The present invention relates to a sequential separation method for the quantification of ^99Tc (technetium), ^90Sr (strontium), ^55Fe (niobium), and/or ^59(63) Ni (nickel) which is a regulation nuclide contained in a radioactive waste and, more specifically, to a new method which rapidly simply separates the nuclides by simply controlling pH of a solution based on ion exchange resin method. The separation method of the present invention separates a nuclide of next step with a simple a chemical treatment such as a pH control in every separation process when the regulation nuclides such as ^99Tc, ^90Sr, ^55Fe, ^94Nb, and/or ^59(63)Ni is separated from the radioactive waste for the quantification. The separation method reduces use amounts of a strong acid and separates nuclides with a noticeably reduced time in comparison with traditional technology. Therefore, a separation procedure is simplified and a time which is required for separation is remarkably reduced. An analyzer is not exposed to radiation for a long time. [Reference numerals] (AA) Input; (BB) Output; (CC,FF) Preprocessing : 3days; (DD) Extracting; (EE) Dipping; (GG) Drying step; (HH,JJ) Preprocessing : 1day; (II) Cutting step; (KK) 59(63)Ni separation(1day); (LL) Traditional technology : total14days(15 samples) consumption; (MM) 99Tc separation(1day); (NN,QQ,TT) Preprocessing : 0.5day; (OO) 90Sr separation(0.5day); (PP) 90Sr refinement(0.5day); (RR) 55Fe separation(0.5day); (SS) 94Nb separation(0.5day); (UU) 59(63)Ni separation(1day); (VV) Technology of the present invention : total 6 days (15 samples) consumption
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