Abstract: Nikethamide is formally determined by the hydrolysis method, which is widely employed as official method in many countries. However,it is rather tedious and time-consuming and the results usually vary with experimental conditions. On the other hand,the precision and accuracy of the refractometric method is rather poor,in spite of its simplicity and rapidity. The nonaqueous titration in glacial acetic acid,using acetous perchloric acid as a titrant,has been developed to overcome the difficulties encountered in above mentioned methods. The method is proposed as follows: Accurately weigh a sample of 180—250 mg into a 120 ml conical flask,dissolve it in 5 ml glacial acetic acid(add two drops of crystal violet indicator and adjust to bluish green color with acetous HClO₄)and titrate with 0.1N acetons perchloric acid to bluish green color. One ml 0.1N HClO₄ is equivalent to 17.82 mg C₁₀H₁₄N₂O.