Abstract: Anion exchange resin has been applied to Re separation after acid digestion of Cu-Pb-Zn ores and Re was determined by Inductively Coupled Plasma-Mass Spectrometry(ICP-MS). ReO₄^- in solution was adsorbed by exchange resin and was then eluted from the resin by eluant. This method has a long process, which affects its stability and accuracy. Matrix elements are selected as the goal and 8 g of 732 cation exchange resin in 2% nitric acid medium for 1.5 h static adsorption is used. This method can effectively eliminate the influence of matrix elements on the ICP-MS determination of rhenium. Quartz was used as the blank and mixed with low Re samples. The acquired detection limit was 0.004μg/g, the precision(RSD) is less than 6%, and the recovery ranged from 96% to 104%. The 732 cation exchange resin under the acidic condition has the recovery of >95% for most matrix elements except tungsten and molybdenum, which reduced ionic strength and the concentration of interference elements. Rhenium can be directly determined by ICP-MS, which is simpler and faster than the anion exchange resin separation method.