In situ monitoring of hydrothermal reactions by X-ray diffraction with Bragg–Brentano geometry

This note describes an autoclave chamber developed and constructed by Anton Paar and its application for in situ experiments under hydrothermal conditions. Reactions of crystalline phases can be studied by successive in situ measurements on a conventional laboratory X-ray diffractometer with Bragg–Brentano geometry at temperatures <483 K and saturated vapour pressure <2 MPa. Variations in the intensity of X-ray diffraction reflections of both reactants and products provide quantitative information for studying the reaction kinetics of both dissolution and crystal growth. Feasibility is demonstrated by studying a cementitious mixture used for autoclaved aerated concrete production. During a period of 5.7 h at 466 K and 1.35 MPa, the crystallization of torbermorite and the partial consumption of quartz were monitored.