedimentary organic matter (SOM) types and reveal the spatial evolution of their properties during thermal maturity advancement, allowing for the development and application of innovative instrument tests to measure thermal indices. Thermal indices innovation research has led to pioneering results in organic petrology, including the first applications of AFM-IR, optical photothermal infrared spectroscopy, fluorescence spectroscopy via confocal laser scanning microscopy, integrated correlative light and electron microscopy, and application of cathodoluminescence as a tool to identify organic matter types.
Objectives:
An important control on reservoir permeability and hydrocarbon storage space in shale petroleum systems is an interconnected nano-porosity network. The consensus is that porosity in SOM consequently forms due to increasing thermal maturity and the generation of petroleum from SOM. There are inconsistencies, however, regarding the thermal regime with respect to its preservation in different matrices, its development in different SOM types, and timing of the onset of organic porosity development. The advancement of understanding these inconsistencies requires the ability to differentiate SOM and observe porosity at the nanoscale. Because electron microscopy is unable to differentiate SOM types, CLEM, CLSM, and AFM-IR techniques are used in this research. Prior innovation research focused on these issues yielded pioneering results on hydrocarbon generation and migration fractionation of petroleum, which led to distribution of these advancements at invited international presentations and in an invited synthesis manuscript.
Continuation of these efforts involves three main objectives to advance the understanding of thermal indices development. The first is to use CLEM techniques to document organic porosity development in different thermal regimes and SOM type at a range of scales. Another goal is to better characterize petroleum formation, expulsion, and migration processes at the microscale. The third overarching goal is to continue to innovate applications of correlative microscopy and spectroscopy techniques to characterize physical and chemical properties of SOM across a range of thermal maturities in both naturally and artificially matured sample series.
- Science
Listed below are other science projects or tasks associated with this project.
Petrographic Thermal Indices Research
A petrographic thermal index is typically an organic matter indicator in sedimentary rocks that allows for estimations of burial temperature. Petrographic thermal indices include the commonly used proxy vitrinite reflectance as well as other approaches such as solid bitumen reflectance, fluorescence, micro-Raman, and micro-Fourier transform infrared (FTIR) spectroscopies. Measurements from these...Vitrinite Reflectance Service
Vitrinite is a maceral group that is derived from the remains of woody material from vascular plants and is composed of the thermally evolved products of lignin and cellulose. A maceral group is a set of organic matter types with similar properties and appearance. Vitrinite reflectance measures the percentage of incident light that is reflected from the surface of vitrinite as calibrated to a...Standardization of Petrographic Thermal Indices
Advent of the shale revolution since about 2005 caused increased demand for reliable petrographic measurements of thermal maturity in shale via vitrinite reflectance, which has long been considered the gold standard approach. The first standardized methodology for vitrinite reflectance measurement in shale became available in 2011. Subsequent interlaboratory studies demonstrated that significant...Hydrous Pyrolysis and Kerogen Conversion
Hydrous pyrolysis (HP) experimentation is a laboratory method used to thermally mature organic-rich sedimentary rocks. It simulates petroleum generation in the closest available analogue to that of a natural system. Artificial maturation of sedimentary organic matter (SOM) to petroleum allows for the examination of its molecular chemistry to address the issue of anomalous reflection measurement... - Data
Listed below are data products associated with this project.
Data from Cretaceous formations of the Babouri-Figuil Sedimentary Basin, northern Cameroon
This study contains TOC and programmed pyrolysis data, as well as vitrinite reflectance collected from 12 samples taken from the Babouri-Figuil Sedimentary basin in northern Cameroon.Evaluation of pore-like features in sedimentary organic matter
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 flaThermal evolution of graptolite and solid bitumen properties at high maturity under natural and artificial conditions
To refine the use of graptolite and solid bitumen properties as thermal proxies at overmature conditions, we evaluated their evolution via Raman and infrared spectroscopies, reflectance, and geochemical screening in high-temperature hydrous and anhydrous experiments in comparison to naturally matured samples. Naturally matured samples included four overmature Wufeng-Longmaxi marine shales from theStrain induced molecular heterogeneity in ancient sedimentary organic matter mapped at nanoscales using optical photothermal infrared spectroscopy
Here we report ultra-high resolution infrared mapping of organic matter functional group distribution in Tasmanites (algal microfossils) from the Upper Devonian Ohio Shale using optical photothermal infrared spectroscopy (O-PTIR). O-PTIR is capable of rapidly measuring the vibrational response of samples in situ with ~500-nm spatial resolution, well below the infrared diffraction limit. Our resultTextural occurrence and organic porosity of solid bitumen in shales
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. %] NewOrganic petrology of Cretaceous Mowry and Niobrara source-rock reservoirs, Powder River Basin, Wyoming, USA
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 electrAtomic Force Microscopy-based Infrared Spectroscopy Data within Immature Eagle Ford Shale at the Nanometer-scale
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, suNanoscale Molecular Composition of Solid Bitumen from the Eagle Ford Group Across a Natural Thermal Maturity Gradient
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 thermalData from Nanoscale Molecular Fractionation of Organic Matter within Unconventional Petroleum Source Beds (2019)
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 are typically invoked to explain this behavior. Given the current emphasis on unconventional (continuous) resources, there is a neHigh Microscale Variability in Raman Thermal Maturity Estimates from Shale Organic Matter - Data Release
Here the spatial variation in Raman estimates of thermal maturity within individual organic domains from several shale geologic reference materials originating from the Boquillas, Marcellus, Niobrara, and Woodford Formations are assessed from the respective Raman response. We show that for all four shales the thermal maturity parameters extracted from Raman spectra by iterative peak fitting can va - Publications
Listed below are publications associated with this project.
