摘要
采用硫酸铵溶液提取离子型稀土原矿试样中离子相稀土,以硫酸铵溶液为基体配制校准系列溶液,建立了电感耦合等离子体质谱法(ICP-MS)测定样品溶液中离子相稀土总量及分量的方法。实验表明:对于10.00g离子型稀土矿试样,加入100mL 50g/L硫酸铵溶液振荡15min后放置30min可有效提取出离子相稀土;采用5.0g/L硫酸铵溶液进行校准系列溶液的基体匹配,选择103 Rh-185 Re双内标可有效校正硫酸铵的基体效应及仪器信号的漂移影响;选择合适的同位素消除了可能存在的质谱干扰。在最佳条件下进行测定,15个稀土元素的校准曲线在10.0~100.0μg/L范围内线性相关系数均大于0.999 91,方法检出限在0.10~0.66μg/g之间。方法应用于不同离子型稀土矿区中离子相稀土总量及分量的测定,结果与电感耦合等离子体原子发射光谱法(ICP-AES)一致,相对标准偏差(RSD,n=11)在1.0%~5.2%之间,回收率在98%~104%之间。
The ionic-phase rare earth in raw ores of ion-adsorption rare earth was extracted by ammonium sulfate and the calibration solution series were prepared with ammonium sulfate solution as matrix.Thus,a method for the determination of total ionic-phase rare earth and component in the sample solution was established by inductively coupled plasma mass spectrometry(ICP-MS).It showed that ionic-phase rare earth could be effectively extracted from 10.00 g of ion-adsorption rare earth ore samples which had been concussed for 15 min with 100 mL of 50g/L ammonium sulfate solution added and kept still for 30min;5.0g/L ammonium sulfate solution was used for matrix matching of calibration solution series,while 103 Rh-185 Re double inner standard method was used to calibrate the matrix effect of ammonium sulfate and the signal shift effect of instrument;the possible mass spectral interference was eliminated with appropriate isotopes.Under optimal conditions,the linear correlation coefficient of the calibration curve of fifteen rare earth elements within 10.0-100.0μg/L were all larger than 0.999 91.The detection limit was 0.10-0.66μg/g.When the method was employed to determine total ionic-phase rare earth and component in different ion-adsorption rare earth ore zones,the results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry(ICPAES).The relative standard deviation(RSD,n=11)was in the range of 1.0%-5.2%,and the recovery was between 98%and 104%.
出处
《冶金分析》
CAS
CSCD
北大核心
2014年第9期14-19,共6页
Metallurgical Analysis
基金
国家自然科学基金(41363003)
广西科学研究与技术开发计划项目(桂科能14123006-12)
