电感耦合等离子体质谱法测定高纯稀土及其氧化物中钪  

Determination of scandium in high purity rare earths and their oxides by inductively coupled plasma mass spectrometry

作　　者：范小龙 包香春[1,2] FAN Xiaolong;BAO Xiangchun(State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization of Baotou Research Institute of Rare Earths,Baotou 014030,China;Ruike National Engineering Research Center of Rare Earth Metallurgy and Function Materials,Baotou 014030,China)

机构地区：[1]包头稀土研究院白云鄂博稀土资源研究与综合利用国家重点实验室,内蒙古包头014030 [2]瑞科稀土冶金及功能材料国家工程研究中心,内蒙古包头014030

出　　处：《冶金分析》2023年第9期14-20,共7页Metallurgical Analysis

摘　　要：随着高纯稀土金属及其氧化物在工业生产中的应用日益广泛,对其纯度要求逐渐提高,准确测定高纯稀土金属及其氧化物中钪的含量十分必要。采用10mL硝酸并加入3~5滴过氧化氢溶解样品,以2%(V/V)硝酸为测定介质,以铯为内标,建立了电感耦合等离子体质谱法(ICP-MS)测定高纯稀土金属及其氧化物中钪含量的方法。从轻、中、重稀土中分别选择高纯氧化钇、高纯氧化镧、高纯氧化镨、高纯氧化铕、高纯氧化钬和高纯氧化镱配制其质量浓度依次为0.20、0.50、0.70、1.00mg/mL的基体溶液,加入钪标准溶液使氧化钪质量浓度均为10.00ng/mL,考察了这几种基体质量浓度在0.20~1.00mg/mL范围内与钪信号强度之间的关系。结果表明,钪的信号强度与基体浓度之间存在良好的线性关系,线性相关系数均不小于0.97,说明在此时基体效应可忽略。考察了不同基体浓度下内标元素铯、铑与钪信号强度的变化情况,结果表明铯信号强度的降低程度与钪基本一致,实验选择10.00ng/mL铯作为内标校正钪的含量。实验表明,钪质量浓度在1.00~100.00ng/mL范围内,校准曲线的相关系数大于0.9995,方法检出限为0.045μg/g,定量限为0.15μg/g。将实验方法应用于高纯镧、高纯氧化镧、高纯氧化铕和高纯氧化镱样品中钪(高纯稀土氧化物的结果以氧化钪计)的测定,测定结果的相对标准偏差(RSD,n=11)为6.2%~7.9%。采用实验方法对高纯镧、高纯钐、高纯镱以及高纯氧化钇、高纯氧化镧、高纯氧化镨、高纯氧化铕、高纯氧化钬和高纯氧化镱样品中钪进行分析,加标回收率为96%~104%,测定结果与标准加入法基本一致。With the extensive application of high purity rare earths and their oxides in industrial production,the requirements for their purity are increased gradually.Therefore,it is necessary to accurately determine the content of scandium in high purities rare earths and their oxides.After the sample was dissolved with 10mL of HNO3and 3-5drops of H_(2)O_(2),a determination method of scandium in high purity rare earths and their oxides by inductively coupled plasma mass spectrometry(ICP-MS)was established with 133Cs as the internal standard and 2%(V/V)HNO3as the determination medium.High purity yttrium oxide,high purity lanthanum oxide,high purity praseodymium oxide,high purity europium oxide,high purity holmium oxide and high purity ytterbium oxide were selected from the light,medium and heavy rare earths to prepare the matrix solutions with matrix mass concentrations of 0.20,0.50,0.70and 1.00mg/mL,respectively,and scandium standard solution was added to make sure that the mass concentrations of scandium oxide were all at 10.00ng/mL.The relationship between these matrix mass concentrations in the range of 0.20-1.00mg/mL and the signal intensity of scandium was investigated.The results showed that there was a good linear relationship between the signal intensity of scandium and matrix concentration with linear correlation coefficients all not less than 0.97,indicating that the matrix effects were negligible.The changes in signal intensity of internal standard of cesium and rhodium with scandium were investigated at different matrix concentrations.The results showed that the reduction degree of cesium signal intensity was basically the same as that of scandium,so 10.00ng/mL of cesium was selected as the internal standard to correct the content of scandium.The results showed that when the mass concentration of scandium was in the range of 1.00-100.00ng/mL,the correlation coefficient of calibration curve was greater than 0.9995,the detection limit of this method was 0.045μg/g,the limit of quantification was 0.15μg/g.The p

关 键 词：高纯稀土金属 高纯稀土氧化物 钪 电感耦合等离子体质谱法(ICP-MS) 高纯氧化钇 高纯氧化镧 高纯氧化镨 高纯氧化铕 高纯氧化钬 高纯氧化镱 

分 类 号：O657.63[理学—分析化学] TG146.45[理学—化学]