Neodymium-di-(2-ethylhexyl) phosphoric acid (DEHPA) species forming in the organic phase during solvent extraction of neodymium with solutions of DEHPA have been studied. Two samples were prepared: one with a low molar ratio of neodymium to DEHPA, which is liquid and clear, and the other with a high molar ratio of neodymium to DEHPA (complete loading), which has the consistency of a gel. Electrospray ionization (ESI) and matrix-assisted laser desorption ionization (MALDI) mass spectrometric investigations show numerous compounds, in addition to the generally assumed species dimeric DEHPA and Nd(DEHPиDEHPA) 3 , in the liquid sample. The nuclear magnetic resonance (NMR) spectroscopic investigation of pure DEHPA and of a completely loaded sample confirm the formula of pure DEHPA and of the organic part of Nd(DEHP) 3 . Furthermore, chemical analysis of a dried, completely loaded sample also proves the existence of the species Nd(DEHP) 3 . Results of X-ray powder diffraction measurements of this sample agree well with literature data.