【引用本文】 常文博, 李凤, 张媛媛, 等. 元素分析-同位素比值质谱法测量海洋沉积物中有机碳和氮稳定同位素组成的实验室间比对研究[J]. 岩矿测试, 2020, 39(4): 535-545. doi: 10.15898/j.cnki.11-2131/td.202003090027
CHANG Wen-bo, LI Feng, ZHANG Yuan-yuan, et al. Inter-Laboratory Comparison of Measuring Organic Carbon and Stable Nitrogen Isotopes in Marine Sediments by Elemental Analysis-Isotope Ratio Mass Spectrometry[J]. Rock and Mineral Analysis, 2020, 39(4): 535-545. doi: 10.15898/j.cnki.11-2131/td.202003090027

元素分析-同位素比值质谱法测量海洋沉积物中有机碳和氮稳定同位素组成的实验室间比对研究

青岛海洋地质研究所, 山东 青岛 266071

收稿日期: 2020-03-09  修回日期: 2020-04-13  接受日期: 2020-06-02

基金项目: 中国地质调查局地质调查项目“研制海底沉积物有机碳氮稳定同位素标准物质和标准方法”(12120113022000)

作者简介: 常文博, 硕士, 研究实习员, 从事同位素及地质年代学分析测试研究。E-mail:susanna0703@163.com

通信作者: 贺行良, 博士, 高级工程师, 主要从事海洋生物地球化学及标准化研究。E-mail:76791772@qq.com

Inter-Laboratory Comparison of Measuring Organic Carbon and Stable Nitrogen Isotopes in Marine Sediments by Elemental Analysis-Isotope Ratio Mass Spectrometry

Qingdao Institute of Marine Geology, Qingdao 266071, China

Corresponding author: HE Xing-liang, 76791772@qq.com

Received Date: 2020-03-09
Revised Date: 2020-04-13
Accepted Date: 2020-06-02

摘要:海洋沉积物中有机碳、氮稳定同位素(δ13C、δ15N)作为一种有效指标,可对不同地质时期空气、温度、降水等参数的变化进行标记。元素分析-同位素比值质谱法是一种测量海洋沉积物有机碳、氮稳定同位素组成的合理、有效的方法。目前我国有诸多实验室使用元素分析仪(EA)与稳定同位素比值质谱仪(IRMS)联用的方法对沉积物中的有机碳、氮稳定同位素进行测试。各实验室之间测试技术及数据稳定性缺少比对依据,测试结果缺乏有效的溯源,使用过程中缺乏规范和统一。本文选取了我国2018年研制的三个国家一级海洋沉积物碳氮稳定同位素标准物质(GBW04701、GBW04702、GBW04703)及两个国际标准物质(EMA-B2152、EMA-B2151),在我国十家实验室对EA-IRMS在线技术测试方法进行实验室间的测量比对实验,以验证方法的稳定性、精密度和准确度。测试结果表明:各家协作实验室的数据准确、稳定,方法的重复性和再现性良好,测得的δ13C和δ15N精密度分别好于0.10‰、0.14‰。通过比对研究,同时证明了EA-IRMS在线技术适用于海洋沉积物中的有机碳、氮稳定同位素的测定,初步建立了一套适合海洋沉积物样品分析的方法。

关键词: 元素分析-同位素比值质谱法, 海洋沉积物, 有机碳稳定同位素, 氮稳定同位素, 比对研究

要点

(1)在我国十家实验室对海洋沉积物中有机碳、氮稳定同位素测试结果进行比较,取得较好精密度。

(2)验证了EA-IRMS对海洋沉积物中有机碳、氮稳定同位素测定的适用性。

(3)为EA-IRMS检测海洋沉积物中有机碳、氮稳定同位素提供了参考。

Inter-Laboratory Comparison of Measuring Organic Carbon and Stable Nitrogen Isotopes in Marine Sediments by Elemental Analysis-Isotope Ratio Mass Spectrometry

ABSTRACT

BACKGROUND:

Organic carbon and nitrogen stable isotopes (δ13C, δ15N) in marine sediments are used as effective indicators to trace the changes of air, temperature, precipitation and other parameters in different geological time. Elemental analysis-isotope ratio mass spectrometry is a reasonable and effective method to measure the composition of organic carbon and nitrogen stable isotopes in marine sediments. At present, many domestic laboratories use the method of element analyzer (EA) and stable isotope ratio mass spectrometer (IRMS) to analyze the stable isotopes of organic carbon and nitrogen. However, the comparison of analytical method and data stability between different laboratories is lacking. The analytical results lack effective traceability, and the process lacks standardization and unification.

OBJECTIVES:

To develop a method for determining organic carbon and nitrogen stable isotopes in marine sediments.

METHODS:

Three newly developed national first-class standard materials (GBW04701, GBW04702, GBW04703) and two international standard materials (EMA-B2152, EMA-B2151) were sent to 10 domestic laboratories, in order to verify the stability, precision and accuracy of EA-IRMS online technology test method through the comparative measurement between laboratories.

RESULTS:

The data of each collaborative laboratory was accurate and stable, and the method had good repeatability and reproducibility. The results showed that precisions of 13C and 15N were better than 0.10‰ and 0.14‰, respectively.

CONCLUSIONS:

Through comparative study, it has been proved that EA-IRMS online technology is suitable for the determination of organic carbon and nitrogen stable isotopes in marine sediments. A suitable method for the determination of marine sediment samples has been preliminarily established.

KEY WORDS: elemental analysis-isotope ratio mass spectrometry, marine sediments, organic stable carbon isotopes, nitrogen stable isotopes, comparative research

Highlights

(1) The comparison of analytical results of organic carbon and nitrogen isotopes in marine sediments has been carried out in ten laboratories in China and good precision has been obtained.

(2) The applicability of EA-IRMS for the determination of organic carbon and nitrogen stable isotopes in marine sediments was verified.

(3) A reference for using EA-IRMS to determine organic carbon and nitrogen stable isotopes in marine sediments has been established.

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Figures And Tables

元素分析-同位素比值质谱法测量海洋沉积物中有机碳和氮稳定同位素组成的实验室间比对研究

常文博, 李凤, 张媛媛, 贺行良