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A high-throughput system for boron microsublimation and isotope analysis by total evaporation thermal ionization mass spectrometry

机译:通过全蒸发热电离质谱法进行硼微升华和同位素分析的高通量系统

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摘要

RATIONALE: Research on the ocean carbon cycle is vitally important due to the projected impacts of atmospheric CO_2 on global temperatures and climate change, but also on ocean chemistry. The direct influence of this CO_2 rise on the seawater pH can be evaluated from the boron isotopic composition in biogenic carbonates; however, conscientious laboratory techniques and data treatment are vital in obtaining accurate and precise results. A rapid-throughput boron purification and Total Evaporation Thermal Ionization Mass Spectrometry method was developed for high accuracy and precision boron isotopic analysis for small (ng) sample sizes. METHODS: An improved microsublimation method, in which up to 20 samples can be processed simultaneously under identical temperature conditions, was developed. Several tests have confirmed the viability of this technique. First, seawater and Porites coral samples were processed with H_2O_2 and the results compared with those obtained using microsublimation; second, the impact of various sublimation times was evaluated; and third, quantitative recovery was assessed using standard addition. RESULTS: Microsublimation provides a valid method for the quantitative recovery and separation of boron from both major elements and organic matter under low-blank conditions. The close agreement of our results with published values validates the accuracy of the measurements. The isotopic ratio for SRM 951a boric acid isotopic standard was 4.0328±0.0054 (2 STD, n = 25). The reproducibility of boron isotopic composition for standards including AE121, IAEA B-1 and an in-house coral standard UM-CP1 was ±0.68% (2 STD, n = 15), ±1.12% (2 STD, n = 24), and ±1.17% (2 STD, n = 14), respectively. The sample sizes were <1 ng for each measurement. CONCLUSIONS: The developed method for preparing and measuring boron isotopic values in a variety of carbonate materials should facilitate the reconstruction of past ocean pH conditions with decadal-scale resolution.
机译:理由:由于预计大气中的CO_2对全球温度和气候变化以及海洋化学的影响,因此对海洋碳循环的研究至关重要。可以从生物碳酸盐中的硼同位素组成来评估这种CO_2升高对海水pH值的直接影响。但是,认真的实验室技术和数据处理对于获得准确和精确的结果至关重要。开发了一种快速通量的硼纯化和总蒸发热电离质谱法,用于对小样本(ng)的样品进行高精度和精密的硼同位素分析。方法:开发了一种改进的微升华方法,其中在相同温度条件下最多可同时处理20个样品。几项测试证实了该技术的可行性。首先,用H_2O_2处理海水和Porites珊瑚样品,并将结果与​​微升华方法进行比较。其次,评估了各种升华时间的影响。第三,使用标准添加物评估定量回收率。结果:微升华提供了一种在低空白条件下从主要元素和有机物中定量回收和分离硼的有效方法。我们的结果与已公布的值非常吻合,验证了测量的准确性。 SRM 951a硼酸同位素标准品的同位素比为4.0328±0.0054(2 STD,n = 25)。包括AE121,IAEA B-1和室内珊瑚标准UM-CP1在内的硼同位素组成的重现性为±0.68%(2 STD,n = 15),±1.12%(2 STD,n = 24),和±1.17%(2 STD,n = 14)。每次测量的样本量小于1 ng。结论:开发的用于制备和测量多种碳酸盐材料中硼同位素值的方法应有助于以数十个尺度的分辨率重建过去的海洋pH条件。

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