The magnetic properties of the metal nanoparticles (NPs) can play remarkable role in electromagnetic interference shielding (EMI Shielding) of many defence and commercial electronic devices. In the present work, coconut oil and PVA capped magnetic cobalt/cobalt oxide nanoparticles (Co/Co₃O₄ NPs) were synthesized by chemical reduction method and impregnated in polymer matrix to verify their EMI shielding behaviour. The coconut oil capped Co/Co₃O₄ NPs with presence of hcp and fcc phases were prepared in the size domain of 7-10 nm and the effect of surfactant (the oil) on size and oxidation state was studied by varying the ratios. The shielding efficiencies of Co/Co₃O₄ NPs PVA nanocomposites were analysed by using vector network analyser (VNA) in X- and Ku-band ranging from 8 GHz-18 GHz. The VNA results showed increased shielding efficiency with increasing concentration of NPs.