A complex of techniques for purification of antimony from arsenic has been examined with the aid of radiotracer ⁷⁶As. The investigated processes comprised vacuum distillation, zone melting and remelting of the metal under artificial slags. The purification efficiencies for the above processes were high and amounted to 94% (for 30% of the charge), 50% (for 50% of the charge) and 99.5% (for 60% of the charge), respectively. The application of the radioactive tracer made it possible to determine rapidly the distribution of impurities after each stage of the process within a wide concentration range (10^-2 – 10^-7 g/g).