首页|微波消解-电感耦合等离子体质谱法测定铁精矿中稀土元素分量和总量

微波消解-电感耦合等离子体质谱法测定铁精矿中稀土元素分量和总量

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准确测定铁精矿中稀土元素分量和总量对铁精矿的综合利用具有重要意义.采用6 mol/L HC1微波消解铁精矿样品,以甲基异丁基甲酮萃取基体中的铁(Ⅲ)以克服基体效应,以50 ng/mL Re作为内标进行校正,采用电感耦合等离子体质谱(ICP-MS)标准模式测定溶液中稀土元素分量和总量,实现了对铁精矿中稀土元素分量和总量的测定.考察了基体效应对测定的影响,结果表明,对样品进行微波消解处理后直接用ICP-MS进行测定,各稀土元素测得结果的回收率为6%~31%,说明此时基体效应对测定的影响不可忽略;对样品进行微波消解后,先以甲基异丁基甲酮萃取法除去铁基体后再用ICP-MS进行测定,各稀土元素的回收率在96%~103%之间,故实验在消解样品后,先采用甲基异丁基甲酮萃取步骤实现铁基体与待测元素的分离后再进行测定.于最优的实验条件下,在5~100 ng/mL范围内,各稀土元素与其对应的质谱信号强度具有较好的线性关系,校准曲线相关系数r为0.999 2~0.999 9,方法检出限为0.000 1~0.060 5 ng/mL.将所建立的方法用于铁精矿中稀土元素分量和总量的测定,结果的相对标准偏差(RSD,n=6)为2.3%~4.2%,稀土元素分量和总量的加标回收率为92%~108%,满足地质矿产行业标准DZ/T 0130-2006对加标回收率的要求.
Determination of total amount of rare earth elements and its component in iron concentrate by inductively coupled plasma mass spectrometry with microwave digestion
The accurate determination of total amount of rare earth elements and its component in iron con-centrate is of great significance for the comprehensive utilization of iron concentrate.In this study,the iron concentrate sample was dissolved by microwave digestion with 6 mol/L HC1.Iron(Ⅲ)in matrix was ex-tracted with methyl isobutyl ketone to overcome the matrix effect.The internal standard correction was conducted with 50 ng/mL Re.The total amount of rare earth elements and its component in solution were determined by inductively coupled plasma mass spectrometry(ICP-MS)using standard mode.The deter-mination of total amount of rare earth elements and its component in iron concentrate was realized.The in-fluence of matrix effect on the determination was investigated.The results showed that the recoveries of rare earth elements were between 6%and 31%if the sample was directly determined by ICP-MS after mi-crowave digestion,implying that the influence of matrix effect on the determination could not be ignored.After microwave digestion,the iron matrix was removed by methyl isobutyl ketone extraction.Then the solution was determined by ICP-MS,and the recoveries of rare earth elements were between 96%and 103%.Therefore,before determination,the methyl isobutyl ketone extraction was adopted after digesting the sample to separate the iron matrix from testing elements.Under the optimal experimental conditions,the mass concentration of rare earth elements in range of 5-100 ng/mL showed a good linear relationship with the corresponding MS signal intensity.The correlation coefficients(r)of calibration curves were be-tween 0.999 2 and 0.999 9.The limits of detection of method were between 0.000 1 ng/mL and 0.060 5 ng/mL.The proposed method was applied for the determination of total amount of rare earth elements and its component in iron concentrate.The relative standard deviations(RSD,n=6)of determination results were between 2.3%and 4.2%.The spiked recoveries of total amount of rare earth elements and its com-ponent were between 92%and 108%,which could meet the analysis requirements on spiked recovery in national geological and mineral industry standard DZ/T 0130-2006.

iron concentratemicrowave digestionrare earth elementsinductively coupled plasma mass spectrometry(ICP-MS)

姚明星、郭晓瑞、毛香菊、王甜甜、倪文山

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中国地质科学院郑州矿产综合利用研究所,河南郑州 450006

国家非金属矿资源综合利用工程技术研究中心,河南郑州 450006

自然资源部多金属矿评价与综合利用重点实验室,河南郑州 450006

铁精矿 微波消解 稀土元素 电感耦合等离子体质谱法(ICP-MS)

国家自然科学基金

22106148

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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