Rb, Sr and REE (Rare Earth Elements) separation from rock samples using ion-exchange resin has been conducted in the clean laboratry. The silicate rock powder is completely decomposed using mixed acid (40% HF + 60% HClO_4 + 30% HCl)in screwed teflon vessel at c. 110℃ for about one week. Rb, Sr and REE from the rock powder is separated by ion-exchange resin of 7.4cm^3 with hydrochloric acid as eluent. The calibration for Rb, Sr and REE windows are determined using chemical reagents for Rb, Sr and Nd as representation of REE. To verify collected ratio of REE concentration using this method, we carried out quantitative analysis for Nd as representation of REE using ICP-AES. The results indicate that the collected ratio is almost 100%. Consequently, Rb, Sr and REE can be separated from rock samples using this method.