Atmosphere XRD measurement technique for iron compound of reduced state

Otsuka, Ichiro*; Tanaka, Tadao ; Inada, Daisuke*

The experiments to elucidate physico-chemical behavior of iron in the low oxygen and reducing condition of deep underground geology have been performed carefully in the glove box controlling oxygen concentration. It is necessary to protect oxidation by oxygen for XRD measurement of Fe(II) compounds that easily oxidize in atmosphere. In the present research, the method to measure XRD of the Fe(II) compounds was proposed. In the argon gas circulating type glove box controlled in oxygen concentration less than 1 ppm, Fe(OH) was prepared. Resulting Fe(OH) was pasted to surface of glass cell, and was sealed by Kapton film. The glass cell was taken out into atmosphere from a glove box and XRD measurement was performed. As to the cell sealed up by Kapton film, only peaks of Fe(OH) was observed. This experimental result shows that the XRD measurement of Fe(OH) in atmosphere is possible by sealing up the sample on glass cell by Kapton film.