D i f f e r e n t i a l p u l s e polarography was used f o r t h e q u a n t i t a t i v e d e t e r m i n a t i o n of y t t e rbium(II1) i n minerals and oxides of o t h e r l a n t h a n i d e s . As the r e d u c t i o n occurs a t f a i r l y neg a t i v e p o t e n t i a l s and t h e reduction of hydrogen i o n s i n t e r f e r e s a t low pH t h e number of s u it a b l e supporting e l e c t r o l y t e s i s l i m i t e d . A t pH > 6 h y d r o l y s i s e f f e c t s cause t h e r e d u c t i o n peak c u r r e n t t o decrease a s a f u n c t i o n of time. D o n t o 5.10-8 M y t t e r b i u m ( I I 1 ) can be d e t e rmined i n the supporting e l e c t r o l y t e L i C l (0.1 -1 M) a t pH 5. The a n a l y s i s of y t t e r b i u m ( I I 1 ) i n commercial samples showed average r e l a t i v e standard d e v i a t i o n s which do n o t exceed 7 %.