富有机质样品Re-Os同位素定年实验方法

武鲁亚; 金之钧; 储著银; 刘可禹

doi:10.11781/sysydz202103513

富有机质样品Re-Os同位素定年实验方法

doi: 10.11781/sysydz202103513

武鲁亚^1,,
金之钧²,
储著银³,
刘可禹^{1, 4, ,}

1.
中国石油大学(华东) 地球科学与技术学院, 山东青岛 266580
2.
中国石化石油勘探开发研究院, 北京 102206
3.
中国科学院地质与地球物理研究所岩石圈演化国家重点实验室, 北京 100029
4.
海洋国家实验室海洋矿产资源评价与探测技术功能实验室, 山东青岛 266071

基金项目:

中国科学院战略性先导科技专项A类项目 XDA14010401

中国石油大学（华东）自主创新科研计划 17CX06032

详细信息

作者简介:
武鲁亚(1993-), 女, 博士研究生, 从事地球化学和油气成藏年代学研究。E-mail: b16010016@s.upc.edu.cn

通讯作者:
刘可禹(1963-), 男, 教授, 从事沉积学与石油地质学等研究。E-mail: liukeyu@upc.edu.cn

中图分类号: TE135
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出版历程
- 收稿日期: 2020-09-30
- 修回日期: 2021-04-16
- 刊出日期: 2021-05-28

Re-Os isotopic dating procedures for organic-rich samples

WU Luya^1
,,
JIN Zhijun²,
CHU Zhuyin³,
LIU Keyu^{1, 4
, ,}

1.
School of Geosciences, China University of Petroleum(East China), Qingdao, Shandong 266580, China
2.
SINOPEC Petroleum Exploration and Production Research Institute, Beijing 102206, China
3.
State Key Laboratory of Lithospheric Evolution, Institute of Geology and Geophysics, Chinese Academy of Sciences, Beijing 100029, China
4.
Laboratory for Marine Mineral Resources, Qingdao National Laboratory for Marine Science and Technology, Qingdao, Shandong 266071, China

摘要

摘要: 近年来，铼—锇（Re-Os）同位素体系在确定含油气系统烃源岩沉积年龄、烃类生成、运移、后期调整改造年龄（古油藏热裂解、硫酸盐热化学还原反应等）以及油源示踪方面取得了一系列成果。但是，富有机质样品的Re-Os同位素体系存在元素丰度低、赋存形式复杂、同位素体系封闭性影响因素以及Os同位素组成均一机制不清等诸多难题，进而导致其构建的等时线年龄误差相对较大。通过测年样品筛选、富有机质样品化学前处理、实验流程空白控制以及国际参考标样监控等4个方面，对现有的富有机质样品的Re-Os同位素分析测试全流程进行了总结与完善，可为拟开展含油气系统Re-Os定年工作的研究人员提高数据质量，构建理想的Re-Os等时线。
- Re-Os同位素定年 /
- 样品筛选 /
- 化学前处理 /
- 流程空白控制 /
- 参考标样 /
- 含油气系统
Abstract: The rhenium-osmium (Re-Os) geochronometer is newly developed technology and has been regarded as a promising radiometric tool for the direct dating of the deposition of source rock, hydrocarbon generation, migration and consequent alteration (e.g., thermal cracking, thermochemical sulphate reduction), and oil-source correlation. However, the complex nature of Re-Os systems in organi-rich samples, including their relatively low elemental contents, multiple origins and occurrences, ambiguous homogenization mechanisms of ¹⁸⁷Os/¹⁸⁸Os and our limited understanding of the closed system of Re-Os systematics etc., often result in the relatively large uncertainties of obtained isochrones. In this paper, to improve their data quality and yield ideal Re-Os isochrons, the existing Re-Os isotopic analysis method was improved by the terms of sample selection and screening, chemical pretreatment, total analytical blank control and international reference material monitoring. Results showed that a comprehensive guide to researching working in Re-Os geochronology for petroleum system analysis can be available.
- Re-Os dating /
- sample selection /
- chemical pretreatment /
- total analytical blank control /
- reference material /
- petroleum system

