In view of the characteristics of complicated types, high salt content and strong matrix effect of associated radioactive solid wastes, and there is no relevant standard method for analyzing radionuclides in associated radioactive solid wastes. Taking molybdenum ore slag, zirconium ore slag and rare earth slag as the measurement objects, the chemical components in the samples were measured by X-ray fluorescence spectrometer, and the simulated efficiency calibration was carried out by combining with the passive efficiency calibration software. The spectrum was measured by gamma spectrometer, and the gamma spectrometry method for the analysis of radioactive nuclides in associated radioactive solid waste was established. The experimental results show that the rare earth waste residue, zirconium waste residue and background matrix samples are uniformly mixed at the ratio of 3∶7 (30 g∶70 g) and 1∶4 (20 g∶80 g), and then put into the ϕ 75 mm× 20 mm sample box for gamma spectrometry measurement. The measurement dead time accounts for 9% and the correction error of self absorption factor is less than 5%; The absolute value of the relative error is less than 5%; The maximum deviation between the passive efficiency scale and the active efficiency scale is 4.74%; When ²³⁸U is measured with 92.6 keV full energy peak, the deviation of the measured results after the interference peak correction meets the requirement of less than 30%. Compared with other methods, the relative deviations of ²³⁸U, ²³²Th and ²²⁶Ra are 1.40%-5.03%, 0.59%-6.13% and 2.30%-3.85%, respectively. When the gamma spectrometer is used to measure the associated radioactive solid wastes, this method optimizes the sample loading quality, reduces the influence of sample self absorption, and does not need to match the solid waste standard sample with the same matrix, and the measurement result is reliable. The results provide a feasible analytical scheme for peer laboratories and technical support for the formulation of relevant industry standards.