The aim of this study is develop a procedure to separation of iodine from intermediate level radioactive waste. The total activity of radionuclide 129I is limited in near surface repository Mochovce and the total limit is 4.58*10E+11 Bq. Proposed procedure consists of several separation and preconcentration steps like distillation, extraction chromatography by means CL-Resin and precipitation. This separation method ensures to determine 129I activity and or reach very low values of MDAs. The sample is prepared as a palladium iodide precipitate for measurements.