泡沫塑料吸附分离富集-电感耦合等离子体质谱法测定稀土矿石中的镓

采用电感耦合等离子体质谱法(ICP-MS)测定稀土矿石中的镓,高含量的稀土元素会造成严重的质谱干扰。本文采用聚氨酯泡沫塑料在6 mol/L盐酸介质中吸附样品溶液中的镓后,以0.5 mol/L氯化铵水浴加热解脱30 min,镓的吸附-解脱效率超过99%,稀土元素等干扰物质基本不进入解脱液中,即在富集镓的同时实现了镓与基体元素的高效分离,降低了质谱干扰。本方法检出限低(0.022μg/g),经土壤及水系沉积物标准物质验证,镓的测定值与标准值吻合(绝对偏差为0.38%~4.70%),实际稀土矿石样品的加标回收率为94.1%~100.6%,精密度(RSD)低于4%(n=12),可应用于分析一般地质样品...

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Bibliographic Details
Published in岩矿测试 Vol. 35; no. 1; pp. 42 - 47
Main Author 董学林 何海洋
Format Journal Article
LanguageChinese
Published 湖北省地质实验测试中心,湖北 武汉,430034 2016
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ISSN0254-5357
DOI10.15898/j.cnki.11-2131/td.2016.01.008

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Summary:采用电感耦合等离子体质谱法(ICP-MS)测定稀土矿石中的镓,高含量的稀土元素会造成严重的质谱干扰。本文采用聚氨酯泡沫塑料在6 mol/L盐酸介质中吸附样品溶液中的镓后,以0.5 mol/L氯化铵水浴加热解脱30 min,镓的吸附-解脱效率超过99%,稀土元素等干扰物质基本不进入解脱液中,即在富集镓的同时实现了镓与基体元素的高效分离,降低了质谱干扰。本方法检出限低(0.022μg/g),经土壤及水系沉积物标准物质验证,镓的测定值与标准值吻合(绝对偏差为0.38%~4.70%),实际稀土矿石样品的加标回收率为94.1%~100.6%,精密度(RSD)低于4%(n=12),可应用于分析一般地质样品以及稀土矿石中的镓。
Bibliography:11-2131/TD
rare earth ore; gallium; polyurethane foam; separation and preconcentration; Inductively Coupled Plasma-Mass Spectrometry
Gallium in rare earth ore is commonly determined by Inductively Coupled Plasma-Mass Spectrometry( ICP-MS),but high content of rare earth will result in significant mass spectrum interferences. In this study,Ga in sample solution was absorbed by polyurethane foam in 6 mol / L HCl. Gallium adsorbed on the foam could be quantitatively eluted with 0. 5 mol / L NH4 Cl solution in a heating water bath for 30 min. The adsorption-eluted efficiency is higher than 99%. Most of the matrix elements could be separated from Ga by polyurethane foam so the mass spectrum interferences were reduced effectively. The detection limit was 0. 022 μg / g. The accuracy of the developed method was evaluated by analyzing Ga in soil and stream sediment standard reference materials. The proposed method was successfully applied to gallium determination in geological samples and rare earth ores. The recoveries
ISSN:0254-5357
DOI:10.15898/j.cnki.11-2131/td.2016.01.008