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A new oscillopolarographic method for the determination of Si (Ⅳ) is described in this paper. In the system HC1- Sb(Ⅲ) -Mo(Ⅵ) -NaCl-ethyl alcohol, Si (Ⅳ) with Sb (Ⅲ) and Mo (Ⅵ) form ternary heteropoly acid. The anion of ternary heteropoly is adsorbed on t