The d e t e r m i n a t i o n of t h e i s o t o p i c c o n t e n t o f Cmethyl groups i n s e l e c t e d t r i t i u m and d e u t e r i u m l a b e l e d compounds by m o d i f i c a t i o n o f t h e Kuhn-Roth method i s p r e s e n t e d . O x i d a t i o n of t h e d e u t e r a t e d or t r i t i a t e d compound u s i n g a s o l u t i o n of sodium dichromate and s u l f u r i c a c i d a t 50-85'C a l l o w s i s o t o p i c a s s a y of t h e C-methyl group a s a c e t i c a c i d . Key Words: C-Methyl Group, T r i t i u m , Deuterium, Oxidation t i o n s w i t h o t h e r c l a s s e s o f compounds c o n t a i n i n g i s o t o p i c hydrogen C-methyl groups. A s o l u t i o n of sodium dichromate and s u l f u r i c a c i d i s employed t o c o n v e r t t r i t i a t e d o r d e u t e r a t e d compounds t o a c e t i c a c i d . The a c i d produced i s i s o l a t e d by steam d i s t i l l a t i o n and h i g h vacuum t e c h n i q u e s . F i n a l l y , t h e p u r i f i e d a c e t i c a c i d i s assayed f o r i s o t o p i c hydrogen. O x i d a t i o n of t r i t i a t e d o r d e u t e r a t e d compounds w i t h sodium