Abstract: 5.0 g of the sample dried at 105℃ was treated by powder tablet machine, and 11 elements, including Pb, As, Cu, Zn, Cr, Ni, Co, V, Mn, Sn and Mo, were determined by X-ray fluorescence spectrometry (XRF). The matrix effect and spectral overlapping interference were corrected by empirical coefficient method and Compton scattered internal standard method. The 65 national reference materials of soil, sediment and rock were selected to fit the calibration curves. It was shown that linear relationships between values of mass fraction of 11 elements and their fluorescence intensities were kept in the definite ranges, with detection limits (3s) in the range of 1.0-3.9 μg·g^-1, and RSDs (n=10) of the determined values were in the range of 0.64%-9.2%. The 30 newly developed reference materials for soil composition of agricultural land were determined, and accuracy of each element was evaluated according to the quality control standard of HJ 780-2015. It was shown that the determined pass rates of Pb, Cu, Zn, Cr, Ni, V and Mn were 100%, indicating that XRF could be used for the determination of those 7 elements in soil. The determined pass rate of Co was 93.3%, which was due to the influence of high content of Fe in the sample. The determined pass rate of As was 80.0%, and accuracy was poor when the mass fraction of As was below 13 μg·g^-1. The determined pass rates of Sn and Mo were less than 50.0%, so XRF was not recommended for the determination of Sn and Mo in soil.