富碳质地质样品Re-Os同位素体系研究进展

李欣尉; 李超; 周利敏; 赵鸿; 屈文俊

doi:10.15898/j.ykcs.202207200135

富碳质地质样品Re-Os同位素体系研究进展

1.
国家地质实验测试中心，北京 100037

2.
中国地质调查局铼-锇同位素地球化学重点实验室，北京 100037

基金项目:
国家自然科学基金青年基金项目(41703059)；中国地质科学院基本科研业务费项目(CSJ-2021-05X)

详细信息

作者简介: 李欣尉，硕士，高级工程师，主要从事Re-Os同位素分析方法研究。E-mail：lixinwei-re-os@qq.com

中图分类号: O657.63

收稿日期: 2022-07-20

修回日期: 2022-08-19

录用日期: 2022-11-02

刊出日期: 2023-03-28

A Review of Research Progress on Re-Os Isotopic System of Carbon-enriched Geological Samples

1.
National Research Center for Geoanalysis, Beijing 100037, China

2.
Key Laboratory of Re-Os Isotope Geochemistry, China Geological Survey, Beijing 100037, China

Received Date: 20 July 2022

Revised Date: 19 August 2022

Accepted Date: 02 November 2022

Publish Date: 28 March 2023

摘要

摘要:
Re-Os同位素定年技术在富有机质沉积岩、低变质沉积岩、湖相沉积物、煤、油气藏样品等富碳质地质样品的尝试和成功应用，使其成为直接厘定地层沉积时代、重大地质事件发生时限和机制、古环境重建、油气藏直接定年、油气演化过程推演等研究的关键技术手段。然而，受到富碳质地质样品中极低的Re和Os丰度、采样方式以及地质作用等因素的影响，很多样品的Re-Os等时线年龄和初始Os同位素比值精度超过10%，不能有效地评价海水Os的真实来源和地质作用程度，影响了对不同沉积体系及油气演化过程中Re和Os的化学行为和Re-Os等时线年龄地质意义的理解。由此，本文从富碳质地质样品的Re-Os化学行为和地质应用进展出发，对富碳质地质样品Re-Os同位素分析过程中的采样和取样方式、溶样方法、分离富集方式和标准物质选择四方面进行了总结和完善。指出以沉积速率为采样间距参考，通过预处理方式提高样品的均匀性，使用流程空白更低、对同位素分馏影响更小的溶样方法和分离富集方式进行Re-Os同位素分析，以基质匹配的地质标样进行数据监控可进一步提高样品Re-Os同位素分析质量，有助于不同类型富碳质地质样品Re和Os赋存机制研究、Re-Os同位素分析技术开发及地质应用拓展。
- Re-Os同位素体系 /
- 富碳质地质样品 /
- 油气演化 /
- Re、Os化学行为 /
- 地质应用 /
- 富碳质地质标样
Abstract:
Re and Os are relatively enriched in organic-enriched sedimentary rocks under an anoxic environment due to their organophilic property, and the seawater Os isotopic composition is recorded during the deposition of sedimentary rocks. Under certain geological conditions, the Re and Os in organic-enriched sedimentary rocks will transfer to oil-gas reservoir samples through the process of hydrocarbon generation. The enrichment mechanism of Re and Os in these carbon-enriched geological samples, such as organic-enriched sedimentary rocks, low-metamorphic sedimentary rocks, lacustrine sediments, coal, and oil-gas reservoir samples is the basis of wide geological applications. Re-Os isotopic system of organic-enriched sedimentary rocks has been applied to directly date deposition ages or stratigraphic boundary ages or oil-gas reservoirs, has been used to provide the occurrence time and explore the mechanism of major geological events, reconstructing paleo-environment, and deducing the evolution of petroleum, which has resulted in many achievements.

