In the present study, calix [4]arene and its derivate 25,27-di(4-nitrobenzyl)-26,28-dihydroxycalix[4]arene were irradiated for 72 hours by 60 Co gamma rays at dose rate of 0.720 kGy/h. These irradiated samples were analyzed by EPR method and it was found that one type of radical was produced in calix[4]arene, and two type of radicals were produced in 25,27-di(4-nitrobenzyl)-26,28-dihydroxycalix[4]arene. The measurements were performed in the temperature range of 273-400 K using x-band EPR spectrometer. It was observed that the spectra, obtained from two samples, have very weak temperature dependence. Hyperfine and g parameters were calculated for two samples.