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Hydrous Pyrolysis of Different Kerogen Types of Source Rock at High Temperature-Bulk Results and Biomarkers

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Hydrous Pyrolysis of Different Kerogen Types of Source Rock at High Temperature-Bulk Results and Biomarkers Journal of Petroleum Science and Engineering 125 (2015) 209–217 Contents lists available at ScienceDirect Journal of Petroleum Science and Engineering journal homepage: www.elsevier.com/locate/petrol Hydrous pyrolysis of different kerogen types of source rock at high temperature-bulk results and biomarkers Mingliang Liang a,b,d, Zuodong Wang a,n, Jianjing Zheng a, Xiaoguang Li c, Xiaofeng Wang a, Zhandong Gao a,d, Houyong Luo a,d, Zhongping Li a, Yu Qian a,d a Key Laboratory of Petroleum Resources Research, Institute of Geology and Geophysics, Chinese Academy of Sciences, Lanzhou, Gansu Province 730000, China b The institute of Biology, Guizhou academy of Sciences, Guiyang 550000, China c Exploration and Development Research Institute, Liaohe Oilfield Company, PetroChina, Panjin 124010, China d University of Chinese Academy of Sciences, Beijing 100049, China article info abstracts Article history: Hydrous pyrolysis experiments were conducted on immature petroleum source rocks containing Received 3 December 2013 different types of kerogen (I and II) at a temperature range of 250–550 1C to investigate the role of Accepted 24 November 2014 kerogen type in petroleum formation at high temperature. At temperatures less than 350 1C, the bulk Available online 3 December 2014 results and biomarker compositions were quite similar and show negligible variations for different Keywords: kerogen types. However, at high-temperature, above 400 1C (400–550 1C), unexpected results were Hydrous pyrolysis observed. The initial and peak temperature of the hydrocarbon generation of type II sources rocks is High temperature lower than the type I. The tricyclic terpenes were common in samples above 400 1C. The Ts/Tm values did Source rock not show a linear relationship with the temperature increase. The C3122S/(SþR) values did not show Kerogen significant change with temperature increase. However, a good correlation between the sterane maturity GC–MS parameters and the thermal maturity were shown, especially for type I kerogen. Temperature increase Biomarkers resulted in significant variation in the relative contents of C27,C28 and C29 steranes, suggesting that the distribution of steranes is greatly affected by thermal maturity. & 2014 Elsevier B.V. All rights reserved. 1. Introduction based on the cognition that organic matter exposed to higher temperature for a shorter period of time has the same maturity as Because of their specific genesis and structural characteristics, organic matter exposed to lower temperature for a longer period of steranes and terpanes are widely used in petroleum exploration. time, suggesting that temperature and time compensate for each They also serve as a molecular fingerprint of sedimentary organic other as effects on organic matter maturity (Stach et al., 1982). matter (OM), indicating its origin of depositional environment, and Therefore, it seems to be valid to simulate the natural maturation thermal maturity (Volkman, 2006; Wang et al., 2009). Previous process in the laboratory by increasing temperature during a short studies have documented that slight enrichment in C27 steranes period of time (Han et al., 2001). Taking into account subcritical occurs with increasing thermal stress, and questioned usage of 20S to water temperatures (Lewan, 1985), most of the hydrous pyrolysis 20R C29 sterane ratio as a maturity index (Lewan et al., 1986). experiments were performed at temperatures below 400 1C. There- Hydrous pyrolysis is used to determine petroleum generation fore, only a few thermal simulation experiments have been con- mechanisms and assess the petroleum generation potential of source ducted and reported at temperatures above 400 1C. In the present rocks (Lewan, 1979, 1983, 1985; Winters et al., 1983). Numerous study, two source rocks containing different types of kerogen (I and hydrous pyrolysis experiments have been done in both open and II) were used for the thermal simulation experiment. Attempts have closed systems, using different types of organic matter and condi- been made to observe the differences productivity of different tions, in order to understand the mechanisms of oil generation kerogen type and variations in the distributions of biomarkers (Huizinga et al., 1987a,b; Michels and Landais, 1994; Michels et al., released from the samples by pyrolysis. Especially, we conducted 1995; Béhar et al., 1997; Pan et al., 2009). These studies are mainly high temperature thermal simulation experiments (400–550 1C) among petroleum source rocks containing different types of kerogen. Andinvestigatedthetrendsandcomparethedistributionofthe n þ þ classic biomarker compositions from different liquid phases at high Corresponding author: Tel.: 86 931 4960921; fax: 86 931 8278667. 