Advent of the ‘shale revolution’ since about 2005 has caused increased demand for reliable petrographic measurements of thermal maturity in shale via vitrinite reflectance, long considered the ‘gold standard’ approach. A standardized methodology for organic reflectance measurement in shale first became available in 2011 (ASTM D7708), based on prior work by task members. However, interlaboratory studies to test reproducibility in vitrinite reflectance measurements demonstrate significant work remains to be done in improving accuracy and precision. Work in this task also examines sample effects caused by preparation technique, e.g., mounting medium (thermoplastic vs. epoxy resin) or polishing method (broad ion beam milling vs. mechanical polish). Standardization efforts in this task were recognized by bestowment of the 2019 Organic Petrology Award from external organization International Committee for Coal and Organic Petrology (ICCP).
Objective:
Improve standardization and reliability of petrographic measurements of thermal maturity including organic reflectance and fluorescence.
Methodology:
Past efforts in this task have established criteria for the identification and distinction of vitrinite and solid bitumens and have codified a technique for their reflectance measurement when dispersed in sedimentary rocks. Testing and methodology improvement is accomplished through interlaboratory studies (ILS) on well-characterized shale samples of different thermal maturity, organic richness and organic matter type abundance. These collaborative studies help to determine best practices, establish repeatability and reproducibility statistics, and promulgate the most successful approaches. The interlaboratory study approach occurs via participation from members of the International Committee for Coal and Organic Petrology (ICCP), the Society for Organic Petrology (TSOP), and through cooperation with the American Society for Testing and Materials (ASTM). The Reston Organic Petrology Laboratory supports this research via project coordination, sample preparation, vitrinite reflectance, fluorescence, quantitative organic petrography assessment, and transmitted light petrography.
Below are other science projects associated with this project task.
Photomicrograph Atlas
Vitrinite Reflectance Service
Thermal Indices Innovation
Hydrous Pyrolysis and Kerogen Conversion
Below are publications associated with this project task.
Investigating the effects of broad ion beam milling to sedimentary organic matter: Surface flattening or heat-induced aromatization and condensation?
Sample mounting for organic petrology: No thermal effects from transient exposure to elevated temperatures
Testing reproducibility of vitrinite and solid bitumen reflectance measurements in North American unconventional source-rock reservoir petroleum systems
Reflectance increase from broad beam ion milling of coals and organic-rich shales due to increased surface flatness
- Overview
Advent of the ‘shale revolution’ since about 2005 has caused increased demand for reliable petrographic measurements of thermal maturity in shale via vitrinite reflectance, long considered the ‘gold standard’ approach. A standardized methodology for organic reflectance measurement in shale first became available in 2011 (ASTM D7708), based on prior work by task members. However, interlaboratory studies to test reproducibility in vitrinite reflectance measurements demonstrate significant work remains to be done in improving accuracy and precision. Work in this task also examines sample effects caused by preparation technique, e.g., mounting medium (thermoplastic vs. epoxy resin) or polishing method (broad ion beam milling vs. mechanical polish). Standardization efforts in this task were recognized by bestowment of the 2019 Organic Petrology Award from external organization International Committee for Coal and Organic Petrology (ICCP).
Objective:
Improve standardization and reliability of petrographic measurements of thermal maturity including organic reflectance and fluorescence.
Methodology:
Past efforts in this task have established criteria for the identification and distinction of vitrinite and solid bitumens and have codified a technique for their reflectance measurement when dispersed in sedimentary rocks. Testing and methodology improvement is accomplished through interlaboratory studies (ILS) on well-characterized shale samples of different thermal maturity, organic richness and organic matter type abundance. These collaborative studies help to determine best practices, establish repeatability and reproducibility statistics, and promulgate the most successful approaches. The interlaboratory study approach occurs via participation from members of the International Committee for Coal and Organic Petrology (ICCP), the Society for Organic Petrology (TSOP), and through cooperation with the American Society for Testing and Materials (ASTM). The Reston Organic Petrology Laboratory supports this research via project coordination, sample preparation, vitrinite reflectance, fluorescence, quantitative organic petrography assessment, and transmitted light petrography.
- Science
Below are other science projects associated with this project task.
Photomicrograph Atlas
The Photomicrograph Atlas provides a basic tutorial in the nomenclature of organic materials as they occur in sedimentary rocks such as coal and shale, information on the taxonomies used by various groups and organizations, and a database of images related to the characterization of fossil fuel resources in the United States and the world.Vitrinite Reflectance Service
Vitrinite reflectance is regarded as the gold standard thermal maturity parameter and vitrinite reflectance data is needed for energy resource assessment and other types of basin analysis studies. This effort provides vitrinite reflectance and qualitative organic petrography of shale, mudrock, coal and other unconventional reservoir samples as a routine in-house service, from the Organic Petrology...Thermal Indices Innovation
Thermal indices innovation utilizes correlative microscopy techniques for innovative approaches to thermal indices development, including confocal laser scanning microscopy (CLSM), AFM-IR (combined atomic force and infrared microscopy), atomic force microscopy (AFM), and SEM of Argon ion-milled sample surfaces combined with traditional organic petrography. The innovation task also is testing...Hydrous Pyrolysis and Kerogen Conversion
This work is directed at understanding the kinetics of vitrinite and solid bitumen maturation through hydrous pyrolysis experiments, potentially enabling a direct methodology to detect ‘vitrinite reflectance suppression,’ a commonly reported problem in the early- to mid-oil window. This task also examines the molecular chemistry of kerogen conversion to petroleum via in situ chemical probing by... - Publications
Below are publications associated with this project task.
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 orgSample mounting for organic petrology: No thermal effects from transient exposure to elevated temperatures
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 thermoplastic (e.g., 180 °C, used by U.S. Geological Survey, USGS). Previous workers have suggested a systematic huminite/vitrinite reflectance (VRo) increase was associated with the thermoplastic preparation process, relative to epoxy moTesting reproducibility of vitrinite and solid bitumen reflectance measurements in North American unconventional source-rock reservoir petroleum systems
An interlaboratory study (ILS) was conducted to test reproducibility of vitrinite and solid bitumen reflectance measurements in six mudrock samples from United States unconventional source-rock reservoir petroleum systems. Samples selected from the Marcellus, Haynesville, Eagle Ford, Barnett, Bakken and Woodford are representative of resource plays currently under exploitation in North America. AlReflectance increase from broad beam ion milling of coals and organic-rich shales due to increased surface flatness
Broad ion beam (BIB) milling is useful in organic petrology because it can yield flat sample surfaces and avert the ‘smearing’ of organic matter (OM) that results from traditional mechanical polishing. This potentially makes BIB especially useful in the study of nano-porosity, where even minor mechanical disruption of the sample surface distorts the sample characteristic of interest—the pore stru