This paper describes the preparation of samples for an experiment to measure the cross-section for 235U(n,n′)235mU in a fast fission spectrum of neutrons provided by a fast pulsed reactor/critical assembly. Samples of 235mU have been prepared for the calibration of the internal conversion electron detector that is used for the 235mU measurement. Two methods are described for the preparation of 235mU. The first method used a U-Pu chemical separation based on anion-exchange chromatography and the second method used an alpha
recoil collection method. Thin, uniform samples of 235mU+235U were prepared for the experiment using electrodeposition.