论文部分内容阅读
不少有机金属化合物,特别是有机稀土金属化合物对微量空气、湿气极为敏感,因而它们的取样和分析技术具有一定的特殊性,并有专门介绍这方面技术的报道。最近我们得到一个四氢呋喃配位的有机镥配合物,它在四氢呋喃溶剂中能生成带溶剂配位的无色斜方晶体。当抽去溶剂或在通氩下,将晶体装入玻璃毛细管时,由于晶体在离开母液后失去配位溶剂分子而变成粉状,因而采用一般的取样方法得不到适用于x-射线晶体结构测定的单晶。为此,我们设计了一种新的单晶取样器(见附图),可以成功地取出单晶样品,并测定其晶体结构。该取样器加工简便,取样安全可靠,可连续取样,以便挑选合适的测试样品。现将装置及取样方法介绍于后。
Many organometallic compounds, especially organic rare earth metal compounds, are extremely sensitive to trace air and moisture. Therefore, their sampling and analysis techniques are of some particularities. Some reports have been devoted to this aspect of technology. Recently, we obtained a tetrahydrofuran coordination organic 镥 complex, which can generate solvent-coordinated colorless rhombic crystals in tetrahydrofuran solvent. When the solvent is removed or under argon, the crystals are loaded into the glass capillary, the crystals become powdered due to the loss of the coordination solvent molecules after leaving the mother liquor, and thus the general sampling method is not suitable for x-ray crystallography Structure determination of single crystal. To this end, we have designed a new single crystal sampler (see attached), which can successfully remove single crystal samples and determine their crystal structure. The sampler is easy to process, safe and reliable sampling, continuous sampling, in order to pick the right test samples. Now the installation and sampling methods introduced later.