Abstract: ²³²U concentration is stringently controlled in nuclear fuel fabrication, an accurate determination method for determining ²³²U concentration is needed. An analytical method was developed for the measurement of ²³²U by combining of α spectrometry and mass spectrometry. The isotopic abundances ratio of ²³⁴U, ²³⁵U and ²³⁶U to ²³⁸U in samples were obtained with mass spectrometry, and the total activities of ²³⁴U, ²³⁵U, ²³⁶U and ²³⁸U, and the activity of ²³²U were measured with α spectrometry. The concentration of ²³²U can be calculated. The uncertainty of the results was evaluated. The relative standard deviation of 16 analysis using this method is 3.43% for the samples with 1.118 ng/g ²³²U. The results show that this method can be used for routine analysis in nuclear fuel fabrication plant.