基体稀释法控制RE_(x)O_(y)中REO及REX/REO标准样品的制备技术  

Preparation Technique for Reference Samples of REO and REX/REO in RE_(x)O_(y) Controlled by Matrix Dilution Method

作　　者：李华昌 王东杰 汤淑芳 王安丽 王振江[3] 王选 Li Huachang;Wang Dongjie;Tang Shufang;Wang Anli;Wang Zhenjiang;Wang Xuan(BGRIMM MTC Technology Stock Co.,Ltd.,Beijing 102600,China;BGRIMM Technology Group,Beijing 102600,China;Physical and Chemical Testing Center,Baotou Rare Earth Research Institute,Baotou 014030,China)

机构地区：[1]北矿检测技术股份有限公司,北京106200 [2]矿冶科技集团有限公司,北京106200 [3]包头稀土研究院理化检测中心,内蒙古包头014030

出　　处：《稀有金属》2024年第3期448-456,共9页Chinese Journal of Rare Metals

基　　金：国家重点研发计划项目(2021YFC2903101)资助。

摘　　要：利用基体稀释的方法,实现稀土氧化物中稀土总量(REO)及稀土配分量(REX/REO)的成分含量控制,使其满足与碳酸稀土和氯化稀土等产品REO成分一致的标准样品候选物要求。通过对稀释剂材料的理论分析和相关试验研究,选择NaCl晶体作为掺杂基体,稀释由La_(2)O_(3),CeO_(2),Pr_(6)O_(11)和Nd_(2)O_(3)等单一稀土氧化物组成的混合物,再通过研磨、混料,制备成满足定值要求的标准样品候选物((LaCe)_(x)O_(y))和(PrNd)_(x)O_(y))。以混合稀土氧化物标准样品(GSB 04-3064-2013)的粒度和扫描电镜(SEM)数据作为参考,研究了标准样品候选物的均匀性和稳定性,有效控制了候选物的REO和REX/REO与自主设计的标准值一致,对比分析了稀土氧化物标准样品和基体掺杂标准样品候选物的粒度和SEM图像,表征了候选物的均匀性和稳定性,形成了RE_(x)O_(y)中REO及REX/REO成分标准样品制备方法,所制备的(LaCe)_(x)O_(y)和(PrNd)_(x)O_(y)中REO分别为38.80%和29.58%。该制备方法适用于同类标准样品的研制,对控制成分标准样品的研制有参考意义。With the development of science and technology,investigators had more stringent requirements for rare earth standard sample preparation methods.This article investigated a method for the preparation of rare earth standard samples using diluents to control the standard values of total rare earths,and the preparation of rare earth standard samples with standard values for total rare earths(REO).Diluents selectedwere stable and did not react chemically with the candidate materials,the candidate materials were designed for composition according to the proportional requirements of the actual product;they were then batched,mixed and ground,and NaCl was added according to the configuration of the designed REO values;and the final standard values representing the properties of the standard samples were obtained.The content of said REO standard values ranged from 28%to 42%.This standard sample preparation method enabled quality control and instrument calibration for the testing process of rare earth products such as carbonated rare earths and chlorinated rare earths,mainly as an evaluation and calibration of the standard methods for the determination of REO by weight and inductively coupled plasma emission spectrometer(ICP-OES)methods.To meet the problem that products such as carbonate and chloride rare earths were inherently unstable and could not be directly prepared as standard samples,the research into the use of matrix doping techniques was performed to achieve a controlled component content of REO and rare earth fractions(REX/REO)in rare earth oxides.NaCl crystals were selected as the doping matrix and a mixture consisting of single rare earth oxides such as La_(2)O_(3),CeO_(2),Pr_(6)O_(11)and Nd_(2)O_(3) was diluted to prepare a standard sample candidate.The homogeneity and stability of the standard sample candidates were investigated by using the particle size and scanning electron microscope(SEM)data of the mixed rare earth oxide standard sample(GSB 04-3064-2013)as a reference,and effectively controlled REO and R

关 键 词：稀土氧化物 稀土总量(REO) 基体稀释 标准样品 制备技术 

分 类 号：X751[环境科学与工程—环境工程]