A method of radioactivation analysis has been developed for the substoichiometric determination of cobalt, copper and manganese in glass and glass-making materials. The substoichiometric extraction of cobalt with α-nitroso-β-naphthol was studied and simple procedures are suggested for the determination of the three elements. Cobalt is extracted substoichiometrically as α-nitroso-β-naphtholate into chloroform from solution of pH 6.2, copper as dithizonate in carbon tetrachloride from weak acidic solution, and manganese as tetraphenylarsonium permanganate into chloroform after oxidation to permanganate. Contents from 2 ppm to 3 ppb of cobalt, copper and managanese were analysed in glass-making materials, and it is shown that the method for their determination is reliable and superior in accuracy and reproducibility.