Nuclear Magnetic Resonance Characteristics and in situ Oil Content Analysis of Shale Crushing and Heat Treatment
Received date: 2025-02-10
Revised date: 2025-04-20
Online published: 2025-06-04
Supported by
the National Natural Science Foundation of China Regional Innovation Joint Fund Project(U22A20574);The Heilongjiang Provincial Key R & D Program(GA23A906)
Shale samples exposed to open environments experience major loss of light hydrocarbons due to pressure release, while simultaneously, the viscosity of retained hydrocarbons increases due to temperature reduction. These changes alter the state of hydrocarbons, making it difficult to accurately quantify shale oil content under in situ temperature and pressure conditions using Nuclear Magnetic Resonance (NMR) at room temperature. This study examines shale from the Qingshankou Formation (Cretaceous) in the Songliao Basin. Representative shale samples at both low and high maturity stages were selected. NMR measurements were performed on high-maturity shale samples with varying degrees of pulverization, as well as on low- and high-maturity shale samples under different temperature conditions, to quantify fluid loss and state transformation during pulverization and heating and to determine oil content characteristics under the influence of temperature. Results showed that during shale crushing from standard plunger size to ~0.04 cm particles, the morphology of the T2 spectrum, the total T1-T2 signal, and the signal strength of each hydrogen-containing component remained largely unchanged. Therefore, prolonged exposure during crushing does not lead to significant residual fluid loss. With increasing temperature, light oil signals increased while water signals decreased in low-maturity shale; in high-maturity shale, both oil and water signals decreased. Additionally, the signal from hydroxyl compounds declined with heating but recovered upon returning to room temperature. These findings indicate that rising temperature leads to continuous free water evaporation. In low-maturity shale, pre-oil bitumen, which has high viscosity at room temperature, transforms from a solid-like state into liquid light oil. After heating to 100 °C, the absolute amount of NMR-detected light oil increased by 107%. In contrast, high-maturity shale oil bitumen already exists as light oil at room temperature and evaporates upon heating. The reversible change in hydroxyl-containing compounds with temperature rise and fall reflects the temperature-dependent water adsorption capacity of clay. Thus, when using NMR to evaluate oil content in low-maturity shale, the transformation of pre-oil bitumen under elevated temperatures must be considered to avoid underestimating shale oil content.
Key words： Shale; T1-T2 map; In-situ oil content; Formation temperatures; Fluid state
Longhui BAI , Bo LIU , Mingbo LIU , Yong SU , Liu WANG , Yingdong HUO , Pengcheng XU , Xiaofei FU . Nuclear Magnetic Resonance Characteristics and in situ Oil Content Analysis of Shale Crushing and Heat Treatment[J]. Advances in Earth Science, 2025 , 40(5) : 525 -539 . DOI: 10.11867/j.issn.1001-8166.2025.034
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