ABSTRACT Organic matter (OM) in petroleum source rocks is a mixture of organic macerals that follow their own specific evolutionary pathways during thermal maturation. Understanding the transformation of each maceral into oil and gas with increasing thermal maturity is critical for both source rock evaluation and unconventional shale oil/gas reservoir characterization. In this study, organic petrology was used to document the reflectance, abundance, color, and fluorescence properties of primary organic macerals and solid bitumen (SB) in 14 Upper Devonian New Albany Shale samples (kerogen type II sequence) from early mature (vitrinite reflectance [VR o ] of 0.55%) to post-mature (VR o 1.42%). Micro-Fourier transform infrared (micro-FTIR) spectroscopy analyses were conducted on these samples to derive information on the evolution of the chemical structure of organic macerals and SB with increasing thermal maturity. Primary OM (amorphous organic matter, alginite, vitrinite, and inertinite) and secondary organic matter (SB) were identified in early mature samples. Amorphous organic matter (AOM) was the dominant organic component in early mature samples and was observed up to the maturity equivalent to VR o 0.79% but could not be identified at VR o 0.80%. An organic network composed of AOM and SB was observed from VR o 0.55 to 0.79%, which, together with the decrease in AOM content being accompanied by an increase in SB content, suggests that with the onset of petroleum generation, SB gradually replaced the original AOM. Alginite, represented by Tasmanites cysts, started to transform to pre-oil bitumen at a maturity corresponding to VR o 0.80%. It shows weak orange-yellow fluorescence at this maturity, a change from strong greenish-yellow fluorescence in early mature samples. Alginite could not be identified at VR o 0.89%, and generated bitumen remained in place or migrated over short distances. Petrographic observations and micro-FTIR study of alginite indicate that substantial hydrocarbon generation from alginite does not start until alginite is completely transformed to pre-oil bitumen. In contrast to AOM and alginite, vitrinite and inertinite derived from terrestrial woody materials occur as dispersed particles and do not change significantly during thermal maturation. A linear relationship between vitrinite and SB reflectance exists for the studied samples. The reflectance of vitrinite is higher than that of SB until VR o 0.99%, and at higher maturities, SB reflectance exceeds vitrinite reflectance. The inclusion of pre-oil SB converted from alginite in reflectance measurements could result in a lower average SB reflectance and, therefore, caution should be applied when using SB reflectance as an indicator of thermal maturity.

Abstract There are a variety of pore types in unconventional resource mudstones and shales. The currently preferred method by geologists and petrophysicists is to examine and analyze these mudstones and shales by argonion and focused ion-beam milling to produce an ultrasmooth surface, coupled with observation under the field emission scanning electron microscope (FESEM). Potential issues with Ar-ion milled/FESEM preparation and imaging include (1) the small size of sample cubes for upscaling, (2) loss of structural fabric during the milling–imaging process, (3) fewer non-inorganic pore types observed than when observed with an unpolished surface, (4) analog use of pores from one shale to another, although the pore types and composition might differ, and (5) the creation of potential artifacts related to desiccation and rock expansion because of core retrieval and sample preparation. Conventional FESEM images obtained from freshly broken surfaces reveal much more textural detail than those obtained from ion-milled (polished) surfaces. Although conventional FESEM methodology may share some of the same limitations as Ar-ion beam-milled/FESEM technology, FESEM methodology should not be overlooked because it provides a more cost-effective and potentially more accurate analysis for estimating porosity and determining pore types and their distribution in shales. Comparison of FESEM images from ion-milled and fresh, non-ion-milled surfaces reveals that organic matter and internal organoporosity are best viewed on ion-milled surfaces, but shale microfabric and non-organoporosity is best viewed under non-milled surfaces. Complete FESEM imagery for shale characterization should include both types of analyses.