For the quantitative surface analysis of multicomponent materials, algorithms for the compensation of the matrix effect and surface compositional change by ion beam sputtering must be established and reference materials having certified compositions are necessary. These certified reference material (CRM)s are needed for the improvement of instrument performance, inter-laboratory comparison and quantitative surface analysis. Surface analysis group of KRISS developed alloy thin film CRMs by and ion beam sputter deposition system and in-situ surface analysis system to control the composition of alloy thin films The real compositions of the CRMs were certified by inductively coupled plasma-atomic emission spectroscopy (ICP-AES).