Several biomass types, such as yeast (in the present Saccharomyces, a brewery waste), have been reported to remove heavy metals (i.e., zinc) from aqueous solution. The separation of metal-loaded biomass and hence, the production of a clean water stream using a hybrid flotation-microfiltration unit were investigated. The hybrid cell consisted of a microfiltration module submerged directly into a flotation cell. Air bubbling, constituting the transport medium during flotation, meanwhile has been used in order to limit the membranes fouling. The effects of air sparging, the solid particle content, and the type and concentration of flotation reagents on the performance of the hybrid process were the main examined parameters.