火花放电原子发射光谱法测定含锆铁铬铝合金校准曲线的扩展及应用  

Extension and application of calibration curve for determination of iron-chromium-aluminum alloy containing zirconium by spark discharge atomic emission spectrometry

作　　者：朱春要 秦建 张继明 董礼男 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)

机构地区：[1]江苏省沙钢钢铁研究院分析测试中心,江苏张家港215625

出　　处：《冶金分析》2023年第12期17-24,共8页Metallurgical Analysis

摘　　要：使用火花放电原子发射光谱法分析含锆铁铬铝合金时,Al、Zr含量均超出了校准曲线的校准范围,导致无法准确分析,从而无法精确指导合金冶炼工艺过程,极大影响了该类产品的合格率。鉴于缺乏铁铬铝合金市场光谱标准样品的现状,通过增加高铬铸铁标样、中低合金钢标样、铬钢标样和自制控制样品完善整体曲线,扩展了Al、Zr校准曲线的分析范围,建立了对含锆铁铬铝合金中C、Si、Mn、P、S、Cr、Ni、Al、Ti、Zr的测定方法。在校正了共存元素干扰后,拟合校准曲线,Al、Zr的测定上限(质量分数)分别由1.53%扩展至5.33%、0.22%扩展至0.57%,Al、Zr校准曲线的决定系数均为0.998。采用实验方法测定含锆铁铬铝合金样品(w(Al)≥3.30%、w(Zr)≥0.28%)中包含Al、Zr在内的10个元素,结果的相对标准偏差(RSD,n=11)为0.05%~4.2%;对比分析了3件含锆铁铬铝生产样品,采用实验方法测定,结果与GB/T 223.8—2000、GB/T 223.11—2008或YS/T 904.X—2013系列标准的测定值基本一致。校准曲线用于含锆铁铬铝样品中C、Si、Mn、P、S、Cr、Ni、Al、Ti、Zr分析,完全满足其工艺过程控制和成品分析要求,解决了火花放电原子发射光谱法无法进行炉前快速分析含锆铁铬铝合金的问题。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

关 键 词：铁铬铝合金 火花放电原子发射光谱法 曲线扩展 干扰校正 铝 锆 

分 类 号：O657.31[理学—分析化学] TF125.13[理学—化学]