H-point standard addition method—First derivative spectrophotometry for simultaneous determination of palladium and cobalt

H-point standard addition method (HPSAM) has been applied for simultaneous determination of palladium and cobalt in trace levels, using disodium 1-nitroso-2-naphthol-3, 6-disulphonate (nitroso-R salt) as a selective chromogenic reagent. Palladium and cobalt in the neutral pHs form red color complexes with nitroso-R in aqueous solutions and making spectrophotometric monitoring possible. Simultaneous determination of palladium and cobalt were performed by HPSAM—first derivative spectrophotometry. First derivative signals at the two pairs of wavelengths, 523 and 589 nm or 513 and 554 nm were monitored with the addition of standard solutions of palladium or cobalt, respectively. The method is able to accurately determine palladium/cobalt ratio 1:10 to 15:1 (wt/wt). Accuracy and reproducibility of the determination method on the various amounts of palladium and cobalt known were evaluated in their binary mixtures. To investigate selectivity of the method and to ensure that no serious interferences were observed the effects of diverse ions on the determination of palladium and cobalt were also studied. The recommended procedure was successfully applied to real and synthetic cobalt or palladium alloys, B-complex ampoules, a palladium-charcoal mixture and real water matrices.