Abstract:A comparative evaluation was carried out to determine the trace metallic constituents in nuclear-grade BeO by D.C. arc carrier distillation and inductively coupled plasma atomic emission spectrometry. D.C. arc carrier distillation is accomplished by physical separation of the major matrix to avoid interference, while ICP-AES employs the solution route because chemical separation of the major matrix is preferred. The method was optimized for Ca, Fe, Mg, Mn, Si, Na, Li, Al, B, Cd, Cr, Cu, Ni, and Zn at minor and trace levels and was optimized using multiple standards and validated using synthetic samples. The analytical performance for both techniques, including detection limits, sensitivity, linear dynamic range, etc., was compared. Though both techniques were found to be suit- able for analysis of nuclear-grade BeO samples, some differences were observed. ICP-AES provides better analytical performance, while D.C. arc requires less sample handling, minimizes process pickup, and results in less toxic expossure in the laboratory.