A methodology of preparing high purity Al-13 through chemical precipitation/separation was developed. Polyaluminum chloride (PACl) with medium high concentration (0.1-1.1 mol/L as Al) was used as the source of Al-13. The factors that affect separation process were thoroughly examined. Intermediate and final products of Al-13 were characterized morphologically and structurally using SEM, XRD, and solid-state 27 Al NMR. The purity of obtained Al-13 product was verified using both ferron assay and Al-27 NMR. It was found that the separation of Al-13 from medium high concentration PACl was feasible and the purity of Al-13 product could be higher than 95%. (C) 2006 Elsevier B.V. All rights reserved.