The accumulation mechanism of Re and Os in organic-enriched sedimentary rocks plays an important role in understanding the geological significance of Re-Os isotopic data obtained from organic-enriched sedimentary rocks. In anoxic seawater, Re and Os are reduced to lower valence states of Re(Ⅳ) and Os(Ⅲ), respectively, and then Re and Os enter into organic-rich sedimentary rocks by combining with organic matter. Re and Os are enriched and fractionated during this process, enabling the Re-Os isotope system of organic-enriched sedimentary rocks to directly determine stratigraphic boundaries and sedimentary ages. The Re-Os isotope system has successfully provided accurate stratigraphic boundary ages of Devonian—Carboniferous, Cambrian—Ordovician, Ordovician—Silurian, Permian—Triassic, middle-upper Triassic, and Jurassic—Cretaceous. Furthermore, the Re-Os isotopic system has unique advantages for the strata lacking biological fossils or volcanic interlayers, which have provided the sedimentary age of the Niutitang Formation black shale in Guizhou province and Doushantuo Formation in South China. During the process of hydrogenous source Os into organic-enriched sedimentary rocks, the relative flux of Os from continental weathering, hydrothermal and cosmic dust was recorded, which was reflected as the initial Os isotopic ratio of sedimentary rocks. The coupling relationship between the variation of Os isotopic ratios, atmospheric oxygen level, crustal weathering degree, glaciation events, meteorite impact events, and Large Igneous Provinces can provide the occurrence time and explore the mechanism of major geological events in the history of the earth. The paleoseawater environment and paleoclimate during sedimentation can be further reduced in multiple dimensions by means of the coordinated variation between Re-Os isotopic data, organic matter accumulation, enrichment degree of redox-sensitive elements, and other geochemical proxies.

The behavior of Re and Os in the oil-gas system has always been the focus and difficulty in the research of oil-gas reservoir chronology, which is an important basis for understanding the geological significance and wide application of oil-gas reservoir-related samples. The chemical behavior of Re-Os varies in different stages of hydrocarbon formation and evolution. It has been found that the Re-Os isotope system of source rocks will not be destroyed during the process of hydrocarbon generation, and Re/Os fractionation and redistribution of Re and Os will occur during the process of hydrocarbon expulsion and migration. During the process of deasphaltizing, biodegradation, thermal alteration, thermal cracking and oil-water reaction, the asphaltene in crude oil will change correspondingly, and Re and Os in crude will migrate and fractionate accordingly, which will affect the closure of Re-Os isotope system, and even reset the Re-Os isotope system in crude. The different chemical behaviors of Re and Os in the process of hydrocarbon formation and evolution determine the geological significance of Re-Os isochrones obtained from oil-gas samples.

Despite the Re-Os isotope system obtaining many achievements and advances in the application of carbon-enriched geological samples, there are still many crucial problems that need to be solved, which restrict the wide application of the Re-Os isotope system. Through statistical analysis of the Re-Os data (including Re and Os contents, ages and initial Os uncertainty) of carbon-enriched geological samples from different sedimentary ages, it is found that the Re and Os contents of organic-enriched sedimentary rocks are at the level of 10^-9-10^-12g/g, and the error of the Re-Os isochron age and initial Os isotopic ratio of many samples exceeds 10%, especially the larger error of initial Os data. In the process of Re-Os isotope analysis, the accuracy of initial Os isotopic ratio data will not only be affected by sample content, procedural blank of chemical treatment method, error propagation and amplification during calculation, but also by geological factors in the process of sampling. The accuracy of the Re-Os data of carbon-enriched geological samples restricts the accurate identification of the paleoenvironment, the occurrence time of major geological events, the true source of seawater Os, and the degree of geological process by using the initial Os isotopic ratio and the Re-Os isochron age of organic-enriched sedimentary rocks. Moreover, the error of Re-Os isotopic data in the oil-gas system is larger than that that in the organic rich sedimentary rocks. Studies on Re-Os chemical analysis methods and sampling methods for different types of oil-gas samples are still insufficient, and the fractionation mechanism of Re-Os in the process of hydrocarbon formation and evolution is still unclear. This hinders the further understanding of the chemical behavior of Re and Os, and the geological significance of Re-Os isochron ages during oil-gas evolution. In addition, the lacustrine sediments and coal have more complex material sources, geological processes, and the impact of terrigenous detrital during the formation process that is difficult to obtain effective sedimentary ages by Re-Os isotope dating at present.

On the basis of existing Re-Os isotope analysis techniques, improving the Re-Os data quality as much as possible is the key to studying the Re-Os enrichment mechanism of carbon-enriched geological samples, especially exploring the chemical behavior of Re and Os and geological significance of the Re-Os isochron age of the oil-gas system. There are four aspects that can improve the accuracy of Re-Os isotopic data of carbon-enriched geological samples.

