Determination of trace scandium in vanadium-titanium magnetite by inductively coupled plasma atomic emission spectrometry combined with alkali fusion and co-precipitation enrichment separation
XIAO Fang1,2,3, NI Wenshan*1,2,3, MAO Xiangju1,2,3, ZHANG Hongli1,2,3, ZHANG Liping1,2,3, SUN Qiliang1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, Zhengzhou 450006, China; 2. China National Engineering Research Center for Utilization of Industrial Minerals, Zhengzhou 450006, China; 3. Key Laboratory for Polymetallic Ores' Evaluation and Utilization, MNR, Zhengzhou 450006, China
Abstract：The vanadium-titanium magnetite sample was fused in muffle furnace at 750 ℃ with a mixed flux of sodium peroxide and sodium hydroxide. Then the melt was leached with boiling triethanolamine(1+9). Iron, titanium and aluminum could complex with triethanolamine and were transferred into the solution. Meanwhile, vanadium also entered the solution in the form of oxysalt. 3 mL of 10 g/L magnesium chloride solution was added to form magnesium hydroxide hydroxide precipitate. During this process, trace scandium in the solution was co-precipitated with magnesium hydroxide, realizing the separation from other elements in the matrix solution. After filtration, the precipitate was dissolved with boiling HCl (1+1). An analysis method for the determination of trace scandium in vanadium-titanium magnetite by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established with Sc 363.075{92} nm as analytical line. The results showed that the method of magnesium hydroxide co-precipitation could separate scandium from interfering elements (iron, titanium, vanadium, chromium, sodium, silicon and aluminum) in the sample, avoiding the interferences of matrix. Under the selected experimental conditions, the emission spectral intensity of scandium had a good linear relationship with its mass concentration in the range of 0.050-2.00 μg/mL. The linear correlation coefficient (r) of the calibration curve was 0.999 9. The limit of detection of the method was 1.5 μg/g, and the limit of quantification was 5 μg/g. The proposed method was applied for the determination of scandium in vanadium-titanium magnetite samples. The relative standard deviations (RSDs, n=6) were 0.58%-2.3%, and the recoveries were 96%-103%. The determination results were consistent with those obtained by spectrophotometry.
张进才,孙明星.分光光度法测定钒钛磁铁矿中痕量钪[J].冶金分析,1991,11(6):53-55.ZHANG Jincai,SUN Mingxing.Spectrophotometric determination of trace scandium in vanadium titanium magnetite[J].Metallurgical Analysis,1991,1(6):53-55.
[3]
杨金秀,张古英.偶氮氯膦Ⅲ分光光度法快速测定钒钛磁铁矿中的微量钪[J].矿冶工程,1992,12(4):67-69.YANG Jiuxiu,ZHANG Guying.The rapid spectrophotometric determination of scandium in vanadium titanium magnetite by azocloclodrine III[J].Mining and Metallurgical Engineering,1992,12(4):67-69.
[4]
林筑,孔凡军,郑美娟,等.离子交换树脂分离-分光光度法测定赤泥中钪[J].冶金分析,2016,38(8):73-77.LIN Zhu,KONG Fanjun,ZHENG Meijuan,et al.Determination of scandium in red mud by ion exchange resin separation and spectrophotometry[J].Metallurgical Analysis,2016,38(8):73-77.
[5]
罗宗铭,彭少锋.钪-埃铬菁R-氯化十六烷基吡啶-乳化剂OP显色体系及其应用研究[J].岩矿测试,1996, 15(3):213-216.LUO Zongming,PENG Shaofeng.Chromogenic system of scandium(Ⅲ)-eriochrome cyanine R-CPC-OP and its application[J].Rock and Mineral Analysis,1996,15(3):213-216.
[6]
董壮龙,魏正妍,韩国防.二溴对羧基氯磺酚光度法测定地质物料中痕量钪[J].岩矿测试,1998,17(2):131-133,137.DONG Zhuanglong,WEI Zhengyan,HAN Guofang.Spectrophotometric determination of trace scandium in geological materials by dibromo-carboxyl chlorosulfonyl[J]. Rock and Mineral Analysis,1998,17(2):131-133,137.
[7]
张进才.钒钛磁铁矿及其冶金产物中微量钪的分离、示波极谱法测定[J].冶金分析,1990,10(4):25-28.ZHANG Jincai.Study on the separation and determination of microammounts of scandium in metallurgical products and vanadium titanium bearing magnetite by oscillopolarographic method[J].Metallurgical Analysis, 1990,10(4):25-28.
[8]
范健, 何捍卫,王国文.石墨炉原子吸收光谱法测定钛铁矿中钪[J].光谱实验室,1993,10(5):29-32.FAN Jian, HE Hanwei,WANG Guowen. Determination of scandium in ilmenite by graphite furnace atomic absorption spectrometry[J]. Chinese Journal of Spectroscopy Laboratory, 1993,10(5):29-32.
[9]
李龙泉,孙晔,淦五二,等.液膜富集原子吸收分光光度法测定痕量钪[J].化学研究与应用,1997,9(1):80-82.LI Longquan,SUN Ye,GAN Wuer, et al. Enrichment and determination of ation of scandium by liquid membrane and atomic absorption spectrometry[J]. Chemical Research and Application,1997,9(1):80-82.
[10]
梁术廷,薛章礼.铜铁试剂沉淀杂质ICP-AES测定地球化学样品中的稀土和钪[J].分析测试通报,1992,11(2):44-46.LIANG Shuting,XUE Zhangli.Determination of REEs and Sc in geochemical samples with ICP-AES using cupferron as precipitiant.[J]. Jouranl of Instrumental Analysis,1992,11(2):44-46.
[11]
郑大中.ICP-AES法测定复杂矿石中钪[J].四川化工,1996(2):22-29.ZHENG Dazhong.Determination of scandium in complex ores by ICP-AES[J].Sichuan Chemical Iudustry,1996(2):22-29.
[12]
杨金辉,杨江柳,胡鄂明,等.电感耦合等离子体发射光谱法(ICP-AES) 测定铀矿石中微量钪、硒、铼[J].南华大学学报(自然科学版),2002,18(4):83-85.YANG Jinhui,YANG Jiangliu,HU Eming,et,al.The determination of Sc,Se and Re in uranium ore with ICP-AES[J].Journal of Nanhua University (Science and Technology),2002,18(4):83-85.
[13]
尚正文,方秀丽,杨常青.电感耦合等离子体原子发射光谱法测定红土镍矿中钪量[J].理化检验(化学分册),2014,50(3):390-391.SHANG Zhengwen,FANG Xiuli,YANG Changqing.Determination of scandium in laterite nickel ore by inductively coupled plasma atomic emission spectrometry[J].Physical Testing and Chemical Analysis(Part B: Chemical Analysis),2014,50(3):390-391.
[14]
王树亮.酸溶共沉淀法 ICP-AES 测定地质样品中痕量钪[J].科技视界,2015(6):240-241.WANG Shuliang.Determination of trace scandium in geological samples by ICP-AES by acid-soluble coprecipitation[J]. Science and Technology Vision,2015(6):240-241.
