A procedure is described for quantitative determination of trace quantities of dodecylammonium acetate (DAA) which are proportionally extracted into chloroform layer with orange II from aqueous solutions containing up to 2.5×10^<-7> mole and down to 1×10^<-8> mole of DAA. It is observed that the stable color developed by DAA and orange II shows the maximum absorption at 485mμ, of which intensity does not change providing the pH of the aqueous solution is 3.5-5.0. The composition of the complex extracted with chloroform is confirmed to be 1 : 1 molar ratio of DAA to orange II by the continuous variation method. This procedure is also suitable for estimating the amount of DAA adsorption on silicate minerals in the flotation pulp.