(1) Sampling methods: In addition to collecting fresh and unweathered organic-carbon geological samples, the deposition rate can be a reference as a sampling interval. This can guarantee the samples have relatively uniform initial Os isotopic value and a wide range of the Re-Os isotopic ratios and can improve the accuracy of the Re-Os isochron and initial Os values. Through different pretreatment, such as mixing for a long time, or extracting with organic reagents improvements to the homogeneity of oil-gas samples and the quality of Re-Os data can be made.

(2) Dissolution methods: Except for the traditional H₂SO₄-CrO₃ and reverse aqua regia method, researchers established two dissolution methods which were HNO₃-H₂O₂ and H₂SO₄-Na₂CrO₄ to solve the problem of high Re blank of the traditional H₂SO₄-CrO₃ method and improve the accuracy of Re-Os data. As the principle of choosing a suitable dissolution method, the Re and Os content of the samples especially the Os content should be considered first and the method with lower procedural blank should be selected.

(3) Enrichment methods: Previous studies presumed that the ¹⁸⁵Re/¹⁸⁷Re data obtained by acetone-NaOH extraction method and anion resin exchange method were consistent. However, recent studies have confirmed that different enrichment methods can produce Re fractionation. The acetone-NaOH extraction method can obtain more consistent results than anion resin exchange method during Re enrichment. The acetone-NaOH extraction method is recommended for samples with Re content less than 1ng/g and for oil-gas samples.

(4) Selection of reference materials: Matrix matched reference materials are very important in monitoring the process, data quality and method accuracy of Re-Os isotope analysis. At present, the main reference materials used are shale and oil shale standard samples (SBC-1, SCo-2 and SGR-1b) of the United States Geological Survey (USGS) and crude standard samples (NIST RM8505) of National Institute of Standards and Technology (NIST). There are also calcareous organic-enriched shales from the USGS and sedimentary rock samples from the Japan Geological Survey. According to the summarized Re-Os data obtained by different dissolution methods, SBC-1, SGR-1b and SCo-2 have relatively uniform Re/Os content and isotope ratio on the whole, which can be used for Re-Os data monitoring of shale and oil shale, respectively. The Re-Os data of calcareous organic-enriched shale standard samples have been reported recently and show good uniformity which have great potential in monitoring Re-Os data. NISTRM8505 has relatively uniform Re-Os isotope ratio and may be more suitable for isotope ratio monitoring.

In conclusion, the Re-Os isotope system of carbon-enriched geological samples provides much key information for the determination of sedimentary age, paleomarine environment evolution, occurrence time of major geological events, and oil-gas evolution, which is significant for understanding Earth's history. It is important to improve the accuracy of Re-Os isotope data of carbon-enriched geological samples by different methods to better understand chemical behavior of Re and Os and the geological significance of Re-Os isochron age. Enriching and improving Re-Os analysis methods, databases and reference materials of carbon-enriched geological samples will provide important support for the study of Re-Os enrichment mechanism of carbon-enriched geological samples and its wide application
- Re-Os isotope system /
- carbon-enriched geological samples /
- petroleum evolution /
- Re-Os chemical behavior /
- geological application /
- carbon-enriched reference materials

HTML全文

图 1 不同成熟度黑色页岩样品Re-Os含量及斜率(引自Li等^[9]，2021)。黑色虚线为不成熟和低成熟样品趋势线，黄色虚线为成熟样品趋势线，红色虚线为过成熟样品趋势线

Figure 1.

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图 2 文献中已报道的富有机质沉积岩Re-Os同位素数据统计：(a)Re含量范围分布；(b)Os含量范围分布；(c)Re-Os等时线年龄和初始Os值误差范围分布

Figure 2.

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图 3 不同文献中的页岩标样SBC-1(a~d)、油页岩标样SGR-1b(e~h)和原油标样RM8505(i~l)的Re-Os数据(IAR、HC、HH和HNaC分别代表逆王水、HNO₃-H₂O₂、H₂SO₄-CrO₃和H₂SO₄-Na₂CrO₄溶样法；黑色虚线为所有数据平均值，阴影部分为所有数据1倍标准偏差)

Figure 3.

