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The measurement of 55Fe and 63Ni is of great significance for the monitoring of liquid effluents from nuclear power plant. In this paper, a combined analysis method of 55Fe and 63Ni in liquid effluent sample is established. 55Fe and 63Ni are enriched by precipitation of iron hydroxide and nickel hydroxide and separated by TRU resin and nickel resin, then measured by low-level liquid scintillation spectrometer. Also the relevant measurement conditions are analyzed and studied. When the amount of sample is 1.0 L and the measurement time is 60 min, the detection lower limit of this method is 0.06 Bq/L for 55Fe and 0.02 Bq/L for 63Ni, which meets the analysis requirements of 55Fe and 63Ni in liquid effluents of nuclear power plant.