Abstract: A extraction-spectrophotometric method for the determination of iron in the HLLW is developed. In the medium of hydrochloric acid, the iron is separated from impurities with isopentanyl acetate. and then iron is back-extracted with water. Sulfosalicylic acid is addcd to colour iron. Then the coloared complex becomes to a new complex with higher degree of complexation by addition of ammonia. whieh is stable and has higher absorption coefficient. The absorptivity is determined. The preetition of this method is better than 2%, when the amount of iron to be determinted is in range of 0 20 μg.