A second derivative spectrophotometric method has been developed for the determination of palladium and platinum in mixtures. The method is based on the formation of the platinum and palladium complexes with 3-(2-thiazolylazo)-2,6-diaminopyridine, (2,6-TADAP), in the presence of 1.7 M * To whom correspondence should be addressed. 93 Downloaded by [University of Connecticut] at 04:45 16 September 2013 94 TORAL ET AL.perchloric acid solution, upon heating at 90° C for 30 min and on the subsequent direct derivative spectrophotometric measurement. The zerocrossing approach and the graphic method were used for determination of platinum and palladium, respectively. Each analyte was determinated in the presence of one another in the ranges 8.9xlO" 7 -3.1x10" M for platinum and 4.6xlO" 7 -6.8xlO" 5 M, for palladium. The detection limits achieved (3a) were found to be 2.7xlO' 7 M of platinum and 1.4xlO' 7 M of palladium. The relative standard deviations were in all instances less than 1.0%. In this work is included a study of effect of interferents and the application of the proposed method in synthetic mixtures.