A procedure for the sequential radiochemical determination of plutonium, strontium, uranium and iron nuclides is described. The separation is carried out on a single anion exchange column. Pu(IV), U(VI) and Fe(III) are fixed on Bio Rad AG 1-X4 from 9 mol/l HCl, while the sample effluent is used for the determination of radio-strontium. Fe and U are eluted separately with 7 mol/l HNO3, and Pu(III) is eluted with 1.2 mol/l HCl containing hydrogen peroxide. Subsequently, Pu and U are electrolysed and counted by alpha spectrometry. Radiostrontium is purified by the nitrate method and counted in a low level beta proportional counter. Fe is purified by extraction and cation exchange and 55Fe is counted by X-ray spectrometry with a Si(Li) detector. The sample preparation and the application of the procedure to large samples, namely aerosols from 105 m3 of air, and monthly deposition samples from 0.6 m2 sampling area (10–100 l) are described. Chemical yields are for Pu 70±20, for Sr 80±15, for U 80–90, and for Fe 75±10%. As an example, the maximum airborne radionuclide concentrations determined with that procedure in fortnightly collected samples at Neuherberg after the Chernobyl accident were: 239+240Pu, 2.58; 238Pu, 1.40; 238U, 0.65; 234U, 0.67; 90Sr, 7600; and 55Fe, 990 μBqm−3. With appropriate changes in sample preparation, the procedure is applicable to other kinds of samples.