A nanocomposite film of NiHCF electrodeposited onto AFCNT was modified on GCE by the electrostatic interaction of multiple scan cyclic voltammetry. Amino groups have been introduced with a positive charge onto the surface of MWCNTs. The presence of NiHCF-AFCNT/GCE was characterized by using FE-SEM, EDS, EIS, and XRD studies. The nanocomposite film of NiHCF-AFCNT was further utilized to determine persulfate and tannic acid, respectively. The nanocompo-site film modified electrode displays linear response from 0.1 to 19 mM and 10 to 170 mM for persulfate and tannic acid with a correlation coefficient of 0.9921 and 0.9869. The detection limits were found to be 0.1 mM and 1 mM, respectively. As results, the electrostatic interaction between positively charged metal ions, amino functionalized CNT and negatively charged hexacyanoferrate can be a new subject for many interesting applications.