电感耦合等离子体原子发射光谱法测定铈铁合金中铝硅镍
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摘要
铈铁合金作为稀土钢的添加剂,对提高稀土钢的产品性能有重要的作用,而快速准确地测定铈铁合金中铝、硅、镍,对产品的质量控制具有重要意义。采用盐酸、硝酸溶解样品,选择Al 396.153nm、Si 251.612nm、Ni 231.604nm为分析谱线,采用基体匹配和空白校正的方法校正基体的影响,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定铈铁合金中铝、硅、镍。各元素质量分数在0.005 0%~0.20%范围内校准曲线呈线性,相关系数均大于0.999 9;方法中铝、硅、镍检出限分别为0.001 2%、0.000 6%、0.000 3%。实验方法用于测定铈铁合金中铝、硅、镍,结果的相对标准偏差(RSD,n=11)小于7%,回收率为90%~115%。按照实验方法测定铈铁合金中铝、硅、镍,并采用分光光度法测定硅、电感耦合等离子体质谱法(ICP-MS)测定铝和镍,测定结果相吻合。
Cerium-iron alloy was a kind of additive for rare earth steel,and it played an important role in enhancing the performance of rare earth steel products.The rapid and accurate determination of aluminum,silicon and nickel in cerium-iron alloy has great significance for the quality control of products.The sample was dissolved with hydrochloric acid and nitric acid.Al 396.153 nm,Si 251.612 nm and Ni 231.604 nm were selected as the analytical lines.The matrix effect was corrected by matrix matching and blank correction.The content of aluminum,silicon and nickel in cerium-iron alloy was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The calibration curves of elements were linear when the mass fraction was in range of 0.005 0%-0.20%,and the correlation coefficients were all higher than 0.999 9.The detection limit of aluminum,silicon and nickel for method was 0.001 2%,0.000 6%and0.000 3%,respectively.The proposed method was applied for the determination of aluminum,silicon and nickel in cerium-iron alloy.The relative standard deviations(RSD,n=11)of results were less than 7%,and the recoveries were between 90% and 115%.The content of aluminum,silicon and nickel in cerium-iron alloy was determined according to the proposed method.Meanwhile,the content of silicon was also determined by spectrophotometry,and the content of aluminum and nickel was determined by inductively coupled plasma mass spectrometry(ICP-MS).It was found that the determination results were consistent for different test methods.
Cerium-iron alloy was a kind of additive for rare earth steel,and it played an important role in enhancing the performance of rare earth steel products.The rapid and accurate determination of aluminum,silicon and nickel in cerium-iron alloy has great significance for the quality control of products.The sample was dissolved with hydrochloric acid and nitric acid.Al 396.153 nm,Si 251.612 nm and Ni 231.604 nm were selected as the analytical lines.The matrix effect was corrected by matrix matching and blank correction.The content of aluminum,silicon and nickel in cerium-iron alloy was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The calibration curves of elements were linear when the mass fraction was in range of 0.005 0%-0.20%,and the correlation coefficients were all higher than 0.999 9.The detection limit of aluminum,silicon and nickel for method was 0.001 2%,0.000 6%and0.000 3%,respectively.The proposed method was applied for the determination of aluminum,silicon and nickel in cerium-iron alloy.The relative standard deviations(RSD,n=11)of results were less than 7%,and the recoveries were between 90% and 115%.The content of aluminum,silicon and nickel in cerium-iron alloy was determined according to the proposed method.Meanwhile,the content of silicon was also determined by spectrophotometry,and the content of aluminum and nickel was determined by inductively coupled plasma mass spectrometry(ICP-MS).It was found that the determination results were consistent for different test methods.
引文
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[3]聂玲清.高分辨电感耦合等离子体质谱法测定钢中痕量铈[J].冶金分析,2009,29(8):11-15.〗NIE Ling-qing.Determination of trace cerium in steel by high-resolution inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2009,29(8):11-15.
[4]刘方升.稀土Ce对4145H钻铤热轧过程组织及性能的影响[D].包头:内蒙古科技大学,2014.LIU Fang-sheng.Effect of rare earth Ce on microstructure and properties of 4145H drill collar during hot rolling[D].Baotou:Inner Mongolia University of Science and Technology,2014.
[5]温世杰,周俊海,张少夫.电感耦合等离子体原子发射光谱法测定钇铁合金中铝、硅、钙、镁、锰[J].有色金属科学与工程,2016,7(1):133-136.WEN Shi-jie,ZHOU Jun-hai,ZHANG Shao-fu.Determination of Al,Si,Ca,Mg,Mn in yttrium-iron alloy by inductively coupled plasma atomic emission spectrometry[J].Nonferrous Metals Science and Engineering,2016,7(1):133-136.
[6]杨新能,冯宗平,羊绍松,等.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,et al.Determination of impurity elements in ferrovanadium alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(11):37-41.
[7]侯社林,李存根,陈延昌,等.电感耦合等离子体原子发射光谱法测定铝铁合金中硅磷锰钛[J].冶金分析,2012,32(9):40-42.HOU She-lin,LI Cun-gen,CHEN Yan-chang.Inductively coupled plasma atomic emission spectrometric determination of silicon,phosphorus,manganese and titanium in ferroaluminum alloy[J].Metallurgical Analysis,2012,32(9):40-42.
[8]高原一,何小庆.铁合金中钼、镍、锰、硅、磷量的快速测定研究[J].信息化建设,2016(1):289.GAO Yuan-yi,HE Xiao-qing.Rapid determination of molybdenum,nickel,manganese,silicon and phosphorus in ferroalloys[J].Information Construction,2016(1):289.
[9]刘青山.铁合金中钼、镍、锰、硅、磷量的快速测定研究[J].科学之友,2010(6):7-8.LIU Qing-shan.Rapid determination of molybdenum,nickel,manganese,silicon and phosphorus in ferroalloys[J].Friends of Science,2010(6):7-8.
[10]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 progress in inductively coupled plasma atomic emission spectrometric analysis instruments and methods[J].Metallurgical Analysis,2014,34(11):1-10.
[11]崔爱端,张秀燕.ICP-AES法测定镨钕氧化物及镨钕金属中的镧、铈、钐、钇、铝和硅量[J].稀土,2006,27(4):75-77.CUI Ai-duan,ZHANG Xiu-yan.ICP-AES detecting method for La,Ce,Sm,Y,Al and Si in Pr-Nd oxide and metal[J].Chinese Rare Earths,2006,27(4):75-77.