As increasingly commented by the literature during the last 5 years, estimating the homogeneity of a powder mixture and following powder mixing processes is not a simple task. In this paper, we present the development and statistical validation of a sampling methodology for defining the number of samples required to provide a reasonable estimation of the homogeneity attained in a laboratory scale tumbler mixer. This method is then used to follow the mixing kinetics of a dilute binary powder mixture in a hoop mixer. Special attention is paid to the statistical meaning of the values obtained and the influence of the physical characteristics such as particle size and shape. The role of the particle shape of the majority powder is particularly emphasised and it is quantitatively demonstrated that spherical particles are harder to mix and more ready to segregate than particles with irregular shapes. The different mixing mechanisms at play are identified; the practical limits of use of such tumbler mixers with pharmaceutical powders are discussed.