The use of Laser Induced Breakdown Spectroscopy as a technique for analysis of europium and samarium concentrations in ceramic aluminum oxide samples was investigated for application to studying lanthanide separation processes. Metal oxide powders of europium and/or samarium were mixed with aluminum oxide at varying concentrations and pressed into pellets. A comparison of different approaches to building a univariate simple linear regression analysis curve is presented. A linear behavior was seen over the total lanthanide concentration range from 0.086 to 12.358 weight percent (wt%). The calculated limits of detection for the univariate calibration curves were determined to range from 0.001 to 0.108 wt% and 0.001 and 0.183 wt% for europium and samarium, respectively.