Abstract:The surface of sample was treated by milling sample machine. Trace calcium and boron in cold forging steel was determined by spark source atomic emission spectrometry with the cutting depth of 2 mm. The analytical conditions of instrument were optimized. The calibration curves of calcium and boron were established using foreign CRMs. The detection limits of calcium and boron were 0.2 μg/g. This method was applicable for the determination of calcium in the range of 0.000 1%-0.015% (mass fraction) and boron in the range of 0.000 1%-0.012% in cold forging steel. The precision was investigated with calcium-boron low alloy steel CRM of No. B.S. CA1A,when the mass fraction of Ca and B was 0.002 1% and 0.001 0%,the relative standard deviation of the determination was 3.5% and 3.9%,respectively. The calcium-boron low alloy steel CRM and actual cold forging steel samples were analyzed, and the determination results were consistent with those obtained by wet method.