Abstract: Radionuclides, ⁷Be and ²¹⁰Pb, are used to calibrate efficiency of HPGe γ spectro-meter system. It has been reported that ⁷Be and ²¹⁰Pb in aerosol samples could be extracted and transferred into a solution for preparation of efficiency calibration source through a series of chemical processes. In the present study we investigated the chemical procedures for extraction of ⁷Be and ²¹⁰Pb from aerosol filter samples. A muffle was used to burning aerosol filter samples to ashes, and concentrated HF, HNO₃, and HClO₄ were used to digest ashing sample. Then, ⁷Be and ²¹⁰Pb in ashing sample can be extracted into the solution. The time is set to 5h for burning aerosol samples to ashes, and the temperature is 500℃. The extraction technique is shown that ⁷Be and ²¹⁰Pb in 0.42 g ashing samples can be extracted into the solution completely by digesting more than 5 times.