Prediction analysis is a method for predicting the accuracy of experimental results as a function of the experimental variables and parameters. The method is useful for the design and planning of experiments. In this paper, the method is described and then applied to the problem of peak separation for which the purpose of the experiment is to determine the unknown amplitudes of two overlapping peaks. This problem is important in such areas as neutron cross section and gamma ray spectroscopy. Results useful for the design of such experiments are included in a dimensionless form.