【引用本文】 胡志中, 晏雄, 王坤阳, 等. 碳酸盐碳氧同位素标准物质性状对分析和保存的影响[J]. 岩矿测试, 2021, 40(4): 476-490. doi: 10.15898/j.cnki.11-2131/td.202011150143
HU Zhi-zhong, YAN Xiong, WANG Kun-yang, et al. Characteristics of Carbon and Oxygen Isotope Standard Materials of Carbonates and Their Effect on Isotope Analysis and Standard Preservation[J]. Rock and Mineral Analysis, 2021, 40(4): 476-490. doi: 10.15898/j.cnki.11-2131/td.202011150143

碳酸盐碳氧同位素标准物质性状对分析和保存的影响

中国地质调查局成都地质调查中心, 四川 成都 610081

收稿日期: 2020-11-15  修回日期: 2021-03-19  接受日期: 2021-05-03

作者简介: 胡志中, 硕士, 高级工程师, 主要从事同位素和微区原位分析。E-mail: hzz_pot@aliyun.com

通信作者: 杜谷, 硕士, 教授级高级工程师, 主要从事岩石和矿物分析研究。E-mail: dugucgs@163.com

Characteristics of Carbon and Oxygen Isotope Standard Materials of Carbonates and Their Effect on Isotope Analysis and Standard Preservation

Chengdu Center of Geological Survey, China Geological Survey, Chengdu 610081, China

Corresponding author: DU Gu, dugucgs@163.com

Received Date: 2020-11-15
Revised Date: 2021-03-19
Accepted Date: 2021-05-03

摘要:碳酸盐物质碳氧同位素广泛应用于地质和气候环境研究,而标准物质是其分析的基准物质和数据比较的重要依据。不同标准物质性状存在差异,对于性状特点的了解,有助于标准的选择和使用、不均匀性的改善以及最佳实验条件的建立。本文采用X射线衍射(XRD)、光学显微镜及能谱扫描-电子显微镜(EDX-SEM)技术,从不同尺度对物源、粒径、颗粒形貌和结构,以及纯净程度等性状不同的碳酸盐碳氧同位素标准物质开展了观察和分析,并采用连续流磷酸法测定部分碳酸盐标准物质的δ13C和δ18O值,从而探讨其性状特点以及对分析和保存的影响。结果表明:天然碳酸盐标准物质普遍含有非碳酸钙成分,如少量石英;以及存在明显性状差异的颗粒,但总量较少。不同标准物质之间、标准物质颗粒之间也存在程度不同的粒径、形貌、微细结构和矿物组分等性状差异。实验测定了不同标准物质的δ13C和δ18O值,多数分析结果与推荐值吻合,其中IAEA-CO-8的δ13C和δ18O值标准偏差相比其他物质偏大,可能与该标准组成复杂且均一性较差有关,而NBS20的δ18O值标准偏差相对偏大以及7902的δ18O值与推荐值偏离较大,推测与其粉末状且组成颗粒细小的性状更容易受到空气中二氧化碳和水的影响有关。结合前人和本研究认为,在推荐使用量下天然碳酸盐标准物质性状对分析精准性造成的影响有限;而为了保证微量分析和研究的准确性,建议根据分析和研究目的,结合标准和物质的性状特点,有针对性地选择标准以及标准中的颗粒,同时粉末状且组成颗粒细小标准物质在制备和保存上需要更加注意。本研究补充和丰富了碳酸盐碳氧同位素标准物质的性状信息,有助于其更好地应用于微量碳酸盐碳氧同位素分析和研究,同时也为保存和制备提供参考。

关键词: 碳酸盐, 碳氧同位素, 标准物质, 矿物组成, 性状, 保存和制备

要点

(1) 采用多种分析技术从不同尺度直观揭示不同碳酸盐碳氧同位素标准物质的物源、粒径、颗粒形貌和结构,以及纯净程度的性状特征和差异。

(2) 对比分析和探讨了不同碳酸盐碳氧同位素标准物质的性状特点对δ13C和δ18O分析的影响。

(3) 为碳氧同位素标准物质的制备、保存提供了参考信息。

Characteristics of Carbon and Oxygen Isotope Standard Materials of Carbonates and Their Effect on Isotope Analysis and Standard Preservation

ABSTRACT

BACKGROUND:

Carbon and oxygen isotopes in carbonates are commonly used in geology and climate studies. Reference materials for these isotopes are an important basis for analysis and data comparison. Understanding the differences in the characteristics of different standard materials is helpful for the selection and use of standards, improvement of heterogeneity, and establishment of optimal experimental conditions.

OBJECTIVES:

To investigate the influence of the characteristics of carbon and oxygen isotope standard materials of carbonates on isotope analysis and preservation of the standards.

METHODS:

In this study, X-ray diffraction (XRD), optical microscopy, and energy dispersive X-ray scanning electron microscopy (EDX-SEM) were used to analyze carbonate carbon and oxygen isotope reference materials with different properties, such as provenance, particle size, particle morphology and structure, and purity. The δ13C and δ18O values of some carbonate reference materials were determined by the continuous flow phosphoric acid method to explore their characteristics and their influence on isotope analysis and standard preservation.

RESULTS:

Natural carbonate reference materials generally contain non-calcium carbonate components, such as small amounts of quartz and other particles with obvious differences in properties. There are also differences in particle size, morphology, microstructure, and mineral composition between different standard materials and between standard material particles. The δ13C and δ18O values of different standard materials were determined, and most results were consistent with the recommended values. The standard deviations of the δ13C and δ18O values of IAEA-CO-8 were larger than those of other standard materials, which is attributable to their complex composition and homogeneity. The standard deviation of the δ18O value of NBS20 was large, while the δ18O value of 7902 deviated from the recommended value. It is inferred that their powdery and fine particles are more likely to be affected by carbon dioxide and water in air.

CONCLUSIONS:

Based on previous research as well as the current study, it is believed that under the recommended usage amount, the properties of natural carbonate reference materials have a limited impact on the accuracy of analysis. To ensure the accuracy of microanalysis and research, while selecting the standard and the particles in the standard, it is recommended to combine the characteristics of standards and materials based on the purpose of the analysis and research. At the same time, the preparation and storage of powdery and fine-grained standard materials require more attention. This study supplements information regarding the properties of carbonate carbon and oxygen isotope standard materials, which helps in the analysis and research of trace carbonate carbon and oxygen isotopes, and provides a reference for standard preservation and preparation.

KEY WORDS: carbonate, carbon and oxygen isotope, standards and reference materials, mineral composition, character, preservation and preparation

HIGHLIGHTS

(1) Various characteristics, including provenance, particle size, particle morphology and structure, and purity of different carbon and oxygen isotope standard materials of carbonates were revealed using a variety of techniques.

(2) The influence of the characteristics of carbonate standard materials on carbon and oxygen isotope analysis was studied.

(3) The research was useful in the preparation and preservation of carbon and oxygen isotope standard materials.

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Figures And Tables

碳酸盐碳氧同位素标准物质性状对分析和保存的影响

胡志中, 晏雄, 王坤阳, 王冠, 潘忠习, 杜谷