五酸溶样-电感耦合等离子体质谱法测定泥质岩中稀土等33种元素  

Determination of 33 elements including rare earths in mudstone by inductively coupled plasma mass spectrometry with five-acid sample digestion

作　　者：夏祥 陆海川 丁洋 龚仓 刘涛 廖炫哲 XIA Xiang;LU Haichuan;DING Yang;GONG Cang;LIU Tao;LIAO Xuanzhe(Civil-Military Integration Center China Geological Survey,Chengdu 610036,China;Key Laboratory of Natural Resource Coupling Process and Effects,Beijing 100055,China)

机构地区：[1]中国地质调查局军民融合地质调查中心,四川成都610036 [2]自然资源要素耦合过程与效应重点实验室,北京100055

出　　处：《冶金分析》2025年第2期25-33,共9页Metallurgical Analysis

基　　金：中国地质调查局地质调查项目(DD20243098);自然资源要素耦合过程与效应重点实验室开放课题(2023KFKTB011)。

摘　　要：准确测定泥质岩中包括稀土在内的微量元素含量,可用于评估泥质岩作为能源资源的潜力,服务于地质学研究及新一轮找矿突破战略行动。本文采用敞开酸溶法以硝酸-盐酸-氢氟酸-高氯酸-硫酸五酸体系对泥质岩样品进行处理,加入过氧化氢-王水混合溶液进行浸提,分别以Rh、Re为内标进行校正,建立了电感耦合等离子体质谱法(ICP-MS)同时测定泥质岩样品中稀土等33种元素(La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Sc、Y、Be、Mn、Co、Ni、Cu、Zn、Rb、Sr、Mo、Tl、Pb、Bi、Th、U、Ti、Nb、Ta)的方法。结果表明,33种元素校准曲线的线性相关系数均大于0.999 5,方法检出限为0.000 1~0.9μg/g,定量限为0.000 4~3.6μg/g。选择GBW07104和5个采自新疆鄯善吐哈盆地的泥质岩样品,按照实验方法测定稀土等33种元素,结果表明,各元素测定结果的相对标准偏差(RSD,n=12)在0.16%~9.9%之间,满足DZ/T 0011—2015规范中相对标准偏差RSD≤10%的要求。选取与泥质岩样品成分相似的岩石标准物质GBW07103、GBW07104,按照实验方法对稀土等33种元素进行测定,结果表明,各元素的测定值与认定值基本一致,对数差值(ΔlgC≤)在0.00~0.08之间,满足DZ/T 0011—2015中ΔlgC≤0.11的要求。称取两个泥质岩样品,按照实验方法进行测定,并分别向样品中加入一定量的混合标准溶液开展加标回收试验,结果表明,泥质岩样品中稀土等33种元素的加标回收率在92%~110%之间,符合《地质矿产实验室测试质量管理规范》(DZ/T 0130—2006)回收率为90%~110%的要求。Accurate determination of trace element contents,including rare earths,in mudstone can be used to assess its potential as an energy resource,serving geological research and the strategic action for a new round of mineral exploration breakthroughs.In this paper,the mudstone sample was treated using an open acid digestion method with a five-acid system of nitric acid,hydrochloric acid,hydrofluoric acid,perchloric acid,and sulfuric acid.A mixed solution of hydrogen peroxide and aqua regia was added for extraction.Rh and Re were used as internal standards for correction.The method for the determination of 33 elements in mudstone including rare earths(La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,Sc,Y,Be,Mn,Co,Ni,Cu,Zn,Rb,Sr,Mo,Tl,Pb,Bi,Th,U,Ti,Nb,and Ta)by inductively coupled plasma mass spectrometry(ICP-MS)was established.The results showed that the linear correlation coefficients of the calibration curves for 33 elements were all greater than 0.9995.The limits of detection and limits of quantification in this method were 0.0001-0.9μg/g and 0.0004-3.6μg/g,respectively.GBW07104 and five mudstone samples collected from the Turpan-Hami Basin in Shanshan,Xinjiang,were selected.The contents of 33 elements including rare earths were determined according to the experimental method.The results showed that the relative standard deviations(RSD,n=12)of the measurement results for each element ranged from 0.16%to 9.9%,which could meet the requirement of RSD≤10%specified in DZ/T 0011-2015.The certified reference materials of rock(GBW07103 and GBW07104)with similar compositions to the mudstone samples were selected.The contents of 33 elements including rare earths were determined according to the experimental method.The results showed that the measured values of each element were basically consistent with the certified values.The logarithmic differences(ΔlgC)ranged from 0.00 to 0.08,which could meet the requirement of ΔlgC≤0.11 specified in DZ/T 0011-2015.Two mudstone samples were measured according to the experimental method

关 键 词：泥质岩 稀土 硝酸-盐酸-氢氟酸-高氯酸-硫酸 五酸体系 敞开酸溶 电感耦合等离子体质谱法(ICP-MS) 

分 类 号：O657.63[理学—分析化学] P588.2[理学—化学]