Application of MARS-5 and UltraWAVE Microwave Systems to the Digestion of Silicate Rocks Followed by ICP-MS Analysis

IF 0.9 4区材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Inorganic Materials Pub Date : 2024-07-19 DOI:10.1134/s0020168524700031

I. V. Nikolaeva, S. V. Palesskiy

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Abstract

Two microwave systems MARS-5 and UltraWAVE are compared in the efficiency with regard to the digestion of silicate rocks with subsequent determination of 32 elements (Sc, V, Cr, Co, Ni, Cu, Zn, Rb, Sr, Y, Nb, Ta, Cs, Ba, 14 REEs, Hf, Ta, Th, U) by inductively coupled plasma mass spectrometry (ICP-MS). The development of digestion methods and validation of the obtained results have been carried out using international reference materials—basalts BHVO-2 and BCR-2, serpentinite UB-N, and peridotite JP-1. Microwave digestion included a two-stage treatment of samples with a mixture of concentrated acids HF, HNO₃, and HCl in MARS-5 (T = 190°C, P = 20 bar) and UltraWAVE (T = 240°C, P = 80 bar) with the distillation of excess fluorides in the form of SiF₄ between microwave digestion stages. The determination of concentrations in the obtained solutions was carried out on an ELEMENT high-resolution mass spectrometer in low and medium resolution according to external calibration with the internal standard (In), taking into account the acid composition of the analyzed solutions. The detection limits of the analytes after acid digestion in MARS-5 and UltraWAVE are comparable and provide the determination of all specified elements, except for Ta in JP-1. The use of the developed sample preparation procedure in MARS-5 ensures the complete decomposition of BHVO-2, BCR-2, and UB-N followed by ICP-MS determination of 32 specified elements in the obtained solutions without additional preconcentration steps. The relative standard deviations for the determined elements are 2–9% for the reference materials BHVO-2 and BCR-2 and 3–12% for UB-N with an increase to 16–25% (Nb, Ta) due to the approach to the detection limit. The more efficient microwave digestion in UltraWAVE compared to MARS-5 was proved by the complete decomposition of JP-1 with the transfer of all the elements, including Cr, into the solution.

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应用 MARS-5 和 UltraWAVE 微波系统消化硅酸盐岩并进行 ICP-MS 分析

摘要通过电感耦合等离子体质谱法（ICP-MS），比较了 MARS-5 和 UltraWAVE 两种微波系统对硅酸盐岩进行消解并随后测定 32 种元素（Sc、V、Cr、Co、Ni、Cu、Zn、Rb、Sr、Y、Nb、Ta、Cs、Ba、14 种 REEs、Hf、Ta、Th、U）的效率。消解方法的开发和所获结果的验证是利用国际参考材料--玄武岩 BHVO-2 和 BCR-2、蛇纹岩 UB-N 和橄榄岩 JP-1 进行的。微波消解包括在 MARS-5（T = 190°C，P = 20 巴）和 UltraWAVE（T = 240°C，P = 80 巴）中用浓酸 HF、HNO3 和 HCl 混合物对样品进行两阶段处理，并在微波消解阶段之间以 SiF4 的形式蒸馏多余的氟化物。在 ELEMENT 高分辨率质谱仪上，根据内标（In）的外部校准，并考虑到分析溶液的酸性成分，对所得溶液中的浓度进行中低分辨率测定。在 MARS-5 和 UltraWAVE 中进行酸消解后，被分析物的检测限相当，可测定所有指定元素，但 JP-1 中的 Ta 除外。在 MARS-5 中使用所开发的样品制备程序可确保 BHVO-2、BCR-2 和 UB-N 完全分解，然后用 ICP-MS 测定所得溶液中的 32 种特定元素，而无需额外的预浓缩步骤。所测定元素的相对标准偏差在参考材料 BHVO-2 和 BCR-2 中为 2-9%，在 UB-N 中为 3-12%，由于接近检测极限，增加到 16-25%（Nb、Ta）。与 MARS-5 相比，UltraWAVE 的微波消解效率更高，JP-1 完全分解，包括铬在内的所有元素都转移到了溶液中。

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来源期刊

Inorganic Materials 工程技术-材料科学：综合

CiteScore

1.40

自引率

25.00%

发文量

审稿时长

3-6 weeks

期刊介绍： Inorganic Materials is a journal that publishes reviews and original articles devoted to chemistry, physics, and applications of various inorganic materials including high-purity substances and materials. The journal discusses phase equilibria, including P–T–X diagrams, and the fundamentals of inorganic materials science, which determines preparatory conditions for compounds of various compositions with specified deviations from stoichiometry. Inorganic Materials is a multidisciplinary journal covering all classes of inorganic materials. The journal welcomes manuscripts from all countries in the English or Russian language.