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酸溶-电感耦合等离子体质谱法测定钒钛磁铁矿中15种稀土元素

Determination of 15 rare earth elements in vanadium-titanium magnetite by acid dissolution-inductively coupled plasma mass spectrometry

  • 摘要: 准确测定钒钛磁铁矿中的稀土元素,可用于评估钒钛磁铁矿中稀土的资源潜力。实验以HNO3-HF-H2SO4体系敞口消解样品,在采样深度3 mm、射频功率1 350 W、雾化气流速1.05 L/min等的仪器优化条件下,以89Y、139La、140Ce、141Pr、146Nd、147Sm、151Eu、157Gd、159Tb、163Dy、165Ho、166Er、169Tm、172Yb、175Lu为待测同位素,采用干扰方程校正了157Gd、159Tb、165Ho、166Er、169Tm的多原子离子干扰,优化考虑了溶液中高含量Ti与Fe对稀土元素的干扰,建立了敞口酸溶-电感耦合等离子体质谱法(ICP-MS)测定钒钛磁铁矿中稀土元素的方法。在优化的实验条件下,各稀土元素校准曲线相关系数均不小于0.999 3,检出限为0.007~0.25μg/g,定量限在0.028~1.00μg/g。将实验方法应用于钒钛磁铁矿样品中稀土元素的测定,各元素测定结果的相对标准偏差(RSD,n=6)为0.85%~3.6%。实验发现河北省承德地区3个不同矿区中钒钛磁铁矿样品的稀土元素配分模式曲线相似,说明它们物源相似。

     

    Abstract: Accurate determination of rare earth elements(REEs) in vanadium-titanium magnetite is essential for evaluating the resource potential of REEs in such ores. Samples were digested using an open-vessel digestion method with an HNO3-HF-H2SO4 acid system. Instrumental conditions were optimized as follows: sampling depth of 3 mm, radio-frequency power of 1 350 W, and nebulizer gas flow rate of 1.05 L/min. The isotopes 89Y, 139La, 140Ce, 141Pr, 146Nd, 147Sm, 151Eu, 157Gd, 159Tb, 163Dy, 165Ho, 166Er, 169Tm, 172Yb, and 175Lu were selected for determination. Interference equations were applied to correct for polyatomic ion interference on 157Gd, 159Tb, 165Ho, 166Er, and 169Tm. The interference from high concentrations of Ti and Fe in the solution was also evaluated and compensated. A method for the determination of REEs in vanadium-titanium magnetite by open-vessel acid digestion-ICP-MS was established. Under the optimized conditions, the correlation coefficients of the calibration curves for all REEs were not less than 0.999 3. The limits of detection(LOD) ranged from 0.007 to 0.25 μg/g, and the limits of quantification(LOQ) were between 0.028 and 1.00 μg/g. The proposed method was applied to the determination of REEs in actual samples, yielding relative standard deviations(RSDs, n=6) of 0.85% to 3.6% for all elements. The similar REE distribution patterns observed for three vanadium-titanium magnetite samples from different mining areas in Chengde, Hebei Province, indicate they share a similar material source.

     

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