A method for determination of Nb, Ta,fe and Mn in niobite-tantalite by Laser micro spectrochemical analysis has been recommended. It was based on applying variable internal standard method, and using powder mineral of known composition as reference standard. The suitable operating conditions has been selected. The determination range for Nb205 and Ta205 were 20-60%，for Fe0 and Mn0 were 9-16%.The relative standard deviation were not more than 土20%.