Of several potential reagents for the indirect polarographic determination of beryllium, benzoylacetone was found to be the most attractive. A study of the relevant properties of this reagent and of the characteristics of its reaction with beryllium led to the development of a new method for the determination of beryllium with good precision at concentrations as low as 10 p.p.m. and with reasonable precision even at 2 p.p.m. Less than 0.5 mg. of beryllium is required. The method, when preceded by an appropriate mercury-cathode separation, is applicable to the determination of beryllium in copper-base alloys. The application of the method was extended to aluminium-base alloys by the development of an ion-exchange procedure for the separation, with at least 95% efficiency, of beryllium from relatively high concentrations of aluminium. A similar method is applicable to the determination of aluminium, in concentrations down to about 20 p.p.m. / Thesis / Master of Science (MS)