Abstract:The neodymium-iron-boron magnetic alloy has been widely used in goods for everyday consumption. With the increasing requirements of goods for everyday consumption in environmental quality, the determination of lead content in neodymium-iron-boron magnetic alloy was attracting attention. The sample was dissolved with aqua regia. The calibration curve was established by iron matrix matching method, and the background was deducted by deuterium lamp. Thus, a determination of lead content in neodymium-iron-boron magnetic alloy by air-acetylene flame atomic absorption spectrometry was realized at spectral line of Pb 283.3nm. The effect of main matrix elements including neodymium, iron and boron in sample on determination of lead was systemically investigated. The results showed that the influence of boron and neodymium could be ignored. However, the interference of iron could not be neglected. According to the structural formula (Nd2Fe14B) of main hard magnetic phase in neodymium-iron-boron magnetic alloy, the mass fraction of iron was approximately 71%. It could be calculated that the mass concentration of iron in sample solution was about 2840mg/L after the sample was digested and diluted to constant volume according to the experimental method. The experiments indicated that the absorbance of lead were stable when the mass concentration of iron was in range of 1600-3600mg/L, while, they were much higher than that of matrix blank. Therefore, the matrix interference was finally eliminated by matching 2800mg/L of iron. Under the selected experimental conditions, the linear range of method was 0.10-5.00mg/L, the correlation coefficient was 0.999, and the detection limit was 0.02mg/L. The content of lead in three neodymium-iron-boron magnetic alloy actual samples was determined according to the experimental method. The relative standard deviation (RSD, n=6) was less than 6%, and the recoveries were between 93% and 103%. According to the limit requirement of lead in goods for everyday consumption, the simulated sample of neodymium-iron-boron magnetic alloy with lead content of 1000mg/kg was prepared and determined by the proposed method. The results were basically consistent with the theoretical values.
胡伯平.钕铁硼稀土磁体产业发展及市场前景[J].磁性材料及器件,2012,43(6):1-8.HU Bo-ping.Development of Nd-Fe-B rare earth magnet industry and market prospect[J].Journal of Magnetic Materials and Devices,2012,43(6):1-8.
[2]
闫文龙,颜世宏,于敦波,等.烧结钕铁硼的发展及其应用现状[J].金属功能材料,2008,15(6):33-37.YAN Wen-long,YAN Shi-hong,YU Dun-bo,et al.Application and development of sintered NdFeB magnets in the world[J].Metallic Functional Materials,2008,15(6):33-37.
[3]
徐静,李明来,李世鹏,等.ICP-AES法高精度测定钕铁硼合金中主量元素[J].中国稀土学报,2014,32(2):234-239.XU Jing,LI Ming-lai,LI Shi-peng,et al.Determination of main components in Nd-Fe-B alloy with high precision by inductively coupled plasma atomic emission spectrometry[J].Journal of the Chinese Rare Earth Society,2014,32(2):234-239.
[4]
代春燕.ICP-OES法同时测定钕铁硼合金中20种元素含量[J].广州化工,2013,41(17):122-124.DAI Chun-yan.Simultaneous determination of twenty elements in Nd-Fe-B alloy by ICP-OES[J].Guangzhou Chemical Industry,2013,41(17):122-124.
[5]
刘晓杰,许涛,于亚辉,等.ICP-AES法测定钕铁硼废料中非稀土杂质[J].稀土,2013,34(6):51-55.LIU Xiao-jie,XU Tao,YU Ya-hui,et al.Determination of non-rare earth impurities in NdFeB waste by inductively coupled plasma-atomic emission spectrometry[J].Chinese Rare Earths,2013,34(6):51-55.
[6]
刘永明.ICP-AES法测定钕铁硼永磁材料中常量元素[J].光谱学与光谱分析,2004,24(10):1257-1259.LIU Yong-ming.Determination of main components in Nd-Fe-B magnetic materials by ICP-AES[J].Spectroscopy and Spectral Analysis,2004,24(10):1257-1259.
[7]
许涛,宋秀荣.钕铁硼合金中铝量的测定—N2O-C2H2原子吸收光谱法[J].稀土,2000,21(1):49-52.XU Tao,SONG Xiu-rong.Determination of aluminum in NdFeB alloy by N2O-C2H2 flame atomic absorption spectrometric method[J].Chinese Rare Earths,2000,21(1):49-52.
[8]
Garcia I L,Cordoba M H.Fast determination of lead in commercial iron oxide pigments by graphite furnace atomic absorption spectrometry using a slurry technique[J].Journal of Analytical Atomic Spectrometry,1989,4(8):701-704.
[9]
Barbosa U A,Santos I F,Santos A M,et al.Determination of Lead in Iron Supplements by Electrothermal Atomization Atomic Absorption Spectrometry[J].Analytical Letters,2016,49(6):799-807.
[10]
Vanloo B,Dams R,Hoste J,et al.Determination of bismuth and lead in steel and cast iron by hydride generation and zeeman atomic absorption spectrometry[J].Analytica Chimica Acta,1983,151(2):391-400.