Sample solution contained 5 mg of niobotantalate mineral can be sepa- sated in the medium of 6 N-HCl-2% H2C204 solution on the account of the two reagents of BPHA and PMBP separately added to the system of extra- ction. The procedue can be used to determine 14 elements such as Nb, Ta, Zr, Ti, Fe, W, Ta, U, RE, Pb, Al, Ca, Mg and Mn. T>}e sample taken only 20- 30 mg for complete annlvsis.