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电感耦合等离子体质谱法测定钒钛磁铁矿中的稀土元素

刘淑君 雷勇 赵朝辉 易建春 王洪彬

刘淑君, 雷勇, 赵朝辉, 易建春, 王洪彬. 电感耦合等离子体质谱法测定钒钛磁铁矿中的稀土元素[J]. 钢铁钒钛, 2024, 45(3): 200-204. doi: 10.7513/j.issn.1004-7638.2024.03.028
引用本文: 刘淑君, 雷勇, 赵朝辉, 易建春, 王洪彬. 电感耦合等离子体质谱法测定钒钛磁铁矿中的稀土元素[J]. 钢铁钒钛, 2024, 45(3): 200-204. doi: 10.7513/j.issn.1004-7638.2024.03.028
Liu Shujun, Lei Yong, Zhao Chaohui, Yi Jianchun, Wang Hongbin. Determination of rare earth elements in vanadium-titanium magnetite by ICP-MS[J]. IRON STEEL VANADIUM TITANIUM, 2024, 45(3): 200-204. doi: 10.7513/j.issn.1004-7638.2024.03.028
Citation: Liu Shujun, Lei Yong, Zhao Chaohui, Yi Jianchun, Wang Hongbin. Determination of rare earth elements in vanadium-titanium magnetite by ICP-MS[J]. IRON STEEL VANADIUM TITANIUM, 2024, 45(3): 200-204. doi: 10.7513/j.issn.1004-7638.2024.03.028

电感耦合等离子体质谱法测定钒钛磁铁矿中的稀土元素

doi: 10.7513/j.issn.1004-7638.2024.03.028
基金项目: 国家自然科学基金战略性矿产资源开发利用专项(典型战略金属氧化矿强化浮选分离过程的多尺度化学原理与调控,编号:2021YFC2900800);中国地质调查项目(金属矿产资源节约与综合利用调查,编号:DD20230039)。
详细信息
    作者简介:

    刘淑君,1984年出生,女,湖南永州人,硕士,工程师,主要从事岩矿分析测试方法研究,E-mail:382120656@qq.com

  • 中图分类号: O657.31,TF041

Determination of rare earth elements in vanadium-titanium magnetite by ICP-MS

  • 摘要: 准确、快速地测定钒钛磁铁矿中的稀土元素,对钒钛磁铁矿的高效利用有着重要的作用。针对目前国内外缺乏钒钛磁铁矿中稀土元素分析方法的问题,试验选取不同矿区具有代表性的5件钒钛磁铁矿作为试验样品,采用盐酸、氢氟酸、硝酸外加硫酸混合酸溶分解的方式,并结合电感耦合等离子体质谱仪检出限低、灵敏度高、干扰小的特点,对钒钛磁铁矿中稀土元素测定过程中的仪器条件、测定模式、内标元素、同位素选择及质谱干扰进行研究。结果表明,在最佳的仪器工作参数的条件下,采用STD模式,选择干扰小且丰度大的同位素,选择合适的内标元素Rh和Re,能够有效地降低基体效应引起的信号强度漂移。此外,通过精密度试验及加标回收试验发现,采用电感耦合等离子体质谱法测定钒钛磁铁矿中的稀土元素能获得良好的精密度与准确度,此方法准确有效。
  • 表  1  电感耦合等离子体质谱仪工作条件

    Table  1.   Inductively coupled plasma mass spectrometer operating conditions

    射频功
    率/W
    雾化器流量/
    (L·min−1)
    冷却气流量/
    (L·min−1)
    辅助气流量/
    (L·min−1)
    采样深
    度/步
    (采样锥/截取
    锥)/mm
    扫描
    方式
    测量
    点/峰
    重复测
    定次数
    停留时间/
    (ms·点−1)
    扫描
    次数
    测量时
    间/s
    1400 1.0 16 1.2 88 1.1/0.7 跳峰 3 3 10 40 60
    下载: 导出CSV

    表  2  分析同位素、内标及干扰校正

    Table  2.   Analysis of isotopes, internal standards and interference correction

    分析元素内标潜在干扰
    89Y103Rh
    139La185Re
    140Ce185Re
    141Pr185Re
    143Nd185Re
    147Sm185ReGd,CeO, BaO
    153Eu185ReBaO
    158Gd185RePrO,NdO,CeO
    159Tb185RePrO,NdO,
    163Dy185ReSmO,NdO
    165Ho185ReSmO
    166Er185ReSmO,NdO
    169Tm185ReEuO
    172Yb185ReDy,SmO,NdO
    175Lu185Re
    下载: 导出CSV

    表  3  方法精密度(RSD)

    Table  3.   Method precision (RSD)

    元素RSD/%
    A1A2A3A4A5
    La2O33.332.513.073.633.03
    CeO21.621.801.691.681.64
    Pr6O116.845.956.197.445.86
    Nd2O32.872.433.203.192.78
    Sm2O36.556.306.226.715.59
    Eu2O35.507.735.864.566.55
    Gd2O35.106.454.544.285.08
    Tb4O76.485.236.316.845.83
    Dy2O36.445.956.646.976.42
    Ho2O33.193.113.082.703.48
    Er2O33.463.673.793.303.55
    Tm2O33.473.603.503.343.61
    Yb2O33.153.262.822.923.11
    Lu2O33.455.394.143.874.53
    Y2O32.282.002.302.142.24
    下载: 导出CSV

    表  4  加标回收率

    Table  4.   Recovery rate of spikes

    元素 回收率/%
    A1 A2 A3 A4 A5
    La2O3 98.35 101.2 97.25 104.56 96.25
    CeO2 102.14 98.15 97.36 103.87 94.57
    Pr6O11 97.38 96.57 102.36 96.74 103.56
    Nd2O3 104.20 103.74 97.58 105.20 95.41
    Sm2O3 102.56 98.97 94.34 104.57 97.37
    Eu2O3 98.51 95.68 96.87 105.67 103.26
    Gd2O3 97.32 94.57 103.25 96.35 105.46
    Tb4O7 104.56 102.69 106.89 97.56 95.48
    Dy2O3 103.86 105.86 98.87 95.42 106.54
    Ho2O3 106.57 107.25 103.25 95.62 104.35
    Er2O3 96.54 98.56 102.87 104.85 103.57
    Tm2O3 104.58 106.25 93.57 96.12 107.25
    Yb2O3 105.65 102.11 97.22 96.15 95.37
    Lu2O3 106.78 104.37 95.87 94.53 103.57
    Y2O3 98.25 95.61 103.58 105.41 97.45
    下载: 导出CSV
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  • 收稿日期:  2023-10-10
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