X射线荧光光谱法在线测定稀土冶炼分离过程中钬铒铥镱  

On-line determination of holmium,erbium,thulium and ytterbium in rare earth smelting separation process by X-ray fluorescence spectrometry

作　　者：梁元[1] 沈学静[1,2] 易启辉 刘明博 屈华阳 胡学强 

机构地区：[1]钢铁研究总院,北京100081 [2]钢研纳克检测技术有限公司,北京100094 [3]广晟有色金属集团有限公司,广东广州510501

出　　处：《冶金分析》2016年第8期1-6,共6页Metallurgical Analysis

基　　金：基金项目:稀土冶炼分离先进工艺标准化示范

摘　　要：我国稀土冶炼分离过程复杂,但多数稀土企业仍依靠实验室离线分析指导工艺,导致分析结果严重滞后,因此现迫切需要一种高效稳定的稀土在线分析方法。实验应用稀土配分在线分析仪,建立了一种在线测定稀土冶炼分离过程中Ho、Er、Tm、Yb配分含量的方法。将采样管置于串级萃取槽水相分隔室内,在蠕动泵作用下将样品输送至分析区域,通过X射线荧光光谱法(XRF)进行检测和数据记录。实验将XRF测试条件优化为电压40kV、电流600μA、测试时间60s,模拟现场工况条件下优化蠕动泵泵速为250r/min,并采用基本参数法消除元素间吸收增强效应。样品11次测定结果的相对标准偏差(RSD)小于0.4%,实验室模拟及现场在线测试结果与电感耦合等离子体原子发射光谱法(ICP-AES)的离线分析结果吻合较好,测试结果滞后时间短,完全能够满足稀土冶炼分离过程工艺动态控制的测定需要。The smelting separation process of rare earths in China is complicated. However, most rare earth enterprises still depend on laboratory off-line analysis to guide the process, leading to serious lagging of analytical results. Therefore, it is necessary to develop a high-efficiency and stable on-line analysis method for rare earths. In this paper, a kind of on-line determination method of holmium, erbium, thulium and ytterbium content in rare earth smelting separation process was established using rare earth distribution pattern on-line analyzer. The sampling tube was located in aqueous phase compartment of cascade-stage extraction tank. The sample was transported to the analysis area by peristaltic pump for X-ray fluorescence spectrometry （XRF） analysis and data record. The XRF testing conditions were optimized： the voltage was 40 kV, the current was 600 μA, and the testing time was 60 s. The in-site conditions were simulated and the optimal peristaltic pump speed was 250 r/min. The absorption enhancement effect among elements was eliminated by fundamental parameter method. The relative standard deviation （RSD, n=11） was less than 0.4%. The laboratory simulation and in-site on-line measurement results were in good agreement with the off-line analytical results by inductively coupled plasma atomic emission spectrometry （ICP- AES）. The lagging time of measurement results was short, which could meet the determination require-ments of dynamic control in rare earth smelting separation process.

关 键 词：X射线荧光光谱法(XRF) 钦 铒 铥 镱 基本参数法 在线分析 稀土冶炼分离 

分 类 号：TF845[冶金工程—有色金属冶金] O657.34[理学—分析化学]