The impact of micro- and mesoporosity of the carbon substrate on nitrogen content and activity of metal-nitrogen-carbon (MNC) catalysts is addressed via electrochemical, structural, and compositional techniques. A closed vessel containing the metal, nitrogen, and carbon precursors controls mass losses due to convection of high temperature byproducts. The resulting catalysts were characterized morphologically using nitrogen physisorption, coupled with DFT analysis to calculate pore size distributions. Bulk nitrogen content was observed using CHN combustion analysis, and the catalysts were characterized electrochemically by rotating ring-disk measurements. The influence of mesoporosity on nitrogen adsorption indicates the importance of precursor transport to potential active sites during pyrolysis.