In this thesis, an electrocatalysis method has been used to measure hydroxylamine and hydrazine as environmental pollutants. Oxidation of these compounds on the surface of carbon paste electrode (CPE) at high potentials and high over-voltage occurs. Using combination of promazine-multiwall carbon nanotubes as electrocatalyst, oxidation of this compound in lower over-voltage occurs. Cyclic voltammetry, linear sweep voltammetry, chronoamperometry and electrochemical impedance spectroscopy were used for electrochemical studies. According to the cyclic voltammetry studies, the anodic peak potential for hydrazine oxidation at CPE in the presence and absence of promazine as mediator are 700 and 800 mV, respectively. Furthermore, the oxidation peak current of promazine was increases linearly proportionate hydrazine concentration. It was also found that the hydroxylamine on the surface of CPE in the range 0.0-1.0 V potential vs. reference electrode Ag/AgCl have any oxidative peak. While in the presence of promazine, mediator anodic peak current increases linearly relative to the hydroxylamine concentration. The effects of instrumental and concentration parameters have been optimized: pH=7.0, 0.2 mM of promazine and scan rate 80 mVs -1 . Under optimized conditions, the calibration curve was linear in two concentration ranges of 5.0 – 640.0 mM and 0.64 – 3.00 mM with a detection limit of 3.5 µM. For the determination of hydroxylamine optimum conditions are: pH=9.0, 0.5 mM promazine and scan rate 20 mVs -1 . Under the optimized conditions and by linear sweep voltammetry two linear segments were obtained: first segment from 0.17 to 1.03 and second from 1.03 to 10.00 mM. Detection limit of 4.2 mM was achieved. The relative standard deviation for 7 repeated measurements for 50.0 mM hydrazine and 0.7 mM hydroxylamine was obtained 2.1% and 1.5% respectively. Some of kinetic parameter such as diffusion coefficient (D), electron transfer coefficient (a) and charge transfer rate constant (k) were determined utilizing chronoamperometry methode. The proposed methode was also successfully used to hydrazine and hydroxylamine determination in the real sample analysis.