Abstract: The ferrovanadium slag sample was fused with sodium carbonate-boric acid at high temperature, then acidified with hydrochloric. Vanadium 310.230 nm, iron 259.940 nm, manganese 257.610 nm and phosphorus 213.618 nm were selected as the analytical lines. The matrix matching method was used to eliminate the influence of matrix effect, the determination method of vanadium, iron, manganese and phosphorus contents in ferrovanadium slag by alkali fusion-inductively coupled plasma atomic emission spectrometry was established. The results showed that the linear correlation coefficients of calibration curves were all higher than 0.999, the limit of detection for vanadium, iron, manganese and phosphorus was 0.0076 μg/mL, 0.0093 μg/mL, 0.0065 μg/mL and 0.0051 μg/mL, respectively. Two ferrovanadium slag certified reference materials were determined according to the experimental method, the relative standard deviations(RSD, n=8) were less than 3.9 %.