The incremental diffusion couples are used for evaluating interdiffusion couples in a narrow composition range and these results are extrapolated to get an estimate of impurity diffusion coefficients. In fact, several incremental couples are needed to get impurity diffusion coefficients at different compositions. This process is generally tedious. The present method describes a relatively simple method for evaluating the diffusion coefficients using “step diffusion couples”. A simple experimental method is described to prepare a step diffusion couple. This method involves preparation of diffusion couples in two stages. In the first stage, diffusion couple is made between the two materials in a conventional way and annealed for extended period of time to have a large diffusion zone typically of the order of 2-3 mm. In the second stage, the starting materials are placed on the diffusion couple in a direction perpendicular to the diffusion zone and annealed at a suitable temperature for diffusion to occur between the diffusion zone and the starting materials. This method is applied to study the interdiffusion behavior in the b phase of the Ti-Zr system. Boltzmann-Matano and Hall’s methods were used to determine the interdiffusion coefficients and their composition dependence. Kirkendall shift is observed towards Ti side and the intrinsic diffusion coefficients of Ti is approximately three times that of Zr. The width of the diffusion zone is strongly dependent on the composition of the step diffusion couple. It is observed that the interdiffusion coefficients evaluated at the terminal compositions matched well those published values in the Ti-Zr system. This experimental technique offers an easy and elegant method to determine the diffusion parameters without the tedious preparation of incremental diffusion couples.