Abstract: A method for determination of chemical composition of ultra-low carbon cold-reduced sheet steel by spark source-AES was proposed.The cube-shaped standard samples for AES analysis were used to prepare calibration curves.The samples was treated by submerged polishing,and adhered on an iron cube with specified binder to avoid its breaking down during electric discharge.The proposed method was applied to the analysis of 4 standard samples,giving results in consistency with the standard values.