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表 1 国内外实验室Re-Os同位素分析方法、流程空白及适用地质样品对比

Table 1. Comparison of commonly used Re-Os isotopic analysis methods, procedural blank and applicable geological samples

溶样方法	优点	不足	主要适用地质样品	流程空白		数据来源
溶样方法	优点	不足	主要适用地质样品	Re含量(pg)	Os含量(pg)	数据来源
H₂SO₄-CrO₃	选择性溶样减少碎屑溶解数据更精确	高Re空白 CrO₃纯化困难环保问题有害健康	富有机质沉积岩油气藏样品	40 16.8±0.06 16.8±0.4 10.8±1.5	<0.1 0.43±0.06 0.4±0.1 0.12±0.05	[104] [22] [8] [105]
逆王水	全流程空白最低试剂易纯化	高有机碳样品易爆炸	硫化物富有机质沉积岩油气藏样品岩浆岩	0.67±0.18 3.7±4.7 4.3±1.8	0.37±0.06 0.34±0.226 0.36±0.22	[105] [75] [59]
HNO₃-H₂O₂	全流程空白较低试剂易纯化	易爆炸	富有机质沉积岩岩浆岩	8~12	0.8±0.2	[59]
H₂SO₄-Na₂CrO₄	全流程空白低 Re空白水平低试剂易纯化	环保问题有害健康	富有机质沉积岩	1~2	0.6	[60]

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表 2 已报道的富碳质地质标样Re-Os同位素数据

Table 2. Reported Re-Os data of carbon-enriched geological references materials

标样编号	研制机构	标样类型	Re含量(ng/g)	Os含量(pg/g)	¹⁸⁷Re/¹⁸⁸Os	¹⁸⁷Os/¹⁸⁸Os	数据来源
SBC-1	美国地质调查局 (USGS)	页岩	11.11±0.14 (n=43, RSD=1.3%)	100.2±4.1 (n=43, RSD=4.1%)	883.5±46.0 (n=43, RSD=5.2%)	5.119±0.270 (n=43, RSD=5.3%)	[58, 60, 71]
SCo-2	美国地质调查局 (USGS)	页岩	1.179±0.042 (n=6, RSD=3.6%)	1167±6.8 (n=6, RSD=5.8%)	57.91±2.95 (n=6, RSD=5.1%)	1.596±0.018 (n=6, RSD=1.2%)	[71]
SGR-1b	美国地质调查局 (USGS)	油页岩	34.71±0.93 (n=24, RSD=2.7%)	0.4541±0.0235 (n=24, RSD=5.2%)	448.8±21.4 (n=24, RSD=4.8%)	1.787±0.009 (n=43, RSD=0.5%)	[59, 71]
ShTX-1	美国地质调查局 (USGS)	钙质富有机质页岩	141.6±0.2 (n=7, RSD=0.1%)	617.8±10.4 (n=7, RSD=1.7%)	1738±24 (n=7, RSD=1.4%)	4.565±0.013 (n=7, RSD=0.3%)	[71]
ShCX-1	美国地质调查局 (USGS)	钙质富有机质页岩	13.62±0.14 (n=7, RSD=1.0%)	424.3±13.9 (n=7, RSD=3.3%)	206.8±7.1 (n=7, RSD=3.4%)	2.702±0.017 (n=7, RSD=0.6%)	[71]
JCh-1	日本地质调查局 (GSJ)	沉积岩	24.53±4.17 (n=8, RSD=17.0%)	5.604±0.375 (n=12, RSD=6.7%)	22.97±3.6 (n=8, RSD=15.7%)	0.5908±0.0189 (n=11, RSD=3.2%)	[74]
JMS-2	日本地质调查局 (GSJ)	沉积岩	126.1±4.1 (n=9, RSD=3.2%)	264.4±12.6 (n=11, RSD=4.8%)	2.540±0.156 (n=7, RSD=6.1%)	0.8138±0.0500 (n=10, RSD=6.2%)	[74]
RM 8505	美国标准局 (NIST)	原油	2.228±0.508 (n=43, RSD=22.8%)	27.06±3.63 (n=36, RSD=13.4%)	445.5±31.5 (n=36, RSD=7.1%)	1.531±0.076 (n=36, RSD=5.0%)	[67-70, 75]

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