A quick, convenient and simple titrimetric method for determination of diuretic drugs e. g., acetazolamide, furosemide, hydrochlorothiazide, mannitol and spironolactone in pure form and in their pharmaceutical formulations viz., diamox (tab), synomax (tab), tebemid (tab), frusemene (tab), aquazide (tab), xenia (tab), kratol (inj), mannigyl (inj), aldactide (tab) and spilactone (tab) with ammonium hexanitratocerate (IV) reagent have been reported. It is a versatile oxidizing agent of cerium (IV) and is being widely used as an oxidant for several classes of organic compounds. The values of percentage error, coefficient of variation (CV) and standard deviation (SD) prove the method is precise and reproducible. To establish authenticity of the method, percentage recovery experiments were also carried out by standard drug addition method indicating non interference of excipients in the method results.