过氧化钠碱熔-电感耦合等离子体质谱法测定地质样品中锆铌铪钽和稀土元素  

Determination of zirconium,niobium,hafnium,tantalum and rare earth elements in geological sample by inductively coupled plasma mass spectrometry with sodium peroxide alkali fusion

作　　者：孙孟华 朱永晓 赵烨 陈庆芝 宋凡 孙凯茜 SUN Menghua;ZHU Yongxiao;ZHAO Ye;CHEN Qingzhi;SONG Fan;SUN Kaixi(Hebei Research Center for Geoanalysis,Baoding 071051,China;Hebei Provincial Key Laboratory of Mineral Resources and Ecological Environment Monitoring,Baoding 071051,China)

机构地区：[1]河北省地质实验测试中心,河北保定071051 [2]河北省矿产资源与生态环境监测重点实验室,河北保定071051

出　　处：《冶金分析》2024年第9期35-44,共10页Metallurgical Analysis

基　　金：保定市科技计划项目(2241ZF350)。

摘　　要：地质样品中Zr、Nb、Hf、Ta和稀土元素的测定,对于开发利用稀土矿资源和研究地球化学、岩石成因等地质环境具有重要意义。采用Na_(2)O_(2)于750℃熔融8 min,沸水提取,过滤后用HCl-H_(2)O_(2)混合液分次溶解氢氧化物沉淀,选用He碰撞池模式和干扰校正方程克服轻稀土元素氧化物或氢氧化物对重稀土元素的干扰,以Rh校正Zr、Nb、Sc、Y、La、Ce、Pr、Nd、Sm,Re校正Hf、Ta、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu,建立了电感耦合等离子体质谱法(ICP-MS)同时测定地质样品中Zr、Nb、Hf、Ta和稀土元素的方法。在优化的实验条件下,20种元素校准曲线的线性相关系数均不小于0.9992,检出限在0.03~2.69μg/g之间,定量限在0.09~8.07μg/g之间。按照实验方法对水系沉积物和岩石标准物质中Zr、Nb、Hf、Ta和稀土元素进行测定,测定值与认定值的相对误差(RE)均不大于6.7%,满足行业标准DZ/T 0130—2006的相对误差允许限要求;相对标准偏差(RSD,n=12)均不大于4.8%。将实验方法应用于土壤、水系沉积物、岩石样品中Zr、Nb、Hf、Ta和稀土元素的测定,各元素测定结果的相对标准偏差(n=6)为0.5%~4.8%。The determination of Zr,Nb,Hf,Ta,and rare earth elements in geological samples has important significance for exploration and utilization of rare earth mineral resources as well as the geological environment researches such as geochemistry and petrogenesis.The sample was melted with Na_(2)O_(2)at 750℃for 8 min followed by leaching with boiling water.After filtration,the hydroxide precipitates were dissolved with HCl-H_(2)O_(2)mixed solution in stages.The interferences of oxides or hydroxides of light rare earth elements with heavy rare earth elements were overcome by selecting He collision cell mode and interference correction equation.Rh was used to correct Zr,Nb,Sc,Y,La,Ce,Pr,Nd and Sm,and Re was used to correct Hf,Ta,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb and Lu.Consequently,a method for simultaneous determination of Zr,Nb,Hf,Ta and rare earth elements in geological sample was established by inductively coupled plasma mass spectrometry(ICP-MS).Under the optimized experimental conditions,the linear correlation coefficients of calibration curves of 20 elements were all not less than 0.9992.The limits of detection were in range of 0.03-2.69μg/g,and the limits of quantitation were in range of 0.09-8.07μg/g.The contents of Zr,Nb,Hf,Ta and rare earth elements in certified reference materials of stream sediment and rock were determined according to the proposed method,and the relative errors(RE)between the results and certified values were all not more than 6.7%,which could meet the allowable limit requirements of relative error in industry standard of DZ/T 0130-2006.The relative standard deviations(RSD,n=12)were all not more than 4.8%.The proposed method was applied for determination of Zr,Nb,Hf,Ta and rare earth elements in soil,stream sediment and rock samples,and the RSDs(n=6)of determination results were between 0.5%and 4.8%.

关 键 词：过氧化钠 碱熔 电感耦合等离子体质谱法(ICP-MS) 地质样品 锆 铌 铪 钽 稀土元素 

分 类 号：O657.63[理学—分析化学] TF031[理学—化学]