High precision MC-ICP-MS measurements of 11B/10B ratios from ng amounts of boron in carbonate samples using microsublimation and direct injection (μ-dDIHEN),Journal of Analytical Atomic Spectrometry

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High precision MC-ICP-MS measurements of 11B/10B ratios from ng amounts of boron in carbonate samples using microsublimation and direct injection (μ-dDIHEN)
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2021-08-03 , DOI: 10.1039/d1ja00109d
Matthieu Buisson ₁ , Pascale Louvat ₁ , Caroline Thaler ₁ , Claire Rollion-Bard ₁

Affiliation

The boron isotopic ratio (δ¹¹B) of marine biogenic carbonates is a proxy for ocean pH through the geological times, provided that δ¹¹B measurements reach precisions better than 0.8‰ (2 SD), corresponding to 0.1 pH-unit (magnitude of the Anthropocene ocean acidification). This level of precision is however challenging to achieve for samples with a small size and low B content used in paleoceanographic reconstructions. We developed a protocol combining (i) the fast-handling and very low blank (9 ± 7 pg, 1 SD, n = 7) microsublimation technique to purify boron from the carbonate matrix and (ii) the direct injection of the samples into the MC-ICP-MS plasma with the new μ-dDIHEN device, allowing for small sample volumes and low uptake rates. We further used Jet sampler and X skimmer cones and implemented two 10¹³ Ω amplifiers to respectively increase the sensitivity and enhance the signal/noise ratio, enabling the precise measurement of small B signals. Our protocol, that consumes only 240 μL for one triplicate sample-standard bracketing (SSB) measurement, was validated through repeated B extractions and measurements of the carbonate reference material MVS-1 at different B concentrations. It yielded 15.93 ± 0.24‰ (2 SD, n = 10) with only 1.2 ng consumed for one triplicate SSB measurement, with individual external repeatabilities (n = 5, 2 SD) of 0.19 ± 0.14‰. We further measured δ¹¹B of modern biogenic carbonates (arthropods, brachiopods, molluscs, red algae and reef carbonate mixes) down to 0.5–0.7 ng of B and successfully compared these δ¹¹B values with those obtained after B extraction of the same samples through ion exchange chromatography.

中文翻译：

使用微升华和直接进样 (μ-dDIHEN) 对碳酸盐样品中 ng 量硼的 11B/10B 比率进行高精度 MC-ICP-MS 测量

海洋生物碳酸盐的硼同位素比 ( δ ¹¹ B) 是整个地质时代海洋 pH 值的代表，前提是δ ¹¹ B 测量值达到优于 0.8‰ (2 SD) 的精度，对应于 0.1 pH 单位（幅度为人类世海洋酸化）。然而，对于古海洋重建中使用的小尺寸和低 B 含量的样本，要达到这种精度水平是具有挑战性的。我们开发了一种结合 (i) 快速处理和非常低的空白 (9 ± 7 pg, 1 SD, n= 7) 从碳酸盐基质中纯化硼的微升华技术，以及 (ii) 使用新的 μ-dDIHEN 设备将样品直接注入 MC-ICP-MS 等离子体中，从而实现小样品体积和低吸收率。我们进一步使用了 Jet 采样器和 X 截取锥并实现了两个 10 ¹³ Ω 放大器，分别提高灵敏度和提高信噪比，从而实现小 B 信号的精确测量。我们的协议，一次重复样品标准包围 (SSB) 测量仅消耗 240 μL，通过重复 B 提取和不同 B 浓度下碳酸盐参考材料 MVS-1 的测量得到验证。它产生了 15.93 ± 0.24‰ (2 SD, n= 10) 一次重复 SSB 测量仅消耗 1.2 ng，单个外部重复性 ( n = 5, 2 SD) 为 0.19 ± 0.14‰。我们进一步测量δ ¹¹现代生物碳酸盐（节肢动物，腕足动物，软体动物，红藻和礁碳酸盐混合）下的B至0.5-0.7纳克B的，并成功地比较这些δ ¹¹ B值与相同样品的乙提取之后获得的那些通过离子交换层析。

更新日期：2021-08-24

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