1.Baotou Research Institute of Rare Earths, Baotou 014030,China; 2.National Engineering Research Centre of Rare Earth Metallurgy and Function Materials, Baotou 014030,China
Abstract：The magnesium-neodymium alloy sample was dissolved with hydrochloric acid (1+2). In 0.12-0.25 mol/L hydrochloric acid medium, 2.5 mL of 50 g/L ammonium molybdate solution was added. It reacted with silicon to form silicon molybdenum yellow complex. After stabilizing for 15 min, 5 mL of 10 g/L sulfuric acid-oxalic acid mixed acid was added to decompose phosphorus and arsenic-molybdenum heteropolyacid. Then, 2.5 mL of 10 g/L ascorbic acid solution was added as reducing agent to form stable silicon molybdenum blue complex. After stabilizing for 15 min, the absorbance was measured at 800 nm on spectrophotometer. The content of silicon could be obtained according to the calibration curve. The determination method of silicon in magnesium-neodymium alloy by spectrophotometry was established. The results showed that the mass of silicon in range of 1-50 μg was linear to the absorbance. The linear regression equation of calibration curve was y=61.634 x+0.007 5 with correlation coefficient of r=1.000. The detection limit of silicon in this method was 0.000 11% (mass fraction). The recovery test of silicon in magnesium-neodymium alloy was conducted according to the experimental method. The obtained recoveries were between 97% and 104%. The proposed method was applied to the determination of silicon in actual sample of magnesium-neodymium alloy. The relative standard deviations (RSD, n=11) were between 0.76% and 7.6%. The found results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES).
周郑,闻向东,邵梅.重量法测定白云石中硅含量的不确定度评定[J].广州化工,2013,41(12):156-157.ZHOU Zheng,WEN Xiang-dong,SHAO Mei. Uncertainty measurement for the determination of silicon in dolomite by gravimetric method[J].Guangzhou Chemical Industry,2013,41(12):156-157.
[3]
贺红侠,王洁源,许鸿英,等.氟硅酸钾容量法测定硅锰合金中硅含量的影响因素[J].河北冶金,2015(2):71-72.HE Hong-xia,WANG Jie-yuan,XU Hong-ying,et al.Factors affecting measurement of silicon content in silicon-manganese alloy with potassium fluosilicate volumetric method[J].Hebei Metallurgy,2015(2):71-72.
[4]
王娜,滕新华,王力强,等.酸溶-氟硅酸钾滴定法测定铅锌矿中二氧化硅[J].冶金分析,2015,35(6):65-69.WANG Na,TENG Xin-hua,WANG Li-qiang,et al. Determination of silicon dioxide in lead-zinc ore by potassium fluosilicate titration with acid dissolution[J].Metallurgical Analysis,2015,35(6):65-69.
[5]
周礼仙,郑小敏,苏洋.硅钼蓝分光光度法测定钒铝合金中硅[J].冶金分析,2015,35(11):74-78.ZHOU Li-xian,ZHENG Xiao-min,SU Yang. Determination of silicon in vanadium-aluminum alloy by silicon molybdenum blue spectrophotometry[J].Metallurgical Analysis,2015,35(11):74-78.
[6]
刘雨星,杨三妹,罗稳,等.电感耦合等离子体发射光谱法(ICP-AES)测定铁矿石中的磷、硅、铝[J].精细化工中间体,2015,45(3):76-78. LIU Yu-xing,YANG San-mei,LUO Wen,et al. Determination of phosphorus,silicon,aluminium in iron ore using inductively coupled plasma atomic emission spectrometry[J].Fine Chemical Intermediates,2015,45(3):76-78.
[7]
李玉梅,刘晓杰,郝茜,等.电感耦合等离子体发射光谱法测定稀土精矿中二氧化硅的含量[J].稀土,2012,33(6):57-60. LI Yu-mei,LIU Xiao-jie,HAO Qian,et al.Determination of silicon oxide content in rare earth concentrate by inductively coupled plasma atomic emission spectrometry[J].Rare Earths,2012,33(6):57-60.
[8]
刘伟,曹吉祥,郭云涛,等.熔融制样-X射线荧光光谱法测定硅锰合金中硅锰磷[J].冶金分析,2015,35(8):51-54. LIU Wei,CAO Ji-xiang,GUO Yun-tao,et al.Determination of silicon,manganese,phosphorus in silicon-manganese alloy by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2015,35(8):51-54.
[9]
李强,张学华,黄雪华.X射线荧光光谱法测定海洋沉积物中二氧化硅的测量不确定度评定[J].冶金分析,2014,34(10):78-82. LI Qiang,ZHANG Xue-hua,HUANG Xue-hua. Evaluation of measurement uncertainty for the determination of silicon dioxide in marine sediments by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2014,34(10):78-82.
[10]
王锦利,赵勇,岳航,等.电感耦合等离子体原子发射光谱法测定镁钕合金中3种杂质元素的含量[J].理化检验:化学分册,2014,50(4):455-457.WANG Jin-li,ZHAO Yong,YUE Hang,et al.ICP-AES determination of 3 impurity elements in Mg-Nd alloy[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2014,50(4):455-457.
[11]
刘荣丽.ICP-AES法测定钕镁合金中铝铜铁镍硅量[J].稀有金属与硬质合金,2013,41(5):43-46.LIU Rong-li.Determination of Al,Cu,Fe,Ni and Si contents in Nd-Mg alloy by ICP-AES[J].Rare Metals and Cemented Carbides,2013,41(5):43-46.
王淑英,潘利华,秦宗益,等.电感耦合等离子体原子发射光谱测定镁-钕合金中稀土和非稀土元素[J].分析化学,1993,21(12):1452-1454.WANG Shu-ying,PAN Li-hua,QIN Zong-yi,et al.Determination of rare earth and non-rare earth elements in magnesium-neodymium alloy by inductively coupled plasma-atomic emission spectrometry[J].Chinese Journal of Analytical Chemistry,1993,21(12):1452-1454.
裴秀玲.光度法测定片状五氧化二钒中的硅[J].有色矿冶,2005,21(5):64-64.PEI Xiu-ling.Determination silicon of vancedium oxide by photometry[J].Non-Ferrous Mining and Metallurgy,2005,21(5):64-64.
