An automated colorimetric procedure is described for the determination of ethinyl estradiol and ethinyl estradiol‐3‐methyl ether in pharmaceutical tablets. Chloroform solutions of the estrogen are automatically extracted with alcohol–sulfuric acid and analyzed at a rate of 20 samples/hr. The relative standard deviation of repetitive sampling of tablet extracts was less than 1 percent, and Beer's law was obeyed over the range of 0.40–8.00 mcg./ml. of sample solution. The procedure is applicable to unit dosage assays and to assays requiring composite samples of pulverized tablets or numerous whole tablets. Copyright © 1968 Wiley‐Liss, Inc., A Wiley Company