Time-resolved powder diffraction using synchrotron X-ray radiation has been used for real-time studies of syntheses and chemical reactions. Recent studies from the NSLS beam line X7B are summarized. in situ cells for hydrothermal synthesis and gas how using quartz glass capillaries are described. A new translating imaging plate (TIP) camera for time-resolved powder diffraction experiments is also described. Measurement of full powder patterns in times as short as 30 s is essential to these studies. New results from in situ studies of hydrothermal synthesis of cobalt-substituted microporous aluminophosphates are presented.