A micro amounts of (cefoperazone, ceftizdime, cefotaxime, cefotriaxone) were determined by two different technique. A) Potentiometrically Technique using a potassium bromate as an oxidant. The method based on oxidation of each drug to the corresponding nitro or carbonyl derivative with KBrO3 in acidic medium, the reaction are complete under acid medium of pH ranging from 2-3 the un reacted bromate are then reduced to bromide which in titrated potentiometrically with AgNO3 using silver electrode coupled with silver silver chloride electrode, the range of drugs concentrations determined were found to be 0.1 to 15 m mol liter of each drug respectively. B) HPLC Technique: The method involved a determination of binary mixture and reanalysis with analysis of ternary mixture using HPLC technique. The method finds a wide application for the drugs determination in both pure and pharmaceutical formulation samples with high accuracy and precise.