An X-ray diffraction method has been developed which was able to describe the diffusion zone produced by annealing nickel plated copper specimens at 750 degrees and 850 degrees. The experimental X-ray diffraction data were first corrected for instrumental broadening and then used to compute concentration-penetration curves across the diffusion zone. the experimental curves are in general agreement with a new mathematical analysis and also the diffusion coefficients reported in the literature. / Master of Science