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A Pragmatic Approach to Coping with Matrix Effects during ICP-MS Analysis of Trace Elements in Silicate Rocks and Calibration of REE Interferences

机译:ICP-MS分析硅酸盐岩中痕量元素和REE干扰校正的一种实用方法

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Operating an Agilent 7700X ICP-MS spectrometer under robust plasma conditions (1550 W) with a He-filled octopole collision cell and analysing solutions (<2000 μg·g~(?1) total dissolved solids) still suffered analyte peak suppression due to matrix effects. International reference rocks BCR-1, BHVO-1, AGV-1, G-2 and BCR-2 all showed count rate reductions for 36 elements (mass range ~(7)Li to ~(238)U) averaging ~10% but with no dependence on isotope mass. Use of an internal standard (~(103)Rh) and/or using a ten-fold dilution of sample solutions reduced these effects but problems with reduced count rates combined with larger errors for some elements introduced other problems. The best approach was to normalise the count rates for each element in the other samples against those for BCR-1 as an external standard; thus the count suppression due to the matrix effect is corrected for each individual element. This approach provides standardization “traceability” in line with the ERM ISO/IEC requirement. Experiments are also reported on quantifying the proportions of Ba and selected REE oxide/hydroxide components versus parent isotopes (XO/X and XOH/X). This information is essential for correcting peak interferences on higher mass number REE for the rock samples, and equations are developed to use measured CeO/Ce and CeOH/Ce ratios to predict such values for any other member of the REE suite. Concentrations obtained show excellent agreement with recommended values for the international reference materials especially for the REE. Robust data are also provided for two other standard rocks: nepheline syenite STM-1 and quartz syenite CAAS-1; the latter shows exceptional enrichments of Zr, REE, Th, and U.
机译:在充满氦气的八极杆碰撞池的强大等离子体条件下(1550 W)下操作Agilent 7700X ICP-MS光谱仪并分析溶液(<2000μg·g〜(?1)总溶解固体)仍然会由于基质而受到分析物峰抑制效果。国际参考岩石BCR-1,BHVO-1,AGV-1,G-2和BCR-2均显示36种元素(质量范围〜(7)Li至〜(238)U)的计数率降低平均〜10%,但不依赖于同位素质量。使用内标(〜(103)Rh)和/或使用十倍稀释的样品溶液可减少这些影响,但计数率降低的问题以及某些元素的较大误差带来了其他问题。最好的方法是将其他样品中每个元素的计数率相对于BCR-1作为外标进行归一化;因此,针对每个单独的元素校正了由于矩阵效应引起的计数抑制。这种方法提供了符合ERM ISO / IEC要求的标准化“可追溯性”。还报道了量化Ba和所选REE氧化物/氢氧化物组分与母体同位素(XO / X和XOH / X)比例的实验。该信息对于校正岩石样品对更高质量数REE的峰干扰至关重要,因此开发了方程式以使用测得的CeO / Ce和CeOH / Ce之比来预测REE套件中任何其他成员的此类值。所获得的浓度与国际参考材料(尤其是稀土)的推荐值显示出极好的一致性。还提供了另外两种标准岩石的稳健数据:霞石正长岩STM-1和石英正长岩CAAS-1;后者显示Zr,REE,Th和U的异常富集。

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