1 E-mail address: [email protected] (Z. Wang). temperature (above 400 C). http://dx.doi.org/10.1016/j.petrol.2014.11.021 0920-4105/& 2014 Elsevier B.V. All rights reserved. 210 M. Liang et al. / Journal of Petroleum Science and Engineering 125 (2015) 209–217 Fig. 1. Location of the Liaohe depression in China and the map of sampling sites. Table 1 Geochemical characteristics of the samples used in the hydrous pyrolysis. Kerogen type Source rock Depth (m) Rc (%) Tmax ( 1C) S1 (mg/g) S2 (mg/g) TOC (%) HI (mg/g) OI (mg/g) II Gray mudstone, Shahejie Fm, Liaohe Basin 2553.6–2558 0.59 427 0.28 10.75 2.37 453 21 I Brown gray shale, Shahejie Fm, Liaohe Basin 1387.49–1390.19 0.54 434 1.86 69.2 8.73 792 23 Rc (%)—vitrinite reflectance was calculated using the methylphenanthrene index (MPI). Tmax—temperature corresponding to S2 peak maximum; S1—free hydrocarbons (mg/g rock); S2—pyrolysate hydrocarbons (mg/g rock);TOC—total organic carbon; HI—hydrogen index (S2  100/TOC) (mg/g TOC); OI—oxygen index (S3  100/TOC) (mg/g TOC). 2. Samples and experimental 350, 400, 450, 500 and 550 1C, which heating rates of 10 1C /h, and kept within 71 1C of the setting point for 24 h. 2.1. Samples 2.4. Expelled oil and bitumen Two source rocks of mudstone and shale containing different types of kerogen (I and II) were used for the thermal simulation Two organic phases were collected from the reactor after experiment. Both of the samples were collected from Shahejie hydrous pyrolysis: expelled oil and bitumen. Expelled oil occurs Formation, Liaohe Basin, North China (Fig. 1)(Mu et al., 2008). The in the reactor as liquid products (Lewan, 1985). The rock chips Shahejie Formation source rocks are comprised of black gray-dark were removed from the reactor and dried in a vacuum oven at gray mudstone, gray mudstone and oil shale, with a total thickness 50 1C for 24 h, and then powdered to less than 100 mesh. Bitumen up to 1000 m. The depths of initial samples are 2553.6–2558/m was extracted from the powdered samples in a Soxhlet apparatus (type II) and 1387.49–1390.19/m (type I), respectively. The present for 72 h with a mixture of chloroform and methanol (97:3, v-v). temperatures are about 93and 51 1C, according to the average After precipitation of the asphaltenes by n-hexane, maltenes were value of geothermal gradient, which reaches 36.5/km (Wang et al., separated into three fractions by column chromatography over 2003). The organic maturity of the two samples are relatively low, silica gel and aluminum oxide (3:1). The saturated hydrocarbons and the Rc values are generally less than 0.6%. For hydrous fraction was eluted with petroleum ether, the aromatic hydro- pyrolysis experiments, samples were first powdered to less than carbons with dichloromethane and the NSO fraction (polar frac- 100 mesh. tion, which contains nitrogen, sulfur, and oxygen compounds) with methanol. 2.2. Rock-eval pyrolysis 2.5. GC–MS analyses Rock-eval pyrolysis was performed using a Rock-eval II system (Delsi instrument, Suresnes, France). And organic-carbon-content The biomarkers in the saturated hydrocarbons fraction of the (TOC) was determined using a Leco CS-344 analyzer. Group expelled oils and bitumen obtained by hydrous pyrolysis were – – organic geochemical data for investigated samples are given in analyzed by gas chromatography mass spectrometry (GC MS). A Table 1. These results indicate that source rocks contain kerogen 6890 N gas chromatograph/5973 N mass spectrometer equipped   μ fi type I and II (Huang et al., 1984). The T values of the two with a HP-5 column (30 m 0.32 mm i.d. 0.25/ m lm thick- max 1 samples are 434 1C and 427 1C, respectively, indicating low to ness) was used. The GC oven temperature was raised from 80 Cto 1 1 À1 marginal thermal maturity (Espitalie et al., 1985). 300 C (held 30 min) at 4 C min . Helium was used as a carrier gas. MS conditions were: electron ionization (EI) at 70 eV with an ion source temperature of 250 1C. A full scan mode (m/z 20 to m/z 2.3. Hydrous pyrolysis 750) was applied. Hydrous pyrolysis experiments were performed in a stainless steel reactor. 15–50 g of powdered sample and 50 ml of deionized 3. Results and discussion water were put in the reactor, and sealed the chamber then flushed three times with pure nitrogen gas to remove the air, 3.1. Amounts of expelled oil and bitumen and then evacuated. A sensor and an external control device were used to control the temperature within the autoclave. The hydrous Group composition data for the investigated samples of pyrolysis experiments were performed at temperatures 250, 300, expelled oil and bitumen are given in Table 2. The amount of M. Liang et al. / Journal of Petroleum Science and Engineering 125 (2015) 209–217 211 Table 2 Group composition for the samples of expelled oil and bitumen. Sample
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