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A new analytical procedure for determination of lanthanides in environmental samples after chemical separation from major matrix elements on DOWEX 50W-X8 resin followed by preconcentration with chelating agent ammonium pyrrolidine dithiocarbamate (APDC) and analyses of thin targets by energy dispersive X-ray fluorescence (EDXRF) method using 109Cd as the source of excitation was presented. Characteristic Lalpha X-ray lines of the lanthanides were used for calculations of the net peak area and mass concentrations. The influence of pH value of the solution and addition of organic matter on the complexation was investigated. Percentage of recovery of each lanthanide after separation on DOWEX 50W-X8 resin was also determined. Accuracy of the method was tested on standard reference materials and real environmental samples (red mud material). For that purpose samples of standard reference materials and red mud were prepared as thick targets and directly analyzed (without the separation step) by EDXRF method using 241Am as the excitation source. In that case lanthanides concentrations were determined over their characteristic Kalpha X-ray lines and results were compared with those obtained after separation/preconcentration step described above. Results showed that selected lanthanides made stable complexes with APDC in the alkaline medium with the maximum recovery at pH=8. The presence of organic matter slightly modified the complexation by means of somewhat higher recovery percentage at pH lower than 7 and approx. 20% lower recovery at pH higher than 7. Recovery of the elements after separation on DOWEX 50W-X8 resin and preconcentration with APDC at pH=8 varied from 91.4% (Pr) to only 24.9% in the case of Dy. Concentrations of lanthanides measured in standard reference material and environmental samples of red mud after microwave digestion, separation on DOWEX 50W-X8 resin, preconcentration with APDC at pH=8 and recalculation on the percentage of recovery were in good agreement with certified values in the case of SRM as well as with the concentrations obtained by direct determination over Kalpha lines using 241Am excitation source in the case of red mud leading to the conclusion that presented method was applicable for the determination of lanthanides in real environmental samples.