四酸消解-电感耦合等离子体质谱法测定砂岩型铀矿中铀钍及稀土元素  

Determination of uranium,thorium and rare earth elements in sandstone type uranium deposits by four-acid digestion-inductively coupled plasma mass spectrometry

作　　者：梁亚丽 吴领军 杨珍 孙银生 阿丽莉 贺攀红 LIANG Yali;WU Lingjun;YANG Zhen;SUN Yinsheng;A Lili;HE Panhong(Henan Nuclear Technology Application Center,Zhengzhou 450044,China;Henan Province Engineering Technology Research Center of Nuclear and Radiation Emergency Technology,Zhengzhou 450044,China)

机构地区：[1]河南省核技术应用中心,河南郑州450044 [2]河南省核与辐射应急技术工程技术研究中心,河南郑州450044

出　　处：《冶金分析》2025年第1期68-75,共8页Metallurgical Analysis

基　　金：国防科技工业局项目(JSJL2020201A003)。

摘　　要：为提高砂岩型铀矿资源勘查和综合利用效率,需准确测定砂岩型铀矿中的铀、钍及稀土元素含量。本法用硝酸-高氯酸-氢氟酸-盐酸密闭微压体系消解样品,以盐酸进行提取,选择4.5 mL/min氦气动能歧视碰撞池模式(KED)测定稀土元素,标准测量模式测定铀、钍,建立了电感耦合等离子体质谱法(ICP-MS)测定砂岩型铀矿中铀、钍及稀土元素等18种元素的方法。以45Sc、89Y、139La、140Ce、141Pr、146Nd、147Sm、159Tb、163Dy、166Er、172Yb、175Lu、238U、232Th为待测同位素,同时以151Eu、157Gd为待测同位素结合数学干扰校正方程进行校正克服了质谱干扰;轻稀土元素La、Ce、Pr、Nd、Sm、Eu选择Rh为内标,重稀土元素Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu及U、Th、Y、Sc选择Re为内标校正分析信号的偏移。在选定的实验条件下,各元素校准曲线的相关系数均不小于0.999 7,检出限在0.002~0.096μg/g之间,定量限在0.008~0.384μg/g之间。按照实验方法分别对砂岩铀矿成分分析标准物质和实际样品进行测定,结果表明,标准物质测定结果的相对标准偏差(RSD,n=7)在0.02%~2.8%之间;样品测定结果的RSD在1.1%~3.3%之间,加标回收率在94%~106%之间,符合国家地质矿产行业标准DZ/T 0130.3—2006《地质矿产实验室测试质量管理规范》中回收率90%~110%的要求。In order to enhance the resource prospection and comprehensive utilization efficiency of sandstone type uranium deposits,the content of uranium,thorium and rare earth elements should be accurately determined.In this study,the sample was digested by nitric acid-perchloric acid-hydrofluoric acid-hydrochloric acid in a closed system followed by extraction with hydrochloric acid.The rare earth elements were determined in kinetic energy discriminating(KED) collision cell mode with helium flow of 4.5 mL/min.The content of uranium and thorium was determined at standard measurement mode.The method for the determination of 18 elements in sandstone type uranium deposite,including uranium,thorium,and rare earth elements,by inductively coupled plasma mass spectrometry(ICP-MS) was established.45Sc,89Y,139La,140Ce,141Pr,146Nd,147Sm,159Tb,163Dy,166Er,172Yb,175Lu,238U and 232Th were isotopes to be measured.Meanwhile,the mass spectrometry interference was overcome by correction based on mathematical interference correction equation and using 151Eu and 157Gd as isotopes to be measured.Rh was selected as the internal standard for the light rare earth elements such as La,Ce,Pr,Nd,Sm and Eu.Re was selected as the internal standard for the heavy rare earth elements including Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,U,Th,Y and Sc to correct the shift of analytical signals.Under the selected experimental conditions,the correlation coefficients of calibration curves of elements were not less than 0.999 7,the limits of detection ranged from 0.002 to 0.096 μg/g,and the limits of quantification ranged from 0.008 to 0.384 μg/g. The certified reference materials and samples of sandstone type uranium deposite were determined according to the experimental method.The results showed that the relative standard deviations(RSD,n=7) of the measurement results of certified reference materials were between 0.02% and 2.8%.The RSDs of actual samples were between 1.1% and 3.3%,and the recoveries were between 94% and 106%,which could meet the recovery requirements of 90%

关 键 词：四酸消解 电感耦合等离子体质谱法(ICP-MS) 砂岩型铀矿 铀 钍 稀土元素 

分 类 号：O657.63[理学—分析化学] TF041[理学—化学]