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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

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

  • 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。

     

    Abstract:
    BACKGROUNDOrganic 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.
    OBJECTIVESTo develop a method for determining organic carbon and nitrogen stable isotopes in marine sediments.
    METHODSThree 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.
    RESULTSThe 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.
    CONCLUSIONSThrough 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.

     

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