This study presents a rapid and quantitative radiochemical separation method for Nb isotopes in radioactive waste samples from the nuclear power plant with anion exchange resin after Fe coprecipitation. After radionuclides were leached from the radioactive waste samples with concentrated HCl and HNO3, the Nb isotopes were coprecipitated with Fe after filtering the leaching solution with 0.45 micron HA filter, while the Sr, Tc and Ni isotopes were in the solution. The Nb isotopes were separated in HCl medium with anion exchange resin. The purified Nb isotopes were measured using a low level liquid scintillation counter after installing quenching curve with standard Nb-94 isotopes. The separation method for Nb isotopes investigated in this study was applied to neutron dosimeter samples from the nuclear power plant after validating the Nb activity concentration with gamma spectrometry system.