Leaching and recovery processes for zinc and copper from brass slag by sulfuric acid were carried out and iron and aluminum were also precipitated as hydroxides in addition to silica gel. The factors affecting the performance and efficiency of the leaching processsuch as agitation rate, leaching time, acid concentration and temperature were separately investigated. The results obtained revealed that zinc and copper are successfully recovered from these secondary resources, where the percent recovery amounts to 95% and 99% for zinc and copper, respectively. The experimental data of this leaching process were well interpreted with the shrinking core model under chemically controlled processes. The apparent activation energy for the leaching of zinc has been evaluated using the Arrhenius expression. Based on the experimental results, a separation method and a flow sheet were developed and tested to separate zinc, copper, iron, aluminum and silica gel from the brass slag.