Solvent extraction experiments have been performed to separate Nd and Pr from chloride leaching solution of monazite sand using single Cyanex272 and mixed extractants as PC88A+Cyanex272 and PC88A+TBP. For this purpose, the effect of the concentration of extractants on the extraction and separation of the two metals were studied by varying the pH of aqueous solution. In the experimental ranges conducted in this study, the distribution coefficients of Nd were higher than those of Pr. In Cyanex272 system, our results indicated that concentration of extractant and initial pH did not affect distribution coefficients, but separation factor was increased with increasing initial pH. In binary extractant system, distribution coefficients were lower than those of single PC88A system, whereas separation factor was similar in both mixed and single extractant system.