A good number of reviews have been made on the use of large number of chromogenic reagents for the spectrophotometric determination of iron and cobalt. Some of the recently proposed spectrophotometric methods for the determination of iron [8–15] and cobalt [16–22] are less sensitive and less selective. We are now proposing simple, sensitive and selective direct and derivative spectrophotometric methods for the determination of iron(II) and cobalt(II) in various complex materials using 2-hydroxy-1-naphthaldehyde-p-hydroxybenzoichydrazone as chromogenic agent. We are also reporting a highly selective second-order derivative method for the simultaneous determination of iron and cobalt in different samples.