Determination of Trace Rhenium in Sandstone-type Uranium Deposits by Inductively Coupled Plasma-Mass Spectrometry with Magnesium Oxide Sintering
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摘要: 砂岩型铀矿中铀的平均含量为635 μg/g，而铼的含量仅为0.3～1.9 μg/g，由于铼的含量低，准确测定高含量铀矿样中的低含量铼仍是分析化学的一个难题。本文建立了电感耦合等离子体质谱法测定砂岩型铀矿中痕量铼的方法。样品经过氧化镁烧结，热水浸提以及采用103Rh作内标元素等方式消除了铀、钼及其他基体元素对测定铼的干扰。在最佳条件下，痕量铼的检出限可低至0.12 ng/g，回收率达99.8%。本方法通过多种标准样品验证，铼的测定值与标准值吻合，对铼含量在0.06～180.57 μg/g范围内的实际样品进行测定，相对标准偏差均小于1.5%，能够满足砂岩型铀矿等高含量铀矿中痕量铼的测定需求。
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关键词:
- 砂岩型铀矿 /
- 铼 /
- 烧结法 /
- 电感耦合等离子体质谱法
Abstract: The average content of uranium in sandstone-type uranium deposits is 635 μg/g, whereas the content of rhenium is 0.3-1.9 μg/g. Because of low rhenium content, now precise determination of low Re in high U ores remains unresolved. In this study, a method for the determination of trace Re in sandstone-type uranium deposits by Inductively Coupled Plasma-Mass Spectrometry was developed. Samples were digested by MgO sintering, and were then extracted by hot water. 103Rh was used as the internal standard element to eliminate the interferences of uranium, molybdenum and other matrix elements on Re. Under optimum conditions, the detection limit of trace rhenium is 0.12 ng/g, and the recovery is 99.8%. The method was validated by a variety of standard samples, the measured Re contents are in good agreement with the standard values. The relative standard deviation (RSD) is less than 1.5% for Re contents of 0.06-180.57 μg/g, which meets the requirement of determining trace Re in high U ores from sandstone type uranium deposits. -
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表 1 ICP-MS测定铼的线性范围与计数值
Table 1. The linear range of ICP-MS determination and count value of rhenium
铼标准工作溶液浓度(ng/mL) 186Re计数值 相对标准偏差(RSD，%) 0.002 43.6 8.7 0.02 469.4 2.7 0.2 4785.3 0.9 2 48282.3 0.4 20 491440.1 1.1 200 5234455.2 1.4 
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表 2 标准物质中铼含量的测定结果
Table 2. Determination results of rhenium in the standard samples
标准物质编号 铼含量的测定值(μg/g) 铼含量的标准值(μg/g) 相对误差(%) GBW07238 0.34 0.35 -2.86 GBW07239 0.13 0.12 8.33
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表 3 矿样中铼含量的测定结果
Table 3. Determination results of rhenium in actual ore samples
样品编号 铼含量5次测量的平均值(μg/g) RSD(%) 1 180.57 1.3 2 11.78 0.6 3 36.26 0.5 4 48.63 0.4 5 0.06 0.4 6 0.09 0.4 7 17.14 0.9 8 20.95 0.9
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