Abstract:The calibration curve was prepared using nine certified reference materials of middle-low alloy steel with various gradients of zirconium content. The determination method of zirconium in middle-low alloy steel by direct current glow discharge atomic emission spectrometry was established. The effect of experimental parameters of direct current glow discharge spectrometer on the determination of zirconium in middle low alloy steel was investigated by single factor method. The following conditions were obtained as follow: the excitation voltage was 1250V, the excitation current was 45mA, the pre-combustion time was 60s, and the integration time was 10s. The calibration curve was plotted using the spectral intensity of zirconium as horizontal ordinate and the corresponding mass fraction as the vertical coordinate. The linear correlation coefficient of calibration curve was 0.9961, and the linear range was 0.0044%-0.35%. The proposed method was applied to the determination of zirconium in standard samples of middle-low alloy steel. The found results were consistent with the certified values. The relative standard deviations (RSD, n=11) were between 0.72% and 1.7%, which could meet the recommended measurement requirements of instrument (RSD was less than 3%). The proposed method was applied to the determination of zirconium in actual samples of middle-low alloy steel. The found results were in good agreement with those obtained by national standard method (GB/T 223.30-1994).
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