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Oxygen Isotope Analysis of Cellulose: An Interlaboratory Comparison

机译:纤维素的氧同位素分析:实验室间的比较

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Oxygen isotope analysis of tree ring cellulose is hindered by the lack of a fast and reliable technique to measure δ↑(18)O at natural abundance levels. Most of the existing off-line techniques are not conducive to rapid generation of oxygen isotope data. Further, a comparison between oxygen isotope values of a cellulose sample measured using the different off-line techniques resulted in a discrepancy of 1.3‰. This discrepancy is a result of inconsistencies inherent to these techniques and the lack of a reliable cellulose oxygen isotope standard. We addressed these problems by analyzing a number of cellulose samples by three different analytical procedures. These include two relatively well established off-line methods (pyrolysis in nickel tubes and decomposition using mercury(II) chloride) and a recently proposed online method based on pyrolysis in the presence of glassy carbon in an elemental analyzer and the subsequent isotope analysis of carbon monoxide. We were successful in improving the reproducibility of the on-line method(σ↓(n-1) ≈0.2‰) to the extent that natural variations can be resolved and found a good agreement between the on-line and off-line methods, although the cellulose samples extracted from tree rings are subject to more scatter than the commercial cellulose samples. The on-line method may even allow determination of δ↑(13)C and δ↑(18)O of a cellulose sample in a single run (from 29/28 and 30/28 ratios of CO).
机译:树环纤维素的氧同位素分析由于缺乏在自然丰度水平下测量δ↑(18)O的快速而可靠的技术而受到阻碍。大多数现有的离线技术都不利于氧同位素数据的快速生成。此外,使用不同离线技术测量的纤维素样品的氧同位素值之间的比较导致差异1.3‰。这些差异是由于这些技术固有的不一致以及缺乏可靠的纤维素氧同位素标准所导致的。我们通过三种不同的分析程序分析了许多纤维素样品,从而解决了这些问题。这些方法包括两种相对完善的离线方法(在镍管中热解和使用氯化汞分解),以及最近提出的在线方法,该方法基于在元素分析仪中玻璃态碳存在下的热解和随后的碳同位素分析一氧化碳。我们成功地提高了在线方法的可重复性(σ↓(n-1)≈0.2‰),以至于可以解决自然变化,并在在线方法与离线方法之间找到了很好的一致性,尽管从树年轮中提取的纤维素样品比商用纤维素样品具有更大的分散性。在线方法甚至可以单次测定纤维素样品的δ↑(13)C和δ↑(18)O(从CO的29/28和30/28比率)。

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