Abstract:The sample was dissolved by nitric acid and hydrofluoric acid. The Zr 327.305 nm was selected as analytical line. The analysis method of zirconium content in hafnium alloy by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The results showed that the determination results of zirconium were insignificantly affected by hafnium when the mass concentration of hafnium was lower than 100 μg/mL. The matrix matching method was not required to prepare the calibration curve. Since the acidity had influence on the determination results of zirconium, the acidity of testing solution should be consistent with the standard solution series. In the experiment, the acidity was about 1.0 mol/L. When the mass concentration of zirconium was in range of 0.2-5.0 μg/mL, the linear regression equation of calibration curve was y=39 966 x+176 with correlation coefficient of r=0.999 7. The detection limit of zirconium was 0.001 5 μg/mL. The proposed method was applied to the determination of zirconium in hafnium alloy. The relative standard deviation (RSD, n=6) was less than 1%, and the recovery was 99%. Meanwhile, the proposed method was compared with X-ray fluorescence spectrometry. It was found that the determination results of two methods were basically consistent.
李中奎,刘建章.中国核用锆铪材料的现状和未来发展[J].稀有金属快报,2004,23(5):10-14.LI Zhong-kui,LIU Jian-zhang.Current situation and future development of the Chinese nuclear materials of zirconium and hafnium [J].Rare Metals Letters,2004,23(5):10-14.
[2]
魏占海,王力军,熊炳昆.核电发展为我国锆铪产业带来发展机遇[J].稀有金属快报,2007,26(1):10-13.WEI Zhan-hai,WANG Li-jun,XIONG Bing-kun.The development of nuclear power has brought opportunities for the development of zirconium and hafnium[J].Rare Metals Letters,2007,26(1):10-13.
[3]
罗新文,罗方承.锆铪材料的性质、应用、生产技术与发展前景[J].江西冶金,2009,29(4):39-41.LUO Xin-wen,LUO Fang-cheng.Zirconium and hafnium materials properties, application, production technology and development prospects[J].Jiangxi Metallurgy,2009,29(4):39-41.
[4]
李军丽,王之昌,于秀兰.锆铪的光度分析进展[J].稀有金属与硬质合金,2007,35(4):36-40.LI Jun-li,WANG Zhi-chang,YU Xiu-lan.Progress in spectrophotometric determination of zirconium and hafnium[J].Rare Metals and Cemented Carbide,2007,35(4):36-40.
[5]
罗志刚,张国权,吕小欢.二甲酚橙分光光度法测定锆和铪[J].华南农业大学学报,1998,19(9):92-97.LUO Zhi-gang,ZHANG Guo-quan,L Xiao-huan.Determination of zirconium and hafnium by two xylenol orange spectrophotometric method[J].Journal of South China Agricultural University,1998,19(9):92-97.
[6]
XU Zhi-gao,WANG Li-jun,WU Yan-ke,et al.Mechanisms of extraction and separation of zirconium and hafnium by DIBK-P204 system [J].The Chinese Journal of Nonferrous Metals, 2013(7):2061-2068.
[7]
葛思清.EDTA络合滴定法测定锆英石中的锆铪合量[J].天津化工,2013(6):42-43.GE Si-qing.Determine the content of zirconium and hafnium in zirconite by EDTA complexometry method[J].Tianjin Chemical Industry,2013(6):42-43.
[8]
Mohsen Aliakbari,Kamal Saberyan,Mohammad Noaparast,et al.Separation of hafnium and zirconium using TBP modified ferromagnetic nanoparticles: Effects of acid and metals concentrations[J].Hydrometallurgy,2014,146(3):72-75.
[9]
Abd El Hamid A M,Zahran M A,Khalid F M,et al.Leaching of hafnium,zirconium,uranium and other nuclear economic elements from petroleum ash [J].RSC Advance,2014,24:12506-12513.
[10]
李红光,王雪,王哲,等.电感耦合等离子体原子发射光谱法测定锆钛砂矿中锆钛铁钍铪[J].冶金分析,2014,34(2):62-65.LI Hong-guang,WANG Xue,WANG Zhe,et al.Determination of zirconium,titanium,iron,thorium and hafnium in zirconium-titanium placer by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(2):62-65.
[11]
童坚,吴辛友,李满芝,等.锆铪的ICP-AES 分析方法研究及应用[J].现代科学仪器,2000(4):62-63.TONG Jian,WU Xin-you,LI Man-zhi,et al.Study on analytical method of ICP-AES for zirconium and hafnium and its'application [J].Modern Scientific Instruments,2000(4):62-63.