A Pre-Treatment Method for the Determination of Organic Carbon Isotope Composition in Sedimentary Rocks
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摘要:
沉积岩的有机碳同位素研究是地质学领域的重要内容，可为地质历史时期的古环境重建、古气候变化解析、碳循环过程理解以及能源资源勘探开发提供重要信息。由于沉积岩中的有机碳主要以干酪根的形式赋存，因此，在获取沉积岩有机碳同位素值之前，需要先对岩石样品开展干酪根提取预处理。提取过程需使用大量危险化学品，制备流程长且面临化学品使用受限等诸多挑战。因此，在实际工作中，亟需开发一种更为便捷、环保的前处理方法。本文建立了一种简易的酸处理方法，实验选取110件不同岩性(灰岩、页岩、油页岩）和不同有机碳含量范围(0.83%～35.33%)的沉积岩样品进行该前处理方法与传统干酪根提取前处理方法的比对实验。结果表明，对于94%的样品，本次建立的前处理方法和干酪根提取方法获得的碳同位素值差值均小于1.0‰，满足行业标准方法重复测定的偏差要求。表明该前处理方法可以有效地实现沉积岩样品中有机碳的分离，进而准确获取有机碳同位素值这一关键地质参数。而且，样品的有机碳含量及岩性未对测定结果产生明显影响，显示该方法对常规地质样品的适用性，可满足地质勘探调查工作需求。
要点(1)沉积岩有机碳同位素测试需以干酪根提取制备为前提，制备流程长，且面临化学品使用受限等诸多挑战，需要开发更为便捷、环保的前处理方法。
(2)建立了一种基于稀盐酸实现沉积岩中有机碳组分有效分离的前处理方法，具有流程简洁、实验耗材易获取、样品用量少等优点。
(3)对比了传统的干酪根提取方法与本文建立的前处理方法对不同TOC值、不同岩性样品有机碳同位素值测定的影响，证明了本文方法对于页岩、灰岩等常见地质样品的适用性。
HIGHLIGHTS(1) The organic carbon isotope test of sedimentary rocks should be based on the extraction and preparation of kerogen, which has a long preparation process and requires the use of a significant quantity of hazardous chemicals. Therefore, more convenient and environmentally friendly pretreatment methods need to be developed.
(2) A pre-treatment method for effective separation of organic carbon components from sedimentary rocks based on dilute hydrochloric acid was established, which has the advantages of simple process, easy access to experimental consumables, and less sample consumption.
(3) The influence of the traditional kerogen extraction method and the pre-treatment method established on the determination of organic carbon isotope values of samples with different TOC values and different lithologies is compared, which proves the applicability of this method for common geological samples such as shale and limestone.
Abstract:The organic carbon in sedimentary rocks is mainly in the form of kerogen, and it is necessary to extract kerogen from samples before obtaining the organic carbon isotope value. The extraction process requires a significant quantity of hazardous chemicals and a long preparation process. Therefore, in daily work, there is an urgent need to develop a more convenient and environmentally friendly pre-treatment method. A simple acid treatment method was established, and 110 sedimentary rock samples with different lithology (limestone, shale, oil shale) and different organic carbon content range (0.83%−35.33%) were selected for comparison experiments of two pretreatment methods. The results show that for 94% of the samples, the difference of carbon isotope values obtained by the acid pretreatment method established in this study and the kerogen extraction method was less than 1.0‰, which met the deviation requirements for repeated measurements, indicating that this pretreatment method can be used to accurately obtain the key geological parameter of an organic carbon isotope value. Furthermore, the organic carbon content and lithology of the samples does not influence the results, demonstrating the applicability of this method to typical geological samples and fulfilling the requirements of geological exploration and investigation. The BRIEF REPORT is available for this paper at http://www.ykcs.ac.cn/en/article/doi/10.15898/j.ykcs.202403110038.
