A laboratory exercise was developed by using variable temperature powder X-ray diffraction (XRD) to determine [alpha] for MgO (periclase)and was tested in the Applied Physical Chemistry and Materials Characterization Laboratories at James Madison University. The experiment which was originally designed to provide undergraduate students with a brief introduction in using powder X-ray diffraction to identify a solid and to measure lattice parameters could also be used for an integrated physical chemistry and instrumental analysis laboratory or an advanced materials science laboratory.