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熊英, 吴峥, 董亚妮, 裴若会, 刘晓艳, 吴赫, 张艳. 封闭消解-阳离子交换分离-电感耦合等离子体质谱法测定铜铅锌矿石中的铼[J]. 岩矿测试, 2015, 34(6): 623-628. DOI: 10.15898/j.cnki.11-2131/td.2015.06.004
引用本文: 熊英, 吴峥, 董亚妮, 裴若会, 刘晓艳, 吴赫, 张艳. 封闭消解-阳离子交换分离-电感耦合等离子体质谱法测定铜铅锌矿石中的铼[J]. 岩矿测试, 2015, 34(6): 623-628. DOI: 10.15898/j.cnki.11-2131/td.2015.06.004
Ying XIONG, Zheng WU, Ya-ni DONG, Ruo-hui PEI, Xiao-Yan LIU, He WU, Yan ZHANG. Determination of Rhenium in Copper-Lead-Zinc Ore by Inductively Coupled Plasma-Mass Spectrometry with Closed Decomposition and Cation Exchange Separation[J]. Rock and Mineral Analysis, 2015, 34(6): 623-628. DOI: 10.15898/j.cnki.11-2131/td.2015.06.004
Citation: Ying XIONG, Zheng WU, Ya-ni DONG, Ruo-hui PEI, Xiao-Yan LIU, He WU, Yan ZHANG. Determination of Rhenium in Copper-Lead-Zinc Ore by Inductively Coupled Plasma-Mass Spectrometry with Closed Decomposition and Cation Exchange Separation[J]. Rock and Mineral Analysis, 2015, 34(6): 623-628. DOI: 10.15898/j.cnki.11-2131/td.2015.06.004

封闭消解-阳离子交换分离-电感耦合等离子体质谱法测定铜铅锌矿石中的铼

Determination of Rhenium in Copper-Lead-Zinc Ore by Inductively Coupled Plasma-Mass Spectrometry with Closed Decomposition and Cation Exchange Separation

  • 摘要: 阴离子交换树脂已被应用于酸法消解-电感耦合等离子体质谱(ICP-MS)测定铜铅锌矿石等地质样品中铼的分离富集, 样品溶液中的ReO4-用树脂交换吸附后再用洗脱剂将ReO4-选择性洗脱, 该方法流程长, 影响其稳定性和准确性。本文以基体元素为吸附交换目标, 用8 g的732强酸型阳离子交换树脂在2%硝酸介质条件下静态吸附1.5 h, 可有效地消除基体元素的影响。用空矿(石英)稀释低含量铼的样品做空白试验, 获得方法检出限为0.004μg/g, 精密度(RSD)小于6%, 加标回收率为96%~104%。本方法应用的732强酸型阳离子交换树脂在适宜酸度条件下, 对矿石中除钨、钼以外的金属元素吸附率高达95%以上, 降低了样品溶液离子强度和干扰元素浓度, 实现了ICP-MS的直接测定, 操作方法比阴离子交换吸附法简便。

     

    Abstract: Anion exchange resin has been applied to Re separation after acid digestion of Cu-Pb-Zn ores and Re was determined by Inductively Coupled Plasma-Mass Spectrometry(ICP-MS). ReO4- in solution was adsorbed by exchange resin and was then eluted from the resin by eluant. This method has a long process, which affects its stability and accuracy. Matrix elements are selected as the goal and 8 g of 732 cation exchange resin in 2% nitric acid medium for 1.5 h static adsorption is used. This method can effectively eliminate the influence of matrix elements on the ICP-MS determination of rhenium. Quartz was used as the blank and mixed with low Re samples. The acquired detection limit was 0.004μg/g, the precision(RSD) is less than 6%, and the recovery ranged from 96% to 104%. The 732 cation exchange resin under the acidic condition has the recovery of >95% for most matrix elements except tungsten and molybdenum, which reduced ionic strength and the concentration of interference elements. Rhenium can be directly determined by ICP-MS, which is simpler and faster than the anion exchange resin separation method.

     

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