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Keywords:
- carbon isotope /
- sedimentary rock /
- pretreatment method /
- acid treatment /
- kerogen
BRIEF REPORTSignificance: The carbon pool in sedimentary rocks comprises both organic and inorganic carbon. Organic carbon predominantly exists in the form of kerogen, which accounts for over 80% of the total organic carbon in these rocks, while inorganic carbon primarily occurs as carbonate[1-2]. There are notable differences in the isotopic values of organic and inorganic carbon, each bearing distinct geological significance[3-6]. Currently, it is widely accepted that the stable carbon isotope value of organic matter is largely determined by its source[7-9], remaining relatively unaffected by thermal evolution. This characteristic renders it a valuable tool for distinguishing types of organic matter in the field of oil and gas geochemistry[10-15].
Since organic carbon in sedimentary rocks primarily exists in the form of kerogen, it is necessary to extract kerogen from samples before obtaining the organic carbon isotope value[30-32].
The preparation process of kerogen is complex and time-consuming, which limits the rapid acquisition of organic carbon isotope data from sedimentary rocks and affects the geological research and exploration evaluations. Furthermore, a significant amount of chemical reagents are utilized in the kerogen preparation process, which can have considerable environmental impacts. Consequently, some researchers have proposed a pretreatment method that only uses hydrochloric acid to replace the pretreatment process of kerogen preparation[33-36]. This method is simple and efficient, and it has garnered significant attention from scholars in recent years. However, the current application objects of this method are mainly modern sediments, while the data for ancient sedimentary rocks are very limited. There is also a lack of systematic comparison of the impact of the two pre-processing methods on the organic carbon isotope value determination of rock samples with different lithology and TOC values. It is not clear whether this simple pretreatment method can completely replace the kerogen extraction method[33-41].
This study established a pre-treatment method for effective separation of organic carbon components from sedimentary rocks based on dilute hydrochloric acid, and experiments were conducted using samples of various lithologies and organic carbon contents, including shale, limestone, and oil shale. The results demonstrate that the organic carbon isotope data obtained through this pre-treatment method are comparable to those acquired via the traditional kerogen extraction method. This research offers a more convenient and environmentally friendly pre-treatment method for isotope research in sedimentary rocks samples.
Methods: 110 typical profile rock samples were collected from Qiangtang Basin, including shale, oil shale and limestone. Each crushed sample was divided into 3 parts for pretreatment and subsequent experimental analysis. The Part 1 sample was used for extraction and preparation of kerogen, with the sample weight of about 100g. Part 2 and Part 3 samples were used to carry out acid treatment with about 5g per sample, and the organic carbon contents and isotope values were measured respectively after treatment.
The total organic carbon (TOC) content of sedimentary rock samples was determined by a Leco CS-744 carbon sulfur analyzer. The EA-IRMS combined system was used to determine the carbon isotope value of the sample. The combustion tube temperature of the element analyzer was set at 950℃, and the reduction tube temperature was set at 600℃. During the test process, the test results of standard substances and repeated samples need to meet the quality requirements of standard methods, and the carbon isotope test error of repeated samples is less than 0.5‰.
Data and Results: The research results indicate that the Δ13C value (δ13Cacid−δ13Cker) of the samples processed by the two methods ranges from −2.8‰ to 1.8‰. A correlation analysis was conducted on the isotope values obtained using these two pre-processing methods, revealing a strong consistency between the two datasets. The correlation followed the linear relationship described by the equation y=0.97x−0.61, with a correlation coefficient of R2=0.97 (Fig.1). Notably, the proportion of samples with Δ13C values less than 1.0‰ constitutes 94% of the total samples. These samples satisfy the repeatability error requirements for carbon isotope determination based on current standards, indicating that the carbon isotope values obtained through different pretreatment methods are highly comparable[2,21,24,30].
The study conducted a comparative analysis of carbon isotope data obtained through two pre-processing methods applied to samples with varying lithology (Fig.2). It was observed that shale samples were significantly more influenced by the different pre-processing methods, and a total of six shale samples exhibit Δ13C values exceeding 1.0%, significantly higher than those of other lithologies. Analysis indicates that this phenomenon may be attributed to either a relatively high clay mineral content in the shale or the presence of non-kerogen organic carbon in these samples[13,32]. However, there is currently little data in this part, and additional experiments are still needed to accurately reveal the reasons for this difference.
