Determination of trace rhenium in molybdenite concentrate by matrix separation-inductively coupled plasma atomic emission spectrometry
WANG Jingfeng1,2,3,4
1. Technology Development of Western Mining Group Co.,Ltd.,Xining 810006,China; 2. The Engineering and Technology Research of Qinghai Western Mining Co.,Ltd.,Xining 810006,China; 3. Qinghai Key Laboratory Plateau Comprehensive Utilization and Mineral Processing Engineering,Xining 810006,China; 4. Qinghai Nonferrous Mineral Resources Engineering Technology Research Center,Xining 810006,China
Abstract:During the determination of rhenium in molybdenite concentrate by inductively coupled plasma atomic emission spectrometry(ICP-AES), molybdenum has serious spectral interference due to its abundant spectral lines. In order to eliminate the interference of matrix molybdenum with the determination of rhenium, the sample was dissolved with 30 mL of nitric acid, 1 mL of ammonium bifluoride and 40 mL of hydrogen peroxide in experiments. The matrix molybdenum was oxidized to molybdenum trioxide precipitate for filtration. Re 197.312 nm was selected as the analytical line for rhenium. The method for the determination of trace rhenium in molybdenite concentrate by ICP-AES after matrix separation was established. The results showed that the linear correlation coefficient (r) of calibration curve was 0.999 99. The limit of detection was 0.000 2%. The content of rhenium in molybdenite concentrate sample was determined according to the experimental method, and the relative standard deviations (RSD, n=6) of measurement results were between 5.6% and 6.0%. The content of rhenium in certified reference material (GBW07144) and sample of molybdenite concentrate was determined according to the experimental method and spectrophotometry in YS/T 555.10-2009. The found results of two methods were consistent.
[1] 马红周,王耀宁,兰新哲.树脂富集钼精矿焙烧烟尘浸出液中铼的研究[J].西安建筑科技大学学报(自然科学版),2005,37(4):584-586. MA Hongzhou,WANG Yaoning,LAN Xinzhe.Study on the sorption of rhenium from the leaching solution of the fume of calcinating molybdenite concentrated ore by anion exchange resin[J].Journal of Xi′an University of Architecture & Technology(Natural Science Edition),2005,37(4):584-586. [2] 中华人民共和国工业和信息化部.YS/T 555.10—2009 钼精矿化学分析方法 铼量的测定 硫氰酸盐分光光度法[S].北京:中国标准出版社,2010. [3] Karadjovm,Velitchkovan,Velevao,et al.Spectral interferences in the determination of rhenium in molybdenum and copper concentrates by inductively coupled plasma optical emission spectrometry(ICP-OES)[J].Spectrochimica Acta Part B:Atomic Spectroscopy,2016,119:76-82. [4] 程秀花,黎卫亮.电感耦合等离子体质谱法测定钼矿石和钼精矿中铼[J].冶金分析,2013,33(1):54-58. CHENG Xiuhua,LI Weiliang.Determination of rhenium in molybdenum ores and molybdenum concentrate by inductively coupled plasma mass spectrometry [J].Metallurgical Analysis,2013,33(1):54-58. [5] 周长祥,王卿,姜怀坤,等.泡沫塑料预富集中子活化测定铜矿中的铼[J].分析化学,2005,33(5):657-660. ZHOU Changxiang,WANG Qing,JIANG Huaikun,e al.Determination of rhenium in copper ores by preconcentration of polyurethane foam-neutron activation analysis[J].Chinese Journal of Analytical Chemistry,2005,33(5):657-660. [6] 王景凤,宋学文,曹雨薇.电感耦合等离子体原子发射光谱法测定氧化镁和氢氧化镁中10种痕量元素[J].理化检验(化学分册),2021,57(6):526-532. WANG Jingfeng,SONG Xuewen,CAO Yuwei.Determination of 10 trace elements in magnesium oxide and magnesium hydroxide by inductively coupled plasma atomic emission spectrometry[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2021,57(6):526-532. [7] 杨红玉,喻生洁,田卫,等.电感耦合等离子体原子发射光谱法测定三氯化铑中11种杂质元素[J].冶金分析,2021,41(10):76-82. YANG Hongyu,YU Shengjie,TIAN Wei,et al.Determination of 11 impurity element in rhodium trichloride by inductively coupled plasma atomic emission spcetrometry[J].Metallurgical Analysis,2021,41(10):76-82. [8] 张育诚,王津.电感耦合等离子体原子发射光谱法测定氧化钼中镧和钇[J].冶金分析,2022,42(2):27-32. ZHANG Yucheng,WANG Jin.Determination of lanthanum and yttrium in molybdenum oxide by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2022,42(2):27-32. [9] 王小龙,陆翌欣,杜效,等.基体分离-电感耦合等离子体原子发射光谱法测定高纯钼中9种元素[J].冶金分析,2020,40(6):43-48. WANG Xiaolong,LU Yixin,DU Xiao,et al.Determination of nine elements in high purity molybdenum by matrix separation-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2020,40(6):43-48. [10] 吴敏,王景凤,王茂盛,等.利用电感耦合等离子体发射光谱测定镍矿石中铂钯含量的方法:中国,ZL 2018 10919864.4[P].2021-02-05. [11] 刘锦锐,加明.电感耦合等离子体原子发射光谱法测定光致发光材料钼酸钙中19种微量杂质元素[J].冶金分析,2021,41(8):76-83. LIU Jinrui,JIA Ming.Determination of nineteen trace impurities in photoluminescent material of calcium molybdate by inductively coupled plasma atomic emission spectrometry[J].Metallurgcial Analysis,2021,41(8):76-83. [12] 颜燕.两种干扰校正方式下电感耦合等离子体原子发射光谱法测定钼铝合金中硅的方法比较[J].冶金分析,2022,42(3):52-58. YAN Yan.Comparison of inductively coupled plasma atomic emission spectrometry for determination of silicon in molybdenum-aluminum alloy with two interference correction methods[J].Metallurgcial Analysis,2022,42(3):52-58.