The substoichiometric separation of Yb(III) can be achieved by the extraction of a substoichiometric amount of thenoyltrifluoroacetone and an excess amount of phenanthroline in benzene. The appropriate pH range for the substoichiometric extraction is 6–8. The reproducibility of the substoichiometric extraction of Yb(III) is very good as RSD 1%. As an example, Yb in a manganese nodule is determined by the substoichiometry combined with the radioactivation analysis. The content of Yb is 17.63±0.23 g/g. The present procedure can be applied to the determination of other rare earth elements.