Spectrochemical procedures have been developed to determine impurities in americium and curium samples. The simultaneous separation of many impurity elements from the base material (americium and curium) is carried out with extraction and extraction-chromatographic methods using di(2-ethyl hexyl phosphoric acid (D2EHPA). It is shown that part of the elements (alkalis, alkaline earths, silicon, tungsten, tantalum and other elements) are separated with extraction or sorption of americium and curium; the other part (rare earths, titanium, zirconium, niobium, molybdenum) with the Talspeak process. Two fractions in the extraction chromatography and three fractions in the extraction separation of americium and curium, containing impurities, are analyzed separately by a.c. or d.c. arc spectrography. To increase the sensitivity of the spectrographic analysis and accelerate the burn-up of impurities from the crater of the carbon electrode bismuth fluoride and sodium chloride were used as chemically active substances. The extraction of impurities from weighed quantities of americium and curium samples of 5-10 mg permits the lower limit of determined impurity concentrations to be extended to 1 × 10 -4-5 × 10 -3% m/m.