Electrochemical copolymerization of o-chlorophenol (oCP) with o-hydroxyphenol (oHP) was carried out in aqueous H2SO4 by using cyclic voltammetry (CV) technique. In addition, CV was used to evaluate the differences in electrochemical characteristics of the copolymer in comparison with the corresponding homopolymers, poly(o-chlorophenol) (PoCP) and poly(o-hydroxyphenol) (PoHP). The variation of peak currents with respect to sweep rates was compared between copolymer and homopolymers, PoCP and PoHP, films. Further support for copolymer characterization was obtained by recording UV-visible, IR spectra and elemental analysis. The mechanism of the electrochemical polymerization has been discussed. The monomer reactivity ratios (r1 and r2) were calculated using Fineman-Röss method and was found to be 0.4 and 1.3 repetitivelly and the copolymer structure is a block structure and more rich in oHP units.

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