1.Jiangsu Longda Superalloy Material Co.,Ltd.,Wuxi 214105,China; 2.Analysis & Characterization Center,Institute of Research of Iron & Steel,Jiangsu Province/Sha-Steel,Zhangjiagang 215625,China
Abstract:The sample was dissolved with hydrochloric acid, hydrofluoric acid, perchloric acid and nitric acid. Zr 257.139 nm was selected as the analytical line. The influence of matrix effect was eliminated by preparing calibration curves using high purity iron matrix matching method. The determination method of high content zirconium in silicon-zirconium alloy by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The mass fraction of zirconium in range of 3.04%-30.42% was linear to the corresponding emission intensity. The linear correlation coefficient of calibration curve was 0.999 8. The detection limit was 0.007% (mass fraction), and the low limit of determination was 0.033%. The content of zirconium in actual sample and standard sample of silicon-zirconium alloy was determined according to the experimental method. The relative standard deviations (RSD, n=6) were less than 1.2%. The proposed method was applied to the determination of zirconium in three silicon-zirconium alloy samples, and the found results were consistent with those obtained by mandelic acid gravimetry.
陈景友.碳热法冶炼硅锆合金的实践[J].铁合金,2008(5):24-25,28.CHEN Jing-you.Smelting ferrozirconium-silicon with carbothermic method[J].Ferro-Alloys,2008(5):24-25,28.
[2]
赵乃成,张启轩.铁合金生产实用技术手册[M].北京:冶金工业出版社,1998:272-274.
[3]
张文和,丁俊,聂富荣.几种孕育剂简介[J].现代铸铁,2007(4):71-73.ZHANG Wen-he,DING Jun,NIE Fu-rong.A brief introduction to some inoculants[J].Modern Cast Iron,2007(4):71-73.
[4]
王海舟.铁合金分析[M].北京:科学出版社,2003:362-363.
[5]
孙宇红,徐炜.EDTA络合滴定法测定铝锆中间合金中的锆[J].兵器材料科学与工程,2004,27(5):47-48.SUN Yu-hong,XU Wei.Determining Zr content in Al-Zr alloy with EDTA complexometric titration method[J].Ordnance Material Science and Engineering,2004,27(5):47-48.
[6]
周锡林,尹继先,刘纪勇,等.铝锆合金的微波消解及锆测定[J].稀有金属与硬质合金,2010,38(4):56-59.ZHOU Xi-lin,YIN Ji-xian,LIU Ji-yong,et al.Microwave digestion and zirconium determination of A1-Zr alloy[J].Rare Metals and Cemented Carbides,2010,38(4):56-59.
李洁,王占明.电感耦合等离子体原子发射光谱法测定铪合金中锆[J].冶金分析,2016,36(1):71-74.LI Jie,WANG Zhan-ming.Determination of zirconium in hafnium alloy by inductively coupled plasma atomic emission spectrometry[J]. Metallurgical Analysis,2016,36(1):71-74.
[10]
周西林,王娇娜,刘迪,等.电感耦合等离子体原子发射光谱法在金属材料分析应用技术方面的进展[J].冶金分析,2017,37(1): 39-46.ZHOU Xi-lin,WANG Jiao-na,LIU Di,et al.Progress in application of inductively coupled plasma atomic emission spectrometry in analysis of metal materials[J].Metallurgical Analysis,2017,37(1):39-46.