A first order derivative spectrophotometric method has been developed for the simultaneous determination of bismuth and zinc by dithizone without time-consuming extraction step. The reactions of bismuth and zinc with dithizone in a three component solution prepared in water, acetone and n-propanol mixture have been investigated. These cations react with dithizone in this mixture at pH 5.0, forming coloured complex that is stable for at least 2 h. The linear range in D evaluation was between 3.0 x 10(-6) and 1.8 x 10(-5) mol 1(-1) for Zn and 2.4 x 10(-6) and 1.2 x 10(-5) Mol 1(-1) for Bi. The limits of detection for the analytical procedure were found 0.05 mg 1(-1) for both cations. The relative standard deviations for the determination of 0.5 mg 1(-1) bismuth and 0.5 mg 1(-1) zinc were 1.2 and 1.1%, respectively, for five determinations. The procedure is simple, rapid and reliable. This method was applied to the determination of bismuth and zinc in the pharmaceutical materials successfully. Good agreement was achieved between the results obtained by the proposed and comparative methods. (c) 2005 Elsevier B.V. All rights reserved.