In this paper, a novel method was developed for the preconcentration, separation, and determination of light (Ce), medium (Eu and Gd), and heavy (Yb) rare earth elements (REEs) by inductively coupled plasma mass spectrometry (ICP-MS), based on the adsorption of Ce3+, Eu3+, Gd3+, and Yb3+ on carbon nanofibers (CNFs) loaded with 1-phenyl-3methyl-4-benzoyl-5-pyrazone (PMBP). The REEs can be adsorbed quantitatively on CNFs-PMBP in the pH range of 5.0 to 8.0 and then eluted completely with 1.0 mol L-1 HNO3. The experimental parameters for the preconcentration and separation of REEs, such as pH, sam...