Formation of either sodium jarosite or lead jarosite from concentrated chloride solutions containing small concentrations of sulphate has been demonstrated. Sodium jarosite is precipitated at 95-100C from FeC13-FeCI2-NaCI-PbCI2 solutions to which was added Na2SO4 or Li2SO4 in amounts greater than 0.05 M. In the absence of alkali metal ions capable of forming jarosites, lead jarosite was precipitated from either FeCI3-PbCI2 or FeCI3-FeCI2-LiCI-PbCI2 solutions to which had been added small amounts of sulphate. Many of the factors affecting jarosite precipitation from chloride solution have been elucidated, and the most critical were sulphate concentration and initial pH. Concentrations of HCI in excess of O. I M essentially suppressed the production of jarosite in chloride media. Alkali jarosite, precipitated in the presence of dissolved lead, incorporates a small amount of this metal into the alkali jarosite lattice. Small but significant amounts of copper can also be incorporated into alkali jarosite and the amount is further increased in the presence of lead. Other divalent base metals such as Zn, Cd or Ni are not significantly precipitated. Sulphate control in either FeCI3 or FeCl3-NaCI leaching systems could likely be maintained by jarosite precipitation provided that the acid concentration of the solution was low.