Ensuring the analysis accuracy by ICP-MS method using radioactive and highly-enriched stable isotope tracers and gamma-r
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Ensuring the analysis accuracy by ICP‑MS method using radioactive and highly‑enriched stable isotope tracers and gamma‑ray spectrometry Vasilii K. Karandashev1 · Vladimir P. Kolotov2 · Ilham I. Sadikov3 Received: 31 January 2020 © Akadémiai Kiadó, Budapest, Hungary 2020
Abstract To increase the accuracy of the analysis of silicon and rock samples by the inductively coupled plasma mass spectrometry, it is proposed to use both highly-enriched stable and short-lived radioactive isotopes with high specific radioactivity obtained in nuclear reactor to control the yield of elements on decomposition. Autoclave decomposition method for silicon and rock samples is proposed. Non-purified silicon sample irradiated in a nuclear reactor was used for testing of element recoveries during sample decomposition. Analysis of granite and black shale reference rock samples has been done using the suggested approach. Keywords Short-lived radionuclides · Stable highly-enriched isotopes · ICP-MS · Silicon and rocks samples
Introduction Inductively coupled plasma mass spectrometry (ICPMS) has become one of the leading methods of elemental analysis, widely used for analysis of various samples. For example, when determining rare-earth elements (REEs), the proportion of work carried out by various methods is as follows: inductively coupled plasma mass spectrometry (ICP-MS)-44%, inductively coupled plasma atomic emission spectrometry (ICP-AES)-21%, neuron activation analysis (NAA)-10%, luminescent analysis-10%, spectrophotometry-6%, X-ray fluorescence and other methods-9% [1]. The NAA has recently lost its leading position, which it held since the 70–80 s.
* Vasilii K. Karandashev [email protected] 1
Institute of Microelectronics Technology and High-Purity Materials of Russian Academy of Sciences, Osypyan str. 6, 142432 Chernogolovka, Russia
2
Vernadsky Institute of Geochemistry and Analytical Chemistry of Russian Academy of Sciences, Kosygin str. 19, 119991 Moscow, Russia
3
Institute of Nuclear Physics of the Academy of Sciences of the Republic of Uzbekistan, U.Gulamov 1, Tashkent, Uzbekistan 100214
ICP-MS method yields the most accurate results when applied to solutions of analysed samples; therefore, various chemical operations are used to decompose the latter. Apparently, it is the step that contributes most to the overall uncertainty of the ICP-MS analysis results. A number of processes take place during the sample preparatory step that seriously affect the analysis results. Among them are (a) incomplete dissolution of the analysed samples; (b) uncontrolled contamination from laboratory glassware, air, reagents, etc.; (c) uncontrolled losses due to spraying and volatilization when using heating, as well as incomplete transfer of solutions; (d) uncontrolled losses due to poor stability of element’s species in solutions, especially when diluted; (e) