Currently, non-volatile nuclides such as 94Nb, 99Tc, 90Sr, 55Fe, and 59/63Ni are used a sequential separation. In this study, we developed a separation for 99Tc and 90Sr by a carbonate precipitation. Sodium Carbonate (Na2CO3) was inserted in the aqueous sample from a Dry Active Waste (DAW) and a carbonate precipitation was produced. The precipitate is composed of di- or tri-valent element such as Co, Sr, Fe, Ni and the supernatant is composed of mono-valent element (Cs) and anion materials (ReO4 -, TcO4 -). In DAW, it was confirmed that the recovery of 90Sr (precipitate) and 99Tc (supernatant) were > 90%, respectively. The precipitate and supernatant separated by using a Sr-resin and an anion-exchange resin, respectively. The separated samples were measured by a Liquide Scintillation Counter (LSC, 90Sr) and Induced-Coupled Plasma-Mass Spectroscopy (ICPMS, 99Tc).