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Molecular and Isotopic Characteristics of Mature Condensates from the East China Sea Shelf Basin Using GC×GC-TOFMS and GC-IRMS

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Molecular and Isotopic Characteristics of Mature Condensates from the East China Sea Shelf Basin Using GC×GC-TOFMS and GC-IRMS Journal of Earth Science, Vol. 30, No. 2, p. 376–386, April 2019 ISSN 1674-487X Printed in China https://doi.org/10.1007/s12583-018-1001-3 Molecular and Isotopic Characteristics of Mature Condensates from the East China Sea Shelf Basin Using GC×GC-TOFMS and GC-IRMS Chao Shan 1, 2, Jiaren Ye *1, Alan Scarlett2, Kliti Grice2 1. Key Laboratory of Tectonics and Petroleum Resources of Ministry of Education, China University of Geosciences, Wuhan 430074, China 2. WA Organic and Isotope Geochemistry Centre, and John de Laeter Centre, the Institute for Geoscience Research, Department of Applied Chemistry, Curtin University of Technology, Perth WA 6845, Australia Chao Shan: https://orcid.org/0000-0002-0846-0832; Jiaren Ye: https://orcid.org/0000-0001-5699-8074 ABSTRACT In this study, biomarkers, together with stable carbon (δ13C) and hydrogen (δD) isotopic compositions of n-alkanes have been examined in a suite of condensates collected from the East China Sea Shelf Basin (ECSSB) in order to delineate their source organic matter input, depositional conditions and evaluate their thermal maturity. Previously, GC-MS analyses have shown that all the condensates are formed in oxidizing environment with terrestrial plants as their main source input. No significant differences were apparent for biomarker parameters, likely due to the low biomarker content and high maturity of these condensates. Conventional GC-MS analysis however, may provides limited information on the sources and thermal maturity of complex mixtures due to insufficient component resolution. In the current study, we used comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (GC×GC-TOFMS) to increase the chromatographic resolution. Compounds such as alkyl cyclohexanes, alkyl cyclopentanes and diamondoids, which can be difficult to identify using conventional GC-MS analysis, were successfully identified using GC×GC-TOFMS. From our analyses we propose two possibly unreported indicators, including one maturity indicator (C5--cyclohexane/C5+-cyclohexane) and one oxidation-reduction environment indicator (alkyl-cyclohexane/alkyl-cyclopentane). Multiple petroleum charging events were proposed as an explanation for the maturity indicators indexes discrepancy between methyl-phenanthrene index (MPI) and methyl-adamantane index (MDI). In addition, the stable isotopic results show that condensates from the Paleogene have significantly higher positive δ13C values of individual n-alkanes than the Neogene samples. Based on δD values, the samples can be divided into two groups, the differences between which are likely to be attributed to different biosynthetic precursors. Variation within each group can likely be attributed to vaporization. KEY WORDS: condensate, biomarker characteristic, source information, GC×GC-TOFMS, GC-IRMS. 0 INTRODUCTION useful information on condensates. The application of GC×GC- Conventional molecular biomarkers (e.g., steranes, ter- TOFMS has been recognized as a powerful method for solving panes) from mature or high mature condensate usually cannot co-elution problems (Aguiar et al., 2010; Ventura et al., 2010), be accurately identified in conventional gas chromatography which can help identify novel compounds and geochemical in- mass spectrometry (GC-MS) analysis due to low content and dicators (Ventura et al., 2012; Aguiar et al., 2011). low signal-to-noise ratio (Chen et al., 1996). Moreover, lots of The gas chromatography-isotopic ratio/mass spectrometry information in the light hydrocarbons of condensate cannot be (GC-IRMS) analytical technique permits continuous flow deter- effectively revealed using conventional GC-MS analysis due to mination of carbon isotopic values of individual components in co-elution (Li et al., 2012). Instrumental methods such as complex mixtures of geochemical interest (Freeman et al., 1990; GC×GC-TOFMS and GC-IRMS as in structural investigations Hayes et al., 1990, 1987; Matthews and Hayes, 1978). This of organic geomacro-molecules, have provided a wealth of method has been successfully applied to investigate the character- istics of specific components in the saturate hydrocarbon fraction *Corresponding author: [email protected] to establish oil-oil and oil-source rock correlations (Inaba and Su- © China University of Geosciences (Wuhan) and Springer-Verlag zuki, 2003; Li et al., 1997). Many researchers have applied this GmbH Germany, Part of Springer Nature 2019 technique to evaluate the presence of unusual polycyclic alkanes in extracts of source rocks and crude oils where hopanoids and Manuscript received November 18, 2015. steranes were either