In this article, we set up a methodology to investigate the relationship between the catalytic activity and the agglomeration state of platinum group metal-free ORR catalysts. To this end, we have developed a statistical approach based on scanning electrochemical microscopy (SECM) and atomic force microscopy (AFM). Two catalysts are investigated at very low loadings in order to access their intrinsic activity. Differences in terms of dispersion, stability of the inks, and adherence on the substrate are observed, highlighting the importance of measuring the exact amount and agglomeration state of the materials under study. The agglomeration state of the deposits measured by AFM explains the differences in activity measured by SECM. The performances of the catalysts are compared, and the contributions of the intrinsic activity and the agglomeration state are identified. This work paves the way toward various applications ranging from the benchmarking of new catalysts to the optimization of an ink formulation, for ORR and beyond.