The coprecipitation method was used to prepare Mg-Al Hydrotalcite-like compounds (HTlcs). The precipitated and calcined Mg-Al HTlcs were characterized using powder X-Ray Diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. The XRD patterns for the materials indicated the presence of the hydrotalcite structure. The IR spectrum for calcined Mg-Al HTlcs with Mg/Al molar ratio of 2 showed reduction in water and C02 characteristics due to their removal during calcination. Subsequent to the calcination, the materials were reduced using Temperature Programmed Reduction (TPR) in order to determine the H2 uptake. The H2 gas consumption was found to be very small and further modifications of the material synthesis are required to yield better results. © 2010 Asian Network for Scientific Information.