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    微波消解-电感耦合等离子体质谱法测定深海沉积物中稀土总量

    Determination of Total Content of Rare Earths in Deep-Sea Sediments by Inductively Coupled Plasma Mass Spectrometry after Microwave Digestion

    • 摘要: 建立了微波消解-电感耦合等离子体质谱法(ICP-MS)测定深海沉积物中稀土总量的方法。将深海沉积物湿样烘干、压碎,剔除杂质,过筛后再次烘干。称取0.20 g样品于微波消解罐中,加入5.0 mL硝酸和2.0 mL氢氟酸,在程序升温条件下进行微波消解,结束后加入3.0 mL高氯酸进行赶酸,再加入50%(体积分数)硝酸溶液加热溶解样品中的盐类。冷却后,用水定容至50 mL。分取5.0 mL,用2%(体积分数)硝酸溶液定容至50 mL,在线加入10 μg·L-1铟内标溶液,按照优化的ICP-MS工作条件测定稀土氧化物含量。结果显示:15种稀土氧化物的质量浓度在一定范围内和其与内标元素铟响应值的比值呈线性关系,相关系数均为0.999 9,检出限(3s)为0.006 2~0.060 0 μg·g-1。对3种深海沉积物样品进行精密度、加标回收及方法比对试验,结果显示:所得测定值的相对标准偏差(n=11)为1.1%~2.9%,回收率为96.0%~104%,方法和国家标准方法GB/T 17417.1-2010所得的测定值基本一致。

       

      Abstract: A method for the determination of total content of rare earths in deep-sea sediments by inductively coupled plasma mass spectrometry (ICP-MS) after microwave digestion was established. The wet samples of deep-sea sediments were dried, crushed and removed impurities, and then dried again after sieving. The sample (0.20 g) was taken and added into the microwave digestion tank, 5.0 mL nitric acid and 2.0 mL hydrofluoric acid were added for microwave digestion under temperature programmed condition. Perchloric acid (3.0 mL) was added to remove acid, and 50% (volume fraction) nitric acid solution was added and heated to dissolve the salt in the sample. After cooling, the solution was diluted by water and its volume was made up to 50 mL. An aliquot of 5.0 mL solution was taken and diluted to 50 mL with 2% (volume fraction) nitric acid solution. 10 μg·L-1 indium internal standard solution was added online, and the contents of rare earth oxides were determined under the optimized ICP-MS working conditions. The results showed that mass concentrations of 15 rare earth oxides were linearly related with the ratios of the response values of rare earth oxides to indium internal standard element in definite ranges, with the same correlation coefficient of 0.999 9 and detection limits (3s) in the range of 0.006 2-0.060 0 μg·g-1. Tests for precision, spiked recovery and method comparison were made, giving results of RSDs (n=11) of the determined values in the range of 1.1%-2.9% and recovery in the range of 96.0%-104%, and the determined values were consistent with those obtained by the national standard method GB/T 17417.1-2010.

       

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