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X-射线衍射晶体结构的分析是确定化合物结构的常用方法之一。对空气敏感的化合物通常采用装毛细管的方法进行。文献上曾有关于金属有机化合物进行X-射线衍射晶体结构分析结果的报道,但保护技术并无详细记载。我们认为,对微量氧和水份十分敏感的化合物进行X-射线结构分析时,如何将大小约为100μm~3晶体试样在惰性气体保护下封入薄壁毛细管是问题的关键。黄吉玲曾介绍了西德马普学会煤炭研究所建立的“裤形管”分装技术,分装对空气敏感的化合物。但对空气和湿度都敏感的化合物,则要在低温操作箱中进行。
Analysis of X-ray diffraction crystal structures is one of the common methods of determining the structure of a compound. Air-sensitive compounds are usually packed in capillaries. There have been reports about the results of X-ray diffraction crystal structure analysis of metal organic compounds in the literature, but the protection technique is not described in detail. In our opinion, how to encapsulate thin-walled capillaries with a size of about 100μm ~ 3 under inert gas protection is the crux of the problem when performing X-ray structural analysis of trace oxygen and water-sensitive compounds. Huang Jiling introduced the “pants-shaped tube” dispensing technology established by the Coal Research Institute of the Western Democrats to dispense air-sensitive compounds. However, both air and humidity sensitive compounds, it is necessary to carry out low-temperature operation box.