Abstract：The new technology, which used V2O5, Cr2O3 and TiO2 for direct reduction and smelting of vanadium-chromium-titanium alloy, could significantly decrease the production cost. However, the influence of introduced impurities by raw materials, reducing reagents and smelting equipment on the product quality should be solved. Therefore, a determination method of 11 microelements including Al, As, Co, Cu, Fe, Mg, Mn, Ni, P, K and Na in vanadium-chromium-titanium (V-4Cr-4Ti) alloy was established by inductively coupled plasma atomic emission spectrometry (ICP-AES). The influencing factors such as matrix effect, spectral interference and continuous background superposition were focused in the system where V, Cr and Ti were coexisting. The interference of high-sensitivity spectral lines by matrix effect and coexisting components was investigated. The analytical lines of testing elements, the background correction area and the working conditions of spectrometer were optimized. The matrix matching and synchronous background correction were used to eliminate the influence of coexisting matrix with high V, high Cr and high Ti. The results showed that the detection range of Al, As, Co, Cu, Fe, Mg, Mn, Ni and P was 0.001%-0.25%, while the detection range of K and Na was 0.002%-0.25%. The linear correlation coefficients of calibration curve were not less than 0.9995. The low limit of determination was 0.0012% (K), 0.0015% (Na), and 0.0003%-0.0009% (other elements). The proposed method was applied for the determination of Al, As, Co, Cu, Fe, Mg, Mn, Ni, P, K and Na in four V-4Cr-4Ti alloy samples. The relative standard deviations (RSD, n=8) of determination results at 0.x% level were less than 5%, and the RSD (n=8) of determination results at 0.0x%-0.00x% were less than 10%. Even for the determination results which were lower than the determination limit of method (i.e., 0.001%), the RSD (n=8) was still less than 15%. The recovery tests of Al, As, Co, Cu, Fe, Mg, Mn, Ni, P, K and Na in four V-4Cr-4Ti alloy samples were conducted according to the experimental method. The recoveries were between 90% and 114%. The proposed method was applied for the determination of Al, As, Co, Cu, Fe, Mg, Mn, Ni, P, K and Na in three V-4Cr-4Ti alloy samples, and the results were consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS).
李增德,崔舜,林晨光,等.聚变用V-Cr-Ti合金的研究现状与展望[J].稀有金属,2007,31(6):1-4.LI Zeng-de,CUI Shun,LIN Chen-guang,et al.Current research state and prospects of V-Cr-Ti alloys designing for fusion applications[J]. Chinese Journal of Rare Metals,2007,31(6):1-4.
[2]
李鱼飞,罗超,王志钢,等.真空自耗电弧重熔V-4Cr-4Ti合金的微观组织结构[J].中国有色金属学报,2008,18(5):805-811.LI Yu-fei,LUO Chao,WANG Zhi-gang,et al.Microstructure of V-4Cr-4Ti alloy fabricated by vacuum are remeltion of consumable electrode[J].The Chinese Journal of Nonferrous Metals,2008,18(5):805-811.
[3]
李鱼飞,罗超,王志钢.VAR法制备钒合金的工艺探索[J].稀有金属,2007,31(增):53-38.LI Yu-fei,LUO Chao,WANG Zhi-gang.Technology exploration of fabricate vanadium alloys by VAR[J].Chinese Journal of Rare Metals,2007,31(Suppl.):53-38.
[4]
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.Inductively coupled plasma atomic emission spectrometry metal material application technology progress[J].Metallurgical Analysis,2017,37(1):39-46.
[5]
郑国经.电感耦合等离子体原子发射光谱分析仪器与方法的新进展[J].冶金分析,2014,34(11):1-10.ZHENG Guo-jing.New advances in inductively coupled plasma atomic emission spectrometries instruments and mtehods[J].Metallurgical Analysis,2014,34(11):1-10.
[6]
杨新能,冯宗平,羊绍松.电感耦合等离子体原子发射光谱法测定钒铁合金中杂质元素[J].冶金分析,2014,34(11):37-41.YANG Xin-neng,FENG Zong-ping,YANG Shao-song.Determination of impurity elements in ferrovanadium alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(11):37-41.
[7]
成勇,敬守斌.电感耦合等离子体原子发射光谱法测定钒铝合金中15种杂质元素[J].理化检验:化学分册,2013,49(1):44-47.CHENG Yong,JING Shou-bin.ICP-AES determination of 15 impurity elements in V-Al alloy[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2013,49(1):44-47.
[8]
冯宗平.电感耦合等离子体原子发射光谱法测定氧化钒中钾钠硫磷铁[J]. 冶金分析,2010,30(3):30-33.FENG Zong-ping.Determination of potassium,sodium,phosphorus,sulfur and iron in vanadium oxide by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2010,30(3):30-33.
[9]
黎涛,冯自平,陈金发,等.电感耦合等离子体原子发射光谱法测定偏钒酸铵中钒含量[J].理化检验:化学分册,2011,47(9):1086-1087.LI Tao,FENG Zi-ping,CHEN Jin-fa,et al.ICP-AES determination of vanadium in ammonium metavana[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2011,47(9):1086-1087.
[10]
赵君威,梅坛,鄢国强,等.电感耦合等离子体原子发射光谱分析中的光谱干扰及其校正的研究进展[J].理化检验:化学分册,2013,49(3):334-339.ZHAO Jun-wei,MEI Tan,TAN Guo-qiang.Spectral interference and its correction in ICP-AES analysis[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2013,49(3):334-339.
