The process of releasing hydrogen from nickel foil permeated with hydrogen is investigated by XRD and a laboratory EXAFS equipment which is attached on a X-ray spectrometer. The results obtained by these two methods show that the phase content of NiH decrease exponentially in this process We also determine a definite atomic ratio of Ni and H in NiH phase and point out the location of hydrogen in the lattice. This laboratory. EXAFS equipment is proved to be suitable for the study of this kind of problem.