Ion chromatographic techniques were investigated for the separation and the quantitative determination of some rare earth elements (REEs) in monazite and xenotime minerals. The influences of selected eluents containing complexing acids including oxalic and alpha-hydroxy isobutyric acid (alpha-HIBA) on the retention and hence the separation efficiency of REEs was studied. Different variables affecting the separation of different REEs such as pH, type, and concentration of the mobile phase were investigated. Gradient elution, using an advanced gradient pump, was controlled automatically by the Dionex AI-450 computer software. Separation of REEs was carried out using an Ion Pac CS5A column followed by a post column derivatization reaction with 4-(2-pyridylazo)resorcinol (PAR) and UV-VIS spectrophotometric detection. Mineral dissolution was carried out using sulfuric acid. A comparative evaluation of REE distribution in monazite and xenotime minerals using both ion chromatography (IC) and inductively coupled plasma atomic emission spectrometric (ICP-AES) techniques was carried out.