Abstract: Powder tablet is a kind of green and pollution-free sample preparation technology, but the conventional powder sample preparation (400kN) has large particle size effect and mineral effect, which often results in large error, and some samples are difficult to press into shape, but increase the pressure of sample preparation can reduce the voids between powder particles, thereby reducing the mineral effect. In this paper, high pressure sample preparation (800kN) technology can be used to press various types of silicate samples into shape, the surface of the sample is smooth and compact. The experiment used national first-class standard materials of silicate rocks, sediments, and soils to establish calibration curves. It corrected the matrix and the overlap of element spectral lines using empirical methods and internal standard methods. By comparing the surface morphology of the samples, the slope of the calibration curve and reproducibility, the study found that the calibration curve established using high-pressure sample preparation was better than that using conventional pressure sample preparation. The detection limits were reduced, and the precision of most components was below 1.0%. The relative standard deviation (RSD) of GBW07453 (RSD, n=4) for niobium and zirconium were 1.66% and 0.77%, respectively, which were greatly improved compared to conventional pressure sample preparation (RSD of niobium and zirconium were 3.80% and 1.55%, respectively). The analysis of actual showed that the measured values of niobium and zirconium were consistent with the chemical values. This method used high-pressure sample preparation technology to achieve the determination of niobium, zirconium, and major elements in geological samples by X-ray fluorescence spectrometry, and the analysis results met the requirements of analysis.