Abstract: 〖JP2〗An acid-soluble digestion method of polysilicon sample was explored. The acid-soluble systems of hydrofluoric acid and nitric acid were confirmed. The optimized acid digestion ratio of V(H2O)〖KG-1.8mm〗∶〖KG-1mm〗V(HF)〖KG-1.8mm〗∶〖KG-1mm〗V(HNO3) was 20〖KG-1mm〗∶〖KG-1mm〗28〖KG-1mm〗∶〖KG-1mm〗10 for polysilicon powder samples. Comparing the digestion effect of closed digestion at room temperature, ultrasound-assisted digestion, water bath heating-assisted digestion and microwave digestion, it was found that the closed 〖JP3〗digestion at room temperature for one hour is the most convenient and effective way to digest polysilicon powder sample. 〖JP〗