Abstract: The tantalum furnace ash was dissolved by microwave digestion with hydrofluoric acid and nitric acid medium, and the samples were prepared after separation and dilution. A semi quantitative analysis was used to analyze the sample solutions, ensuring the preparation of calibration solutions to be suit for the amount of tantalum, and a series of calibration solutions were also prepared. Ta 240.063 nm was the selected as the analytical spectral line, and the standard addition method was used to remove the matrix effect, and then the contents of tantalum in tantalum ashes were determined by inductively coupled plasma emission spectrometry (ICP-OES). The results showed that the linear correlation coefficients of the standard curves were over 0.999, and the relative standard deviations (RSDs, n=7) were less than 0.50% with a recovery of 94.6%~107.9%.