Filter Total Items: 24Cathodoluminescence differentiates sedimentary organic matter types
High-resolution scanning electron microscopy (SEM) visualization of sedimentary organic matter is widely utilized in the geosciences for evaluating microscale rock properties relevant to depositional environment, diagenesis, and the processes of fluid generation, transport, and storage. However, despite thousands of studies which have incorporated SEM methods, the inability of SEM to differentiateAuthorsPaul C. Hackley, Ryan J. McAleer, Aaron M. Jubb, Brett J. Valentine, Justin E. BirdwellScanning electron microscopic evaluation of broad ion beam milling effects to sedimentary organic matter: Sputter-induced artifacts or naturally occurring porosity?
Research examining organic-matter hosted porosity has significantly increased during the last decade due to greater focus on understanding hydrocarbon migration and storage in source-rock reservoirs, and technological advances in scanning electron microscopy (SEM) capabilities. The examination of nanometer-scale organic-matter hosted porosity by SEM requires the preparation of exceptionally flat gAuthorsBrett J. Valentine, Paul C. HackleyMapping ancient sedimentary organic matter molecular structure at nanoscales using optical photothermal infrared spectroscopy
Elucidating the molecular structure of sedimentary organic matter (SOM) is key to understanding petroleum generation processes, as well as ancient sedimentary environments. SOM structure is primarily controlled by biogenic source material (e.g., marine vs. terrigenous), depositional conditions, and subsurface thermal history. Additional factors, e.g., strain, may also impact the molecular structurAuthorsAaron M. Jubb, Martha (Rebecca) Stokes, Ryan J. McAleer, Paul C. Hackley, Eoghan Dillion, Jing QuRelating systematic compositional variability to the textural occurrence of solid bitumen in shales
This study presents Raman spectroscopic data paired with scanning electron microscopy (SEM) images to assess solid bitumen composition 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 sampleAuthorsMartha (Rebecca) Stokes, Brett J. Valentine, Aaron M. Jubb, Paul C. HackleyEvaluating aromatization of solid bitumen generated in the presence and absence of water: Implications for solid bitumen reflectance as a thermal proxy
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 hydrogen from water, organic-rich (22 wt% total organic carbon, TOC) mudrock samples from the Eocene lacAuthorsPaul C. Hackley, Aaron M. Jubb, Patrick L. Smith, Ryan J. McAleer, Brett J. Valentine, Javin J. Hatcherian, Palma J. Botterell, Justin E. BirdwellCharacterization of bituminite in Kimmeridge Clay by confocal laser scanning and atomic force microscopy
This work investigates bituminite (amorphous sedimentary organic matter) in Upper Jurassic Kimmeridge Clay source rock via confocal laser scanning microscopy (CLSM) and atomic force microscopy (AFM). These petrographic tools were used to provide better understanding of the nature of bituminite, which has been historically difficult to identify and differentiate from similar organic matter types inAuthorsPaul C. Hackley, Jolanta Kus, João Graciano Mendonça Filho, Andrew D. Czaja, Angeles G. Borrego, Dragana Životić, Brett J. Valentine, Javin J. HatcherianThe 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 examineAuthorsPaul C. Hackley, Jolanta Kus, João Graciano Mendonça Filho, Andrew D. Czaja, Angeles Borrego, Dragana ŽivotićHydrous pyrolysis of New Albany Shale: A study examining maturation changes and porosity development
The characterization of nanoscale organic structures has improved our understanding of porosity development within source-rock reservoirs, but research linking organic porosity evolution to thermal maturity has generated conflicting results. To better understand this connection, an immature (0.25% solid bitumen reflectance; BRo) sample of the New Albany Shale was used in four isothermal hydrous pyAuthorsBrett J. Valentine, Paul C. Hackley, Javin J. HatcherianCompositional evolution of organic matter in Boquillas Shale across a thermal gradient at the single particle level
The molecular composition of petroliferous organic matter and its compositional evolution throughout thermal maturation provides insight for understanding petroleum generation. This information is critical for understanding hydrocarbon resources in unconventional reservoirs, as source rock organic matter is highly dispersed, in contact with the surrounding mineral matrix, and may occur as multipleAuthorsJustin E. Birdwell, Aaron M. Jubb, Paul C. Hackley, Javin J. HatcherianInvestigating 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 orgAuthorsPaul C. Hackley, Aaron M. Jubb, Brett J. Valentine, Javin J. Hatcherian, Jing-Jiang Yu, William K. PodrazkyExamination 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 catagenesAuthorsAaron M. Jubb, Paul C. Hackley, Justin E. Birdwell, Javin J. Hatcherian, Jing QuNanoscale 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 therAuthorsAaron M. Jubb, Justin E. Birdwell, Paul C. Hackley, Javin J. Hatcherian, Jing Qu