Reduction in piston-cylinder experiments: The detection of carbon infiltration into platinum capsules
Reduction in piston-cylinder experiments: The detection of carbon infiltration into platinum capsules
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DOI：
10.2138/am-1998-9-1006
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发表时间：
1998-10
影响因子：
3.1
通讯作者：
R. Brooker;J. Holloway;R. Hervig
中科院分区：
文献类型：
--
作者：
R. Brooker;J. Holloway;R. Hervig
摘要在用活塞-圆筒装置制备含CO2硅酸盐玻璃的研究中，经常报告与样品间歇性和不同程度的变黑有关的问题。这种现象通常归因于H渗透，其导致CO2的还原和石墨的沉淀以及伴随的水的形成。在这项研究中，我们表明，碳扩散到铂胶囊可能是一个常见的原因变黑的玻璃和这个过程中可以检测到使用傅立叶变换红外光谱（FTIR），以确定CO的存在下，没有升高的H2O含量。使用二次离子质谱（西姆斯）和显微FTIR分析说明了12 C从石墨炉到含13 C样品中的模拟渗透。仔细FTIR监测变量样品减少有助于确定所需的预防措施，以减少C（和H）渗透固体介质组件，它似乎是物理屏障可能比传统上采用的化学缓冲液更重要。
Abstract Problems associated with intermittent and variable degrees of sample blackening are often reported for studies involving the preparation of CO2-bearing silicate glasses in piston- cylinder apparatus. This phenomenon is generally attributed to H infiltration, which leads to the reduction of CO2 and the precipitation of graphite with the concomitant formation of water. In this study we demonstrate that carbon diffusion into platinum capsules may be a common cause of blackened glasses and this process may be detected using fourier transform infrared spectroscopy (FTIR) to identify the presence of CO without elevated H2O contents. The simulated infiltration of 12C from a graphite furnace into a 13C -bearing sample is illustrated using secondary ion mass spectroscopy (SIMS) and micro- FTIR analysis. Careful FTIR monitoring of variable sample reduction has helped to identify the precautions required to reduce C (and H) infiltration in solid media assemblies and it appears that physical barriers can be more important than the chemical buffers traditionally employed.