{"title":"Application of MARS-5 and UltraWAVE Microwave Systems to the Digestion of Silicate Rocks Followed by ICP-MS Analysis","authors":"I. V. Nikolaeva, S. V. Palesskiy","doi":"10.1134/s0020168524700031","DOIUrl":null,"url":null,"abstract":"<h3 data-test=\"abstract-sub-heading\">Abstract</h3><p>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, HNO<sub>3</sub>, and HCl in MARS-5 (<i>T</i> = 190°C, <i>P</i> = 20 bar) and UltraWAVE (<i>T</i> = 240°C, <i>P</i> = 80 bar) with the distillation of excess fluorides in the form of SiF<sub>4</sub> 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.</p>","PeriodicalId":585,"journal":{"name":"Inorganic Materials","volume":null,"pages":null},"PeriodicalIF":0.9000,"publicationDate":"2024-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Inorganic Materials","FirstCategoryId":"88","ListUrlMain":"https://doi.org/10.1134/s0020168524700031","RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"MATERIALS SCIENCE, MULTIDISCIPLINARY","Score":null,"Total":0}
引用次数: 0
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.
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.
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