Two-stage columbite solid state reaction route has been used for the preparation of 3 2/3 1/3 O Nb B Pb) (′ materials (B′ ′ = Mg, Ni and Cd). The columbite precursor phase was structurally characterized using diffraction data. MgNb 2 O 6 , NiNb 2 O 6 and CdNb 2 O 6 show orthorhombic structures i.e. pure columbite phase. Final phase materials get stabilized in mixed phase. The diffraction pattern shows that it is a mixture of cubic pyrochlore and perovskite phase. Percentage of perovskite phase was calculated using the band intensities of (110) perovskite and (222) pyrochlore peaks. The calculated percentages show the dominant perovskite phase. Possible reasons for mixed phase are discussed.