This chapter reviews the research on morphology development in polymer blends and describes the different experimental methodologies used to determine blend morphology in three different types of polymer processing equipment: twin screw extruder, single-screw extruder, and twin rotor batch mixer. It describes some miniature mixing devices that have been used for specialty materials available in milligram quantities. For postmortem morphology analysis, sample preparation may require a few minutes or a few hours for each sample, depending on the imaging technique. Light scattering has been used for morphology characterization for postmortem samples and for analysis inline. When polymer blends are prepared from a mixture of solid pellets or powder, the melting order of the components is important in determining the morphology development. The morphology created in the Alberta Polymer Asymmetric Minimixer matched those found in batch mixer and twin-screw extruder, and was superior to that created in standard operation of a MiniMax mixer.