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59Co-Internal Field Nuclear Magnetic Resonance (IFNMR), 57Fe-IFNMR measurements are carried for the different materials like bulk cobalt, carbon coated cobalt (Co@C), bulk iron, carbon coated iron nanoparticles (Fe@C). The comparison of obtained results for bulk cobalt and Co@C shows that the bulk cobalt exists in the both the phases i.e., fcc and hcp phases, while the other exist only in the fcc phase. Further, the comparison of the NMR results of bulk iron and Fe@C confirms the presence of the single domain particles in the Fe@C samples. Thus, we propose IFNMR as a powerful tool to identify the structural and magnetic properties of ferro/ferrimagnetic materials. [ABSTRACT FROM AUTHOR]