熔融制样-X射线荧光光谱法测定轻稀土精矿中稀土总量

发布时间：2018-05-01 12:38

  本文选题：X射线荧光光谱法(XRF) + 熔融法　； 参考：《冶金分析》2017年12期

【摘要】：作为稀土工业的原料,稀土精矿中稀土总量的测定方法步骤多、流程长。实验采用熔融制样-X射线荧光光谱法测定轻稀土精矿中稀土总量,研究了制样和测量条件。准确称取6.000 0g无水四硼酸锂和偏硼酸锂混合熔剂(质量比2∶1)于铂黄坩埚中,以0.500 0g硝酸锂为氧化剂消除试样中还原物质对铂黄坩埚的侵蚀,称取0.600 0g稀土精矿试样,再于试样表面均匀覆盖0.500 0g氧化硼防止试样喷溅,滴加0.5mL 20mg/mL的溴化铵溶液作为脱模剂。将坩埚放进预加热到1 050℃的熔样机内熔融19min制备样片,可消除矿物效应、粒度效应及表面效应。通过各稀土元素X射线荧光谱线的选择减少谱线干扰,以经验系数法校正谱线干扰和基体效应,用稀土精矿标样建立各稀土元素校准曲线。各组分校准曲线的相关系数在0.991~0.999之间,试样重复测量的相对标准偏差(RSD)小于0.5%,稀土总量测定结果与重量法一致。方法的精密度和正确度能够满足生产要求。
[Abstract]:As the raw material of rare earth industry, there are many steps and long process to determine the total amount of rare earth in rare earth concentrate. The total amount of rare earth in light rare earth concentrate was determined by melting sample preparation-X-ray fluorescence spectrometry. The conditions of sample preparation and measurement were studied. The mixture flux of 6.000 g anhydrous lithium tetraborate and lithium metaborate (mass ratio 2: 1) was accurately used in the platinum yellow crucible, 0.500 g lithium nitrate was used as oxidant to eliminate the erosion of the reducing substance to the platinum yellow crucible in the sample, and the 0.600 g rare earth concentrate sample was used as the sample. Then 0.500 g boron oxide was uniformly covered on the surface of the sample to prevent the sample from spattering, and the ammonium bromide solution of 0.5mL 20mg/mL was added as the release agent. When the crucible is put into the melting prototype heated to 1 050 鈩，

本文编号：1829420