Nickel is a constituent of wide range of construction materials in nuclear industry and their corresponding activation products are often encountered in low level solid radioactive waste and effluents. The article presents the radiochemical analytical method for determination of 63Ni in the concrete samples originated from Nuclear Power Plant Mochovce, Slovakia. The sample of concrete was ashed and leached with aqua regia thereafter hydroxides were precipitated with ammonia solution, leaving Ni in aqueous phase. The next purification steps included a precipitation as Ni–dimethylglyoxime (DMG) complex, an anionic exchange column and an extraction chromatography on Nickel resin. The purified 63Ni fraction was mixed with the scintillation cocktail and the mixture was measured by liquid scintillation counting (LSC). The radiochemical yield of the separation procedure was determined by atomic absorption measurement of stable Ni in the range of 49–71%. Up to the sample amount of 50 g the detection limit was 0.002 Bq g−1 at counting time 180 min and 95% confidence level.