Abstract:The analytical conditions of copper, niobium, silicon and boron in FeCuNbSiB alloy by spark source atomic emission spectrometry were discussed. The optimal analytical conditions were as follows: the flow rate of high-purity argon (φ≥99.999%) was 180 L/h, the flush time of argon was 4 s, the pre-combustion (HEPS) time was 6 s, the integral time for silicon, niobium, boron and copper was 8 s, 8 s, 3 s and 3 s, respectively. The calibration curves of copper, niobium, silicon and boron were prepared using the self-made standard samples. The calibration curves were fitted after correcting the interference of coexisting elements. The analytical lines of B 345.1 nm/Fe 360.7 nm were used to prepare the calibration curve of high-content boron, and the analytical range of boron was 0.94%-3.37%. The analytical lines of Nb 319.5 nm/Fe 297.1 nm were used to prepare the calibration curve of niobium, extending the calibration curve of niobium in steel which had been established in instrumental software. The analytical range of niobium was extended to 0.002 0%-7.16%. The analytical lines of Si 390.6 nm/Fe 281.3 nm and Cu 212.3 nm/Fe 216.2 nm were used to prepare the calibration curve of silicon and copper, respectively. The calibration curves of silicon and copper in steel which had been established in instrumental software were improved. The analytical range of silicon and copper was 0.010 0%-19.40% and 0.001 3%-3.95%, respectively. The proposed method was applied to the determination of copper, niobium, silicon and boron in FeCuNbSiB alloy sample, and the relative standard deviations (RSD, n=8) of determination results were less than 1.0%. The found results were consistent with those obtained by gravimetric method and inductively coupled plasma atomic emission spectrometry (ICP-AES). The copper, niobium, silicon, boron and other alloying elements in FeCuNbSiB alloy sample could be simultaneously determined after excitation once of analytical samples.
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