Peroxy compounds such as H2O2, peroxydisulfate (PDS), peroxymonosulfate (PMS), sodium perborate (SPB), and tert-butyl hydroperoxide (TBHP) have been used as efficient catalysts for nitration of aromatic and heteroaromatic compounds in presence of NaNO2/KHSO4 under mineral acid-free conditions. The reactions afforded very good yields of under different conditions. Depending on the nature of peroxide and substrate, reaction times recorded under conventional conditions reduced from (2 to 7hrs) hours to (25 to 60) minutes with grindstone technique, which in turn reduced to (25 to 120) seconds in microwave assisted reactions. Product yields are also increased from 6 to 10% under microwave irradiation as compared to conventional procedures. All synthesized compounds were characterized by 1 H NMR and mass spectral studies.