ICP-MS法测钪的干扰研究及选冶尾矿中钪的直接测定

发布时间：2018-05-25 19:16

本文选题：钪 + 测定　；参考：《光谱学与光谱分析》2017年04期

【摘要】：白云鄂博矿经选铁后,尾矿中钪含量可达0.05%,具有很高的开发利用价值。建立了一种操作简便、灵敏度高并能够准确测定尾矿及富铌渣中微量钪的电感耦合等离子体质谱(ICP-MS)测定方法。对仪器参数、试样处理方法、共存元素的干扰和消除方法进行了系统研究,选用铯、铊和铑作为内标元素,对非谱干扰加以校正。对质谱干扰研究表明,尾矿中的硼、硅、钙、锆和铝均可能对钪的测定造成质谱干扰,其中硼浓度较低(100μg·mL~(-1))时,对钪测定没有明显干扰,在测定条件下铝和钙的干扰较小,可以忽略。锆和硅的质谱干扰较严重,其中锆的干扰为双电荷(~(90)Zr~(++))干扰,由于双电荷离子电离产率一般不高,锆含量低时干扰可忽略,锆的含量较高时,采用公式c′=0.021c_((Zr))-0.55对结果加以校正。硅的干扰为氧化物干扰,而硅氧键解离能大,硅的氧化物(~(28)Si~(17)O~+,~(29)Si~(16)O~+)稳定性高,且相关同位素丰度较大,在测定条件下干扰较严重,可以采用式c″=0.013c(Si)+0.019扣除该影响。选择了四种不同的样品处理方式,结果表明采用HCl+HF+H_2SO_4混酸方法处理,标样测定结果与标准值一致,且能有效的克服硅和硼的质谱干扰,同时降低了测定液的含盐量,减小了非质谱干扰,标样回收率在97%~99%之间。标准样品及实际样品测定表明,采用ICP-MS法直接测定白云鄂博选冶尾矿中钪含量,结果准确,相对标准偏差小于5%,方法测定下限为0.000 1%。
[Abstract]:After iron separation in Baiyunebo Mine, the content of scandium in tailings can reach 0.05%, which has high value of exploitation and utilization. A simple, sensitive and accurate ICP-MS method for the determination of trace scandium in tailings and niobium rich slag has been developed. The instrument parameters, sample processing methods, interference and elimination methods of coexisting elements were systematically studied. Cesium, thallium and rhodium were selected as internal standard elements to correct non-spectral interference. The results of mass spectrometric interference show that boron, silicon, calcium, zirconium and aluminum in tailings may interfere with the determination of scandium by mass spectrometry. When the concentration of boron is lower than 100 渭 g / mL, there is no obvious interference with the determination of scandium, but the interference of aluminum and calcium is small under the conditions of determination. It is negligible. The interference between zirconium and silicon by mass spectrometry is serious, among which the interference of zirconium is the interference of double charge ion 90% zirconium. Because the ionization yield of double charge ion is generally not high, the interference can be neglected when the content of zirconium is low, and the interference is higher when the content of zirconium is high. The results were corrected by formula c'=0.021c_((Zr))-0.55. The interference of silicon is oxide interference, but the dissociation energy of silicon and oxygen bond is large. The oxide of silicon has high stability and relative isotopic abundance, and can be deducted by formula c "0.013 csi) 0.019. Four different sample treatment methods were selected. The results showed that the standard samples were treated with HCl HF H_2SO_4 mixed acid method, and the results were consistent with the standard values, and could effectively overcome the interference of silicon and boron mass spectrometry, and reduce the salt content of the determination solution. The non-mass interference was reduced and the standard sample recovery was between 97% and 99%. The measurement of standard sample and actual sample shows that the content of scandium in the tailings of Bayan Obo dressing and smelting is determined directly by ICP-MS method. The result is accurate, the relative standard deviation is less than 5, and the lower limit of determination is 0.000.
【作者单位】：北京科技大学化学系;包头稀土研究院;
【基金】：国家自然科学基金项目(21176027)资助
【分类号】：TD926.4;O657.63

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