Separation of zinc (II) and iron (III), present in acidic HCl solutions, with tri-n-octylamine was studied applying a rotating film pertraction (RFP) technique. The effect of the main process parameters, disc rotation velocity and hydrochloric acid concentration in the feed, was investigated. It was found that tri-n-octylamine is a suitable extractant for zinc recovery or Zn/Fe separation from chloride media. High feed acidity favors more complete zinc recovery, while moderate HCl concentration ([HCl] = 0.25 mol/L) provides much better separation of the metals. The lower acidity (less than 0.10 mol/L) is recommended when pure zinc strip solution is aimed at.