Аннотация:Increasing interest in sodium-ion batteries (SIBs) implementation leads to investigation and optimization of differentsodium-based cathode materials. Sodium-iron phosphate-pyrophosphate Na4Fe3(PO4)2(P2O7) (NFPP) is a promisingcathode material due to its low cost, safety, stability, non-toxicity and relatively high Fe3+/Fe2+ redox potential value.One of the significant problems related to synthesis of NFPP is formation of impurity phases – NaFePO4 and Na2FeP2O7,which leads to degradation of materials electrochemical performance. The correct identification and estimation ofelectrochemical activity of impurity phases is a crucial task for further development of synthetic routes for NFPP-basedcathode materials. Herein we suggest a novel approach to identification and quantitative estimation of peculiar phaseactivity in multiphase NFPP-based cathode materials using electrochemical data. The approach is based on comparingexperimentally obtained galvanostatic curves with model galvanostatic curves derived from quantitative phaseanalysis based on Rietveld refinement of the powder X-ray diffraction data. Implementation of such approach allowedus to distinguish the contribution of NFPP, NaFePO4 and Na2FeP2O7 phases into galvanostatic discharge curves profile.Furthermore, the conditions for synthesizing NFPP with optimal electrochemical properties were established,providing a pathway for the development of high-performance NFPP cathodes.