Extension and application of calibration curve for determination of iron-chromium-aluminum alloy containing zirconium by spark discharge atomic emission spectrometry
ZHU Chunyao, QIN Jian, ZHANG Jiming, DONG Li′nan
Analysis and Characterization Center, Institute of Research of Iron and Steel, Jiangsu Province/Sha-steel, Zhangjiagang 215625, China
Abstract：During the analysis of iron-chromium-aluminum (Fe-Cr-Al) alloy containing zirconium by spark discharge atomic emission spectrometry, the contents of Al and Zr elements exceeded the range of calibration curve, which led to the failure of accurate analysis and thus the inability to guide the alloy smelting process accurately. Therefore, the qualification rate of such products was greatly affected. In view of the lack of iron-chromium-aluminum alloy certified reference materials for spectral analysis in the market, the global curve was improved by adding the certified reference materials of high-chromium cast iron, medium-low alloy steel, chrome steel, and self-made control samples. The analysis ranges of Al and Zr calibration curves were expanded. Thus, a determination method of C, Si, Mn, P, S, Cr, Ni, Al, Ti and Zr in iron-chromium-aluminum alloy containing zirconium was established. After correcting the interference of coexisting elements, the calibration curves were fitted, and the upper determination limit of Al and Zr (mass fraction) was expanded from 1.53% and 0.22% to 5.33% and 0.57%, respectively. The determination coefficients of calibration curves for Al and Zr were both 0.998. The contents of 10 elements including Al and Zr in iron-chromium-aluminum alloy containing zirconium (w(Al)≥3.30%, w(Zr)≥0.28%) were determined according to the proposed method, and the relative standard deviations (RSD, n=11) of determination results were 0.05%-4.2%. Three production samples of iron-chromium-aluminum alloy containing zirconium were compared and analyzed. The determination results were consistent with those obtained by GB/T 223.8-2000, GB/T 223.11-2008 or YS/T 904.X-2013. The calibration curves were used for the analysis of C, Si, Mn, P, S, Cr, Ni, Al, Ti, Zr in iron-chromium-aluminum alloy containing zirconium, and it could met the requirements of process control and products analysis. The proposed method solved the problem that the online rapid analysis of iron-chromium-aluminum alloy containing zirconium could not be realized by spark discharge atomic emission spectrometry.
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