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An undergraduate quantitative analysis experimentThe facile ion-exchange chromatographic separation of numerous first-row transition metal ions based on differential stability of their chloro complexes has been demonstrated by Kraus and Moore (I). A number of undergraduate laboratory experiments have been developed, based on their procedure. These experiments have been commonly restricted to the separation of pairs of metal ions {2-4) such as Ni(II) and Co(II) {3, 4), but occasionally they are extended to the separation of Ni(II), Co(Il), and Fe(III) (5), or more {1) metal ions. The sources cited adequately cover the theoretical basis of the separation. The most common quantitation schemes utilize EDTA titrations (2, 4, 5). Spectrophotometric (1, 3) and radiotracer {1) methods have also been applied. In separations involving Fe(III), Fe(III) quantitation is typically omitted (5) or performed via radiotracer methods (I), since extensive Fe(III) precipitation interferes with analysis under pH conditions favorable for EDTA titrations. We have developed a simple atomic-absorption analysis scheme which circumvents the Fe(III) precipitation problem and enables convenient separation and quantitation of a mixture containing Ni(II),