Nitrogen Mass Fraction and Stable Isotope Ratios for Fourteen Geological Reference Materials: Evaluating the Applicability of Elemental Analyser Versus Sealed Tube Combustion Methods,Geostandards and Geoanalytical Research

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Nitrogen Mass Fraction and Stable Isotope Ratios for Fourteen Geological Reference Materials: Evaluating the Applicability of Elemental Analyser Versus Sealed Tube Combustion Methods
Geostandards and Geoanalytical Research ( IF 2.7 ) Pub Date : 2020-06-02 , DOI: 10.1111/ggr.12345
Toby J. Boocock ₁ , Sami Mikhail ₁ , Julie Prytulak ₂ , Tommaso Di Rocco _{1,

3} , Eva E. Stüeken ₁

Affiliation

Thirteen commercially available silicate reference materials (RM) and one in‐house reference material, eleven of which have no previously published values, were analysed for nitrogen mass fraction and isotopic ratios with an Elemental Analyser (EA), and a Sealed Tube Combustion line, coupled to a continuous flow isotope ratio mass spectrometer (IRMS). These materials ranged from < 10 μg g⁻¹ to 1% m /m nitrogen mass fractions and δ¹⁵N of −0.5 to +19.8‰. Existing nitrogen RM BHVO‐2, MS#5 and SGR‐1b were used to assess the accuracy of the data from the sealed tube combustion line, which was found to be in good agreement with existing published values. In contrast, the EA‐IRMS failed to fully liberate nitrogen from all silicate rocks and minerals (achieving a mean of 44 ± 10% nitrogen yield) resulting in kinetic fractionation of isotope values by −1.4‰ on average. Therefore, sealed tube combustion is better suited for analyses of silicate‐bound nitrogen. The EA worked reliably for organic samples, but care should be taken when using the EA for silicate nitrogen research. Moving forward, it is recommended that BHVO‐2, Biotite‐Fe, FK‐N and UB‐N be used as quality control materials as they appear to be most reproducible in terms of nitrogen mass fraction (relative error < 10%, 1s ), and isotopic composition (< 0.6‰, 1s ).

中文翻译：

十四种地质参考物质的氮质量分数和稳定同位素比：评估元素分析仪与密封管燃烧方法的适用性

使用元素分析仪（EA）和密封管燃烧线分析了13种市售的硅酸盐参考物质（RM）和一种内部参考物质，其中11种没有以前公布的值，分析了氮的质量分数和同位素比，与连续流动同位素比质谱仪（IRMS）耦合。这些材料从<10微克克范围^-1〜1％米/米氮质量分数和δ ¹⁵N为-0.5至+ 19.8‰。现有的氮气RM BHVO-2，MS＃5和SGR-1b用于评估密封管燃烧管线数据的准确性，发现该数据与现有公布的值高度吻合。相比之下，EA‐IRMS无法从所有硅酸盐岩和矿物中完全释放出氮（平均氮产率为44±10％），从而导致同位素值的动态分级平均为-1.4‰。因此，密封管燃烧更适合硅酸盐结合氮的分析。EA可以可靠地用于有机样品，但是在使用EA进行硅酸盐氮研究时应格外小心。展望未来，建议将BHVO-2，Biotite-Fe，FK-N和UB-N用作质量控制材料，因为它们似乎在氮质量分数方面具有最高的再现性（相对误差<10％，1s）和同位素组成（<0.6‰，1 s）。

更新日期：2020-06-02

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