电感耦合等离子体质谱法测定铀铌铅矿重选流程样品中铀

发布时间：2018-03-14 15:02

  本文选题：铀铌铅矿　切入点：铀　出处：《冶金分析》2017年05期 　论文类型：期刊论文

【摘要】：采用HCl、HNO_3、HF和HClO_4溶解铀铌铅矿,以电感耦合等离子体质谱法(ICPMS)测定了铀铌铅矿重选流程样品(原矿、精矿、中矿和尾矿)中铀(U)。通过选择合适的同位素238 U避免了质谱干扰,通过稀释基体质量浓度不大于0.30mg/mL和选择45ng/mL185 Re为内标相结合的方法消除了非质谱干扰。实验表明,在选定的实验条件下,U质谱强度与ρ(U)在5~60ng/mL范围内呈良好的线性关系,校准曲线相关系数r为0.999 2,方法检出限为0.000 4ng/mL。将实验方法应用于铀铌铅矿重选流程中的原矿、精矿、中矿和尾矿实际样品中U的测定,所得结果的相对标准偏差(RSD,n=6)为0.80%~3.9%,加标回收率为102%~106%。采用实验方法对铀铌铅矿重选流程样品(原矿、精矿、中矿和尾矿)中任意3个流程样品中的U含量进行测定,将其测定值代入质量守恒定律计算得到第4个流程样品中U含量的计算值,由实验方法对第4个流程样品中U含量的测定值与其计算值相比可计算得到第4个流程样品中U的回算率,实验表明,U的回算率为98%~106%。
[Abstract]:Using HClHNO3HF and HClO_4 to dissolve uranium niobium and lead ore, the uranium U U in uranium niobium lead ore gravimetric separation process samples (raw ore, concentrate, middle ore and tailings) was determined by inductively coupled plasma mass spectrometry (ICPMS). The interference of mass spectrometry was avoided by selecting suitable isotope 238U. The non-mass interference was eliminated by diluting the mass concentration of the matrix not more than 0.30 mg / mL and selecting 45ng / mL 185 re as the internal standard. The experimental results show that there is a good linear relationship between the mass mass intensity of U and 蟻 U in the range of 560 ng / mL under the selected experimental conditions. The calibration curve correlation coefficient r is 0.999 2, and the detection limit of the method is 0.000 4 ng / mL. The experimental method has been applied to the determination of U in the raw ore, concentrate, middle ore and tailings in the gravity separation process of uranium niobium and lead ore. The relative standard deviation (RSD) of the obtained results is 0.80 and 3.9.The recovery rate is 102and 106.The U content in any three flow samples (raw ore, concentrate, middle ore and tailings) of uranium niobium and lead ore gravimetric separation process samples is determined by experimental method. The calculated value of U content in the fourth flow sample is calculated by substituting the measured value with the law of conservation of mass. Compared with the calculated value, the back calculation rate of U in the fourth flow sample can be calculated by the experimental method. The experimental results show that the calculation rate of U in the fourth flow sample is 98% and 106%.
【作者单位】： 中国地质科学院郑州矿产综合利用研究所;国家非金属矿资源综合利用工程技术研究中心;国土资源部多金属矿评价与综合利用重点实验室;
【基金】：重要矿产和土地资源节约集约综合利用标准研究(项目编码:2016YFF0201604)
【分类号】：O657.63;TD922
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本文编号：1611720