This study investigates the irreversible electrochemical oxidation of Amino Trimethylene Phosphonic Acid (ATMP) in ClO4−–electrolyte on original unmodified graphite electrodes (GRE) and glassy carbon electrodes (GCE) using cyclic voltammetry (CV) as the main analytical technique. The oxidation reaction starts at ≈ +0.7 V on GRE and ≈ +0.92 V on GCE vs. Ag/AgCl (3M KCl) respectively. Four distinct electrode/electrolyte systems were selected for a comprehensive analysis of charge transfer and mass transport processes at non-Faradaic and Faradaic current regions at various scan rates υ (SR). These systems comprised of GRE/ClO4−–electrolyte, GRE/ATMP–ClO4−–electrolyte, GCE/ClO4−–electrolyte, and GCE/ATMP–ClO4−–electrolyte. Charging currents in the so-called double-layer region of the CV are found to scale linearly with SR on GCE (Adsorption mechanism); instead, the charging currents obey a nearly square root law on GRE (Diffusion mechanism). The electrochemical oxidation kinetics of ATMP in ClO4−–electrolyte using GRE and GCE obey nearly the fourth root law of the maximum oxidation current density (at the upper reverse potential) vs. SR. Finally, we identified the major transformation products generated from the ATMP electrochemical oxidation: ortho-phosphate (o− PO4), iminodimethylphosphonic acid (IDMP), and aminomethylphosphonic acid (AMPA).