absent or present in extremely low abundance Manuscript accepted March 17, 2016. samples (Zhu et al., 2003; Schaeffer et al., 1994). Shan, C., Ye, J. R., Scarlett, A., et al., 2019. Molecular and Isotopic Characteristics of Mature Condensates from the East China Sea Shelf Basin Using GC×GC-TOFMS and GC-IRMS. Journal of Earth Science, 30(2): 376–386. https://doi.org/10.1007/s12583-018- 1001-3. http://en.earth-science.net Molecular and Isotopic Characteristics of Mature Condensates from the East China Sea Shelf Basin 377 The East China Sea Shelf Basin (ECSSB) is China’s largest 2012; Li et al., 2009; Yang et al., 2004). Developed on Pre-Cam- offshore basin with good exploration prospects. Previous bi- brian and Paleozoic metamorphic basement, the sedimentary se- omarker parameter studies show that the condensates in this area quence, with approximately 10 000 m in maximum thickness, are usually derived from terrestrial organic matter and most consists of fifteen formations (Fig. 1). formed in the oxidation sedimentary environment (Zhu et al., So far, four hydrocarbon-bearing formations have been iden- 2012), however, this information is insufficient for the analysis tified in the Xihu depression, including the Baoshi, Pinghu, of oil-source correlation as many source formations are present Huagang and Longjing formations from bottom to top. Economic in similar sedimentary environments which make it hard to dis- oil and gas reservoirs are mostly distributed in the Pinghu and tinguish the characteristics of each formation. This study aims to Huagang formations, while gas-bearing intervals identified in examine the natural compositions of condensates and carbon and Lishui depression are located in the Mingyuefeng Formation. hydrogen isotopic values of n-alkanes from the ECSCB using GC×GC-TOFMS and GC-IRMS in order to effectively distin- 1.2 Sample Collection, Column Chromatography and 5Å guish their depositional environments and source input. This Molecular Sieving study benifits further oil-oil correlations or oil-source rock cor- Seven typical condensate samples were collected from relations in this area. the Mingyuefeng, Pinghu and Huagang formations. The physical property characteristics of these condensates are 1 BACKGROUND AND ANALYZING METHOD shown in Table 1. 1.1 Geological Setting Saturated hydrocarbon, aromatic hydrocarbon and non- The East China Sea Shelf Basin is China’s largest offshore hydrocarbon (polar/resin/NSO) fractions were chromatographically basin with an area of about 2.4×105 km2. This basin can be fur- separated on a column (25 cm×1 cm i.d.) of neutral alumina over ther subdivided into several depressions that formed at different silica gel (120 °C, 8 h). Saturated fractions were eluted with hexane stages of tectonic development. Among them, Xihu depression (40 mL), the aromatic hydrocarbon fraction with a mixture of n- and Lishui depression have been two focal points for intensive hexane and DCM (40 mL, 7 : 3, v : v) and the polar (NSO) fraction petroleum exploration in ECSSB (Dai et al., 2014; Cukur et al., with a mixture of DCM and MeOH (40 mL, 1 : 1, v : v). Figure 1. General structure and the strata of the East China Sea Shelf Basin. Inset map shows the locality of the basin and the tectonic units (modified after Dai et al., 2014): (1) Min-Zhe uplift belt; (2) East China Sea Shelf Basin; (3) Diaoyudao folded uplift belt; (4) the frontal basin of continental shelf; (5) Okinawa trough; (6) Ryukyu Island and (7) Ryukyu Trench. 378 Chao Shan, Jiaren Ye, Alan Scarlett and Kliti Grice Then, the total saturated hydrocarbon fraction was sepa- analysis, average values of at least three analyses of each sample rated into normal alkane and branched/cyclicalkane fractions and with a standard deviation of less than 4‰ were reported. through 5Å molecular sieves before gas chromatography isotope Carbon and hydrogen isotopic compositions are reported ratio mass spectrometry (GC-IRMS) analysis to reduce problems using the V-PDB (Vienna PeeDee Belemnite) for carbon and with coelution of compounds and to enhance the precision of standard δ-notation relative to V-SMOW (Vienna Standard carbon isotopic analysis. Specifically, samples in cyclohexane Mean Ocean Water) for hydrogen. was added to a 2 mL vial, 3/4 of it filled with activated 5Å mo- lecular sieves. The vial was capped and placed into an oven 2 RESULTS AND DISCUSSION (80 °C, overnight). The resulting solution was then cooled and 2.1 Basic Geochemical Parameters filtered through a small column of silica plugged with cotton The basic geochemical parameters for the selected samples wool (pre-rinsed with cyclohexane) and the sieves were rinsed are reported in Table 1. The thin liguid chromatography flame thoroughly with cyclohexane yielding the branched/cyclic frac- ionization detector (TLC-FID) analysis shows that the saturated tion (5Å excluded). The n-alkanes were recovered by dissolution
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