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建立了熔融制样-X射线荧光光谱法测定氟碳铈矿中镧、铈、镨、钕、钐、钇、铕、钆等八种稀土元素,硅、铝、钙、铁等造岩元素以及磷、钡、锶、氟等伴生矿物元素的分析方法。基于各待测稀土元素地壳丰度及常见的伴生矿物组合,通过人工混合稀土氧化物与国家标准物质的方式建立校准曲线。选择熔融制样作为样品前处理手段,通过观察实验现象、分析待测元素响应,优化熔样温度、脱模剂种类等实验参数。研究了F在熔融制样过程中的损失规律,通过实验结果确定了对其定量分析的基础。确定取样量0.5000 g,混合熔剂四硼酸锂/偏硼酸锂(质量比为67∶33)用量8.0000 g,熔样温度1100℃,预熔时间300 s,熔样时间300 s,静置时间30 s,540 s时补充脱模剂,脱模剂选择NH4I。应用所建方法处理稀土矿石与铈富集物样品,与传统方法结果对照吻合,具备线性范围宽、迅速准确等优点。
In this paper, eight kinds of rare earth elements, such as lanthanum, cerium, praseodymium, neodymium, samarium, yttrium, europium and gadolinium, as well as rock-forming elements such as silicon, aluminum, calcium and iron in bastnaesite were established by the method of X-ray fluorescence spectrometry Phosphorus, barium, strontium, fluorine and other associated mineral elements analysis. Based on the crustal abundance of rare earth elements to be tested and the common associated mineral assemblages, a calibration curve was established by artificially mixing rare earth oxides with national standards. Select the melting sample preparation as a sample pre-treatment means, by observing the experimental phenomena, analyze the response of the elements to be tested, optimize the melting temperature, mold release agent type and other experimental parameters. The loss regularity of F in the process of melt sample preparation was studied. The basis of the quantitative analysis was confirmed by the experimental results. The sample volume was 0.5000 g, the amount of mixed solvent lithium tetraborate / lithium metaborate (mass ratio 67:33) was 8.0000 g, the sample temperature was 1100 ℃, the pre-melting time was 300 s, the melting time was 300 s, and the standing time was 30 s 540 sec when added release agent, release agent NH4I. Application of the proposed method of processing rare earth ore and cerium enrichment samples, and the traditional method of control consistent with the results, with a wide linear range, rapid and accurate.