The aim of this research was to develop and optimize a procedure for determination of REEs in xenotime and monazite samples collected from Bangka Island, which were compared to Standard Monazite (71 AG) of Bureau of Analyzed Samples, London. ICP-OES method was used for the determination. The samples were dried and sterilized by heating for a week at 110°C, before digesting with nitric acid and hydrofluoric acid, using a microwave-assisted digestion system. After a careful line selection, at the detection limits for all REEs in the ng/mL the REEs were reliably obtained at the 0.09 – 38% level.