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In this paper are introduced basic magnetic resonance (MR) methods for measuring the properties of the conductive gel structure during polymerization, particularly relaxation times T1, T2. Gel electrolytes based on the NaClO4 inorganic salt was measured. The measurement deals with 23Na nuclei. In our case to measure relaxation time T2, the Hahn echo was used. To measure relaxation time T1, the IR techniques (Inversion Recovery) was used. The value of relaxation time T2 is obtained by approximation of spectral lines and the value of relaxation time T2 is obtained by approximation of spin echo decline signal with two exponentials using a genetic algorithm for both times. The change of relaxation times T2 and T1 of 23Na nuclei during polymerization process indicate a change in the internal structure and chemical composition of gel electrolytes based on NaClO4.