HTML全文

图 1 国外典型含油气系统原油样品Re-Os同位素等时线

a.英国Shetland群岛原油(原始数据引自文献[11])；b.美国Bighorn盆地Phosphoria原油(原始数据引自文献[12])

Figure 1. Re-Os isochrons of crude oil samples from two typical petroleum systems abroad

下载: 全尺寸图片幻灯片

图 2 意大利Ragusa盆地Gela-1井原油样品Re-Os同位素等时线

a.Noto和Sciacca组的全油和沥青质组分；b.Streppenosa组原油可溶组分(马青烯)(原始数据引自文献[16])

Figure 2. Re-Os isochrons of crude oil from well Gela-1 in Ragusa Basin, Italy

下载: 全尺寸图片幻灯片

图 3 富有机质样品Re-Os同位素分析完整实验流程

Figure 3. Procedure for determining Re-Os concentrations and isotopic compositions of organic-rich samples

下载: 全尺寸图片幻灯片

图 4 不同实验测定的NIST8505原油标样的Re含量(a)、Os含量(b)，¹⁸⁷Re/¹⁸⁸Os(c)和¹⁸⁷Os/¹⁸⁸Os比值(d)

图a和图b中灰色虚线为不同实验室测定数据的平均值；图中红色实线为实验室间平均值，红色虚线表示其各自的2σ标准偏差原始数据引自文献[16, 28, 35, 45, 54-55]。

Figure 4. Concentrations of Re (a) and Os (b) and isotopic compositions (c-d) of crude oil standard sample NIST8505 analyzed by three different laboratories

下载: 全尺寸图片幻灯片

表 1 国内外Re-Os实验室常用溶样方法比较

Table 1. Comparison of commonly used sample digestion methods for Re-Os isotopic analysis

溶样方法	优点	缺点/局限性
酸溶法(HBr，HCl-乙醇)	可避免产生挥发性的OsO₄，本底低	样品溶解不完全，回收率低
碱熔法	可完全溶解难熔相	实验本底高，消解过程中难达到同位素交换平衡
硫化镍火试金法	溶样量大，可有效避免Os的“块金效应”	Re的数据可信度较低，Os本底高，溶样过程中存在Os的损失
Carius管溶样法	密闭体系，样品近完全溶解，易达到同位素交换平衡，本底低	对于一些难溶矿物不能完全溶解，易爆炸
高温高压反应釜法	完全、快速消解样品，本底低，安全性高	实验装置较为昂贵，溶样管重复利用
注：表中数据据文献[29-35]整理。

下载: 导出CSV

表 2 近几年国内外主要Re-Os实验室全流程Re-Os本底水平对比

Table 2. Total analytical blanks of major Re-Os laboratories reported recently

Re-Os同位素实验室	溶样方法	Re本底水平/pg	Os本底水平/pg	¹⁸⁷Os/¹⁸⁸Os	数据来源
科罗拉多州立大学	HPA-S逆王水溶样	16.3±16.2	0.102±0.066	0.53±0.31	^[16]
	Carius管逆王水溶样	3.7±4.7	0.34±0.226	0.251±0.02	^[16]
	HPA-S硝酸溶样	0.98±0.18	0.167±0.024	0.31±0.04	^[16]
杜伦大学	Carius管逆王水溶样	1.63±0.67	0.065±0.013	0.23±0.02	^[17]
杜伦大学	Carius管硫酸氧化铬溶样	16.8±0.4	0.4±0.1	0.25±0.21	^[21]
中科院地质与地球物理研究所	Carius管逆王水溶样	7±0.62	0.25±0.12		^[41]
中科院广州地球化学研究所	Carius管逆王水溶样	8.8±3.2	0.28±0.2	0.259±0.038	^[48]
	Carius管硫酸氧化铬溶样	0.75±0.32	0.33±0.29	0.206±0.025	^[50]
	Carius管H₂O₂-HNO₃溶样	8±3	0.8±0.2	0.128 9± 0.004 8	^[50]
国家地质实验测试中心	Carius管HNO₃-HCl-H₂O₂溶样	2	0.1		^[49]
科廷大学	Carius管逆王水溶样	17	0.54	0.137 ± 0.028	^[51]

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