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The nanocrystalline samples of 10wt.%Scandia stabilized Zirconia (10ScSZ) and 1wt.%Ceria doped ScSZ (1Ce10ScSZ) prepared via co-precipitation route were characterized and compared to commercially available samples regarding their transport properties and electrical conductivity. The results of oxygen isotope experiments show that for Zirconia-based electrolytes, the rate of heteroexchange is lower than that for Samaria-doped Ceria. The results of Secondary Ions Mass Spectrometry (SIMS) indicate that all admixed components are present both in the surface layer and the bulk of the studied samples with pronounced segregation on the grain boundary. The highest total conductivity is observed for DKKK sample. In the range of 600-400°C the highest conductivity observed for synthesized nanocrystalline 1Ce10ScSZ sample is explained by the effect of segregated Scandia doped Ceria surface layers.