In addition, the article compared the conditions of samples with varying total organic carbon (TOC) contents (Fig.3). The results indicate that the TOC content does not consistently influence the differences between the two methods. Specifically, only six samples exhibit differences greater than 1.0‰, with their TOC values primarily ranging from 5.00% to 15.00%. Notably, these samples tend to have a high oil content. During the acid treatment process, an oil film forms around the samples, which hinders the acid from fully contacting and reacting with them, ultimately leading to discrepancies in the measurement results.
The study selected three crucibles with varying water permeability rates to conduct comparative experiments. The results indicate that the differences in water permeability rates of acid treatment containers do not significantly impact the organic carbon isotope values.
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图 1 样品δ13Cacid与δ13Cker线性关系
Figure 1. The linear relationship between δ13Cacid and δ13Cker of samples
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图 2 不同岩性样品在不同|Δ13C|范围的数量统计
Figure 2. The quantitative statistics of samples with different lithology in different |Δ13C| value ranges.
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图 3 不同有机碳含量样品在不同|Δ13C|范围的数量统计
Figure 3. The quantitative statistics of samples with different TOC content in different |Δ13C| value ranges.
表 1 实验使用的标准物质及有机碳含量
Table 1 Details of reference materials and their organic carbon content
测试项目 标准物质编号 研制单位 有机碳含量推荐值(%)或
同位素组成δ13C推荐值(‰)总有机碳含量 GBW01117 江苏省铸造热处理研究所 3.08±0.02 501-676 美国力可公司 0.13±0.04 501-024 美国力可公司 3.19±0.03 502-694 美国力可公司 10.80±0.26 碳同位素组成 GBW（E）04407 石油勘探开发科学研究院 −22.43±0.3 GBW（E）04408 石油勘探开发科学研究院 −36.93±0.3 USGS24 美国地质调查局 −16.05±0.3 NBS-22 国际原子能机构 −30.03±0.05 
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表 2 样品岩性信息及TOC、δ13Cker、δ13Cacid、Δ13C测定结果
Table 2 Lithological information of samples and measured results of TOC, δ13Cker, δ13Cacid and Δ13C
样品岩性 样品数量
(件)TOC(%) δ13Cker(‰) δ13Cacid(‰) Δ13C(‰) 测定值范围 平均值 测定值范围 平均值 测定值范围 平均值 测定值范围 平均值 灰岩 39 0.83～18.69 9.62 −27.5～−22.2 −24.6 −27.3～−22.4 −24.4 −0.3～1.1 0.2 页岩 59 0.87～35.33 11.73 −34.6～−21.8 −26.3 −34.5～−20.0 −26.2 −2.8～1.8 0.1 油页岩 12 6.53～21.94 14.25 −25.8～−21.5 −24.0 −25.9～−21.1 −23.8 −0.6～0.5 0.2
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表 3 三种坩埚酸处理取得的δ13C测定结果
Table 3 The measurement results of δ13C obtained by acid treatment with three crucibles.
样品编号 δ13C测定值(‰) δ13C测定平均值
(‰)δ13C测定值
标准偏差(‰)Ⅰ型坩埚 Ⅱ型坩埚 Ⅲ型坩埚 页岩1 −33.8 −34.1 −34.1 −34.0 0.2 页岩2 −32.8 −32.8 −32.9 −32.8 0.1 页岩3 −31.3 −31.4 −31.3 −31.3 0.1 页岩4 −30.7 −30.7 −30.8 −30.7 0.1 页岩5 −30.3 −30.5 −30.5 −30.4 0.1 页岩6 −29.5 −29.4 −29.5 −29.5 0.1 页岩7 −29.4 −29.3 −29.2 −29.3 0.1 页岩8 −28.4 −28.3 −28.4 −28.4 0.1 灰岩1 −27.2 −27.3 −27.3 −27.3 0.1 灰岩2 −26.5 −26.6 −26.6 −26.6 0.1
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