Abstract: This is an article in the field of mineral analysis and testing. A rapid method for the simultaneous determination of Nb, Ta, Li and Be in Nb Ta ore by alkali fusion inductively coupled plasma mass spectrometry was established. The mixed alkali of sodium peroxide and sodium hydroxide=1:1 is used to decompose the sample. During extraction, niobium, tantalum and other elements are completely precipitated and separated from the liquid. The content of niobium, tantalum, lithium and beryllium in the sample is determined by inductively coupled plasma mass spectrometer after conversion and precipitation with 25 mL of 10% sulfuric acid+10% hydrogen peroxide solution. This method is used to determine the national first-class reference materials GBW 07153, GBW 07155 and GBW 07185. The measured values of each element are basically consistent with the certified values, with a relative error of 0.50%～4.77% and a relative standard deviation (n=6) of -0.009%～0.008%. It is applicable to the determination of niobium and tantalum in niobium tantalum concentrates, refractory or complex samples, and has been applied in production practice.