摘要
由于目前的方法和标准无法直接测定高纯铈中的14种稀土杂质元素,要进行复杂的前处理工作,本文建立了三重串联电感耦合等离子体质谱法直接测定高纯铈中14种稀土杂质元素的方法。通过仪器参数的优化试验,最终选定No Gas模式测定钕、钐、铕、镝、钬、铒、铥和镱,氨气质量转移模式测定铽,氧气质量转移模式测定钇、镧、镨、钆和镥。测定时均以内标元素进行校正以减少基体效应、仪器的信号漂移和雾化进样等因素的影响。加入5 mL硝酸(1+1)和2 mL过氧化氢(30%)溶解试样,在试样中分别添加含0.2 mg/mL和1.0 mg/mL的其他14种稀土元素浓度进行加标回收试验。通过试验选择最佳的分析试液酸度、最佳的仪器参数、最佳的内标元素,最终选用5%的硝酸浓度作为分析试液的酸度并选用铊做内标元素。通过11次独立试验,得出样品加标回收率在90%~120%之间,各稀土元素的检出限在0.002 mg/mL~0.034 mg/mL之间,各稀土元素测定下限在0.013μg/g~0.224μg/g之间。对四个实际样品分别进行了11次独立试验,测得四个实际样品的相对标准偏差(RSD)分别在0.81%~5.40%之间。该方法准确可靠,操作简单,准确度和精密度均能满足分析的要求。
It is impossible to directly determine 14 kinds of impurities of rare earth in high purity cerium at present,so complex pretreatment work is needed.A method was developed for direct determination of fourteen different impurities in high purity cerium by ICP-MS/MS in this study.Through the optimization experiment of instrument parameters,neodymium,samarium,europium,dysprosium,holmium,erbium,thulium and ytterbium were determined by mass spectrometry with No Gas mode,terbium was determined by ammonia mass transfer mode and yttrium,lanthanum,praseodymium,gadolinium and lutetium were determined by oxygen mass transfer mode in this paper.Internal standard elements were used to correct the determination which can reduce the influence of matrix effect,the signal drift of instrument and atomization sampling.The matrix and the internal standard were used in this method,the sample was dissolved by nitric acid(1+1,5 mL)and hydrogen peroxide(30%,2 mL),adding other 14 kinds of rare earth ions with concentration of 0.2 mg/mL and 1.0 mg/mL respectively.The best acidity,the best instrument parameters and the best internal standard elements were selected through the experiment.Finally,5%nitric acid concentration was selected as the acidity of the analytical solution and the thallium was selected as the internal standard elements.After 11 independent measurements,the recovery of the standard addition is between 90%and 120%,and the detection limit of each element of 14 rare earth impurities was 0.002 mg/mL and 0.034 mg/mL,the lower limit of each element was between 0.013μg/g and 0.224μg/g.The relative standard deviations of the four samples were between 0.81%and 5.4%.The method is accurate,reliable,simple to operation,the accurate and precise can meet the requirements of analysis.
作者
肖石妹
徐娜
汤英
蒋威
凌细平
XIAO Shi-mei;XU Na;TANG Ying;JIANG Wei;LING Xi-ping(Jiangxi Center of Quality Supervision and Inspection for Tungsten and Rare Earth Products,Ganzhou 34X000,China;Jiangxi Institute of Tungsten and Rare Earth,Ganzhou 341000,China)
出处
《稀土》
EI
CAS
CSCD
北大核心
2021年第2期109-118,共10页
Chinese Rare Earths
基金
江西省市场监督管理局项目(G2J201508)。
关键词
三重串联电感耦合等离子体质谱
高纯铈
稀土杂质元素
干扰
基体
triple series inductively coupled plasma mass spectrometry(ICP-MS/MS)
high purity cerium
the impurity elements of rare earth
interference
matrix
