首页|微敞开体系消解-电感耦合等离子体质谱法测定地球化学样品中稀土元素

微敞开体系消解-电感耦合等离子体质谱法测定地球化学样品中稀土元素

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稀土是地质勘查工作和新一轮找矿突破战略行动关注的重点,准确测定地球化学样品中稀土元素含量至关重要.本文基于聚四氟乙烯消解管,采用电热石墨消解仪以硝酸-氢氟酸-高氯酸-硫酸体系消解样品,实现了微敞开体系消解-电感耦合等离子体质谱法(ICP-MS)对地球化学样品中稀土元素的测定.实验表明,在微敞开环境下,控制硝酸-氢氟酸-高氯酸-硫酸体系用量为8 mL,选择最高消解温度240 ℃下保持2.5 h(总消解时间4.5 h)即可将样品消解完全.校准曲线的线性相关系数均大于0.999,方法检出限为0.001~0.03 μg/g,定量限为0.004~0.12 μg/g;实验方法中各稀土元素的方法检出限大部分低于标准方法DZ/T 0279.32-2016和GB/T 14506.30-2010.按照实验方法对水系沉积物、土壤、岩石标准物质中的稀土元素进行测定,结果表明,各元素测定值与认定值的对数差值(Δlg(C))为0.00~0.03,相对标准偏差(RSD,n=6)在0.74%~7.2%之间,分别满足DZ/T 0011-2015所规定的Δlg(C)≤0.11和RSD≤10%的要求.选择岩石和土壤标准物质,分别采用实验方法与封闭酸溶-ICP-MS对样品中稀土元素进行测定,两种方法的测定值基本一致.本方法酸用量少,样品消解时间短,可用于地球化学样品中稀土元素的批量测试.
Determination of rare earth elements in geochemical samples by inductively coupled plasma mass spectrometry after digestion in micro-open system
Rare earths are a key focus of geological exploration work and a new round of strategic explora-tion breakthroughs.The accurate determination of contents of rare earth elements in geochemical samples is very important.In this study,the sample was digested with nitric acid-hydrofluoric acid-perchloric acid-sulfuric acid system using an electric graphite digestion device equipped with polytetrafluoroethylene diges-tion tube.The determination of rare earth elements in geochemical samples by inductively coupled plasma mass spectrometry(ICP-MS)after digestion in micro-open system was realized.The results showed that the sample could be fully digested in micro-open system under the following conditions:the dosage of nitric acid-hydrofluoric acid-perchloric acid-sulfuric acid system was 8 mL;the highest digestion temperature was 240 ℃,which was kept for 2.5 h(total digestion time of 4.5 h).The linear correlation coefficients of cali-bration curves were all greater than 0.999.The limits of detection of this method were 0.001-0.03 μg/g,and the limits of quantification were 0.004-0.12 μg/g.The limits of detection for most rare earths in ex-periments were lower than those obtained by standard method DZ/T 0279.32-2016 and GB/T 14506.30-2010.The contents of rare earths in certified reference materials of stream sediment,soil and rock were determined according to the experimental method.The results showed that the logarithmic difference(Δlg(C))between the measurement values and certified values of elements was 0.00-0.03,and the relative standard deviations(RSD,n=6)were between 0.74%and 7.2%,which could meet the requirements ofΔlg(C)≤0.11 and RSD≤10%specified in DZ/T 0011-2015.The rare earth elements in certified reference materials of rock and soil were determined according to the experimental method and ICP-MS after acid dis-solution in closed system.The measurement results of two methods were basically consistent.The acid consumption in this method was low and the sample digestion time was short.It could be used for the batch test of rare earth elements in geochemical samples.

rapid digestion in micro-open systeminductively coupled plasma mass spectrometry(ICP-MS)geochemical samplesrare earth element

陆海川、袁新、夏祥、贾炳超、刘涛、龚仓

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中国地质调查局军民融合地质调查中心,四川成都 610036

微敞开快速消解 电感耦合等离子体质谱法(ICP-MS) 地球化学样品 稀土元素

中国地质调查局"拉萨河流域自然资源综合调查"项目

DD20220866

2024

冶金分析
中国钢研科技集团有限公司(钢铁研究总院) 中国金属学会

冶金分析

CSTPCD北大核心
影响因子:1.124
ISSN:1000-7571
年,卷(期):2024.44(2)
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