The research Includes simple, sensitive and rapid spectrophotometric method for determination of atenolol in aqueous solution. The method is based on the Schiff's base formation which is achieved by coupling of atenolol with salicyldehyde to yield a yellow colour product exhibiting maximum absorbance at 378 nm. Beer's law is obeyed in the concentration range 12 - 84 μg/ml of atenolol, with a molar absorptivity 3728.2 L.mol-1.cm-1 and sandell index of 0.0714 μg.cm-2. The average recovery is 100.016%, relative standard deviation 0.181-1.907% and D.L of 0.4340 μg/ml. This method has been applied successfully to determination of isoniazid in pharmaceutical preparations.