Abstract: 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.