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Sodium and potassium can be separated from the other constituents of silicate rocks by cation exchange resin (Amberlite IR-120). The sample is decomposed with hydrofluoric and sulfuric acids and passed through the resin bed after expulsion of the fluorine. The column is eluted with 0.12N hydrochloric acid at a fast flow rate of 4 ml. per sq. cm. per minute and the sodium and potassium are recovered together within a reasonable time. 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