Abstract: Magnetically assisted sample preparation(MASP) can effectively reduce the detection limit of the XRF. The core of MASP is magnetic carrier. In this work, the co-precipitation magnetization method had been used to prepare magnetic TEVA resin, which was used as the magnetic carrier for MASP/XRF analysis trace Tc in samples from reprocessing process. It was characterized by SEM, FTIR, XRD and other analytical methods. The results show that the iron oxide, which mainly composes of Fe₃O₄, is physically embedded with resin. The prepared magnetic TEVA resin retains the selective adsorption of TEVA resin to perrhenate under low acid and has paramagnetic properties, which can be used for MASP/XRF analysis. The preparation method has good repeatability. The obtained magnetic resin has stable and good performance. The sample recovery rate for MASP is more than 99%, which can effectively reduce the detection limit of the method.