Dublyansky Yuri V, Spötl Christoph
Institut für Geologie und Paläontologie, Leopold-Franzens-Universität, Innrain 52, 6020 Innsbruck, Austria.
Rapid Commun Mass Spectrom. 2009 Sep;23(17):2605-13. doi: 10.1002/rcm.4155.
An analytical line for stable isotope analyses of water recovered from fluid inclusions in minerals was built and successfully tested. The line is based on the principle of continuous-flow analysis of water via high-temperature reduction on glassy carbon. It includes a custom-designed set of high-efficiency crushers and a cryo-focusing cell. This paper provides details of the line design and discusses strategies for line conditioning and mitigation of memory effects. The line allows measurements of hydrogen and oxygen isotopes during a single acquisition. The precision of the analyses depends on the amount of water released from the inclusions. The best results are obtained for samples containing at least 0.1-0.2 microL (0.06-0.11 micromol) H(2)O. For such samples precision is better than 1.5 per thousand for deltaD and 0.5 per thousand for delta(18)O (1sigma). Smaller amounts of water can be measured but at lower precision. Analyses of modern calcite formed under stable conditions in a deep cave allowed assessment of the accuracy of the analyses. The deltaD values measured in fluid inclusions of this working standard match the deltaD value of the parent water, and the oxygen isotope values agree within ca. 0.5 per thousand. This indicates that fluid inclusions trapped in calcite at near-ambient temperatures (e.g. speleothems and low-temperatures phreatic calcite) faithfully preserve the original isotopic composition of the parent waters.
建立了一条用于对从矿物流体包裹体中回收的水进行稳定同位素分析的分析线,并成功进行了测试。该分析线基于通过在玻璃碳上进行高温还原对水进行连续流分析的原理。它包括一组定制设计的高效破碎机和一个低温聚焦池。本文详细介绍了该分析线的设计,并讨论了分析线调节和记忆效应减轻策略。该分析线允许在一次采集过程中测量氢和氧同位素。分析的精度取决于从包裹体中释放出的水量。对于至少含有0.1 - 0.2微升(0.06 - 0.11微摩尔)H₂O的样品可获得最佳结果。对于此类样品,δD的精度优于1.5‰,δ¹⁸O的精度优于0.5‰(1σ)。可以测量较少量的水,但精度较低。对在深洞穴稳定条件下形成的现代方解石进行分析,从而评估了分析的准确性。在该工作标准的流体包裹体中测得的δD值与母水的δD值相符,氧同位素值在约0.5‰范围内一致。这表明在接近环境温度下(例如洞穴沉积物和低温潜水方解石)被困在方解石中的流体包裹体忠实地保留了母水的原始同位素组成。