Some sorbents impregnated with tetraoktyldiglycolamid were used for the separation of americium macroamounts from a number of pollutants. The effect of nitric and hydrochloric acids on neptunium (IV), uranium (VI), americium (III), europium (III), cerium (III), thorium (IV) and iron (III) sorption was studied. The optimal conditions for the separation of microamounts of cerium (III), sodium, potassium, nickel, zinc, aluminum, chromium (III), silicon, titanium (III), iron (III) and macroamounts of europium (III) and americium were stated. An extraction-chromatographic method of americium macroamounts separation for subsequent spectrographic determination of impurities in 241AmO2 was developed and tested on the real samples. The results showed the applicability of the method to impurities separation for their spectrographic determination in 241AmO2.