Brunelli Michela, Fitch Andrew N
ESRF, BP 220, F38043 Grenoble, France.
J Synchrotron Radiat. 2003 Jul 1;10(Pt 4):337-9. doi: 10.1107/s0909049503007969. Epub 2003 Jun 24.
A rotating glass capillary cell with a gas handling system has been built to allow in situ studies by powder X-ray diffraction. The cell can be used to condense volatile compounds, or to follow solid-state chemical reactions under vacuum or at gas pressures up to around 7 x 10(5) Pa. Using the cell, cooled by a stream of helium gas, the solid phases of 1,2-dichlorotrifluoroethane (HCFC-123a) and 2-chloro-1,1,1,2-tetrafluoroethane (HCFC-124) have been investigated using powder synchrotron X-ray radiation. These were found to have disordered hexagonal structures, with a = 4.018 (5), c = 6.553 (1) A and a = 4.048 (1), c = 6.625 (1) A, respectively, at 64 K.
已构建了一个带有气体处理系统的旋转玻璃毛细管池，以便通过粉末X射线衍射进行原位研究。该池可用于冷凝挥发性化合物，或在真空或高达约7×10⁵帕的气体压力下跟踪固态化学反应。使用由氦气流冷却的该池，利用粉末同步加速器X射线辐射研究了1,2 - 二氯三氟乙烷（HCFC - 123a）和2 - 氯 - 1,1,1,2 - 四氟乙烷（HCFC - 124）的固相。发现在64K时，它们分别具有无序的六方结构，晶格参数a = 4.018(5)，c = 6.553(1) Å和a = 4.048(1)，c = 6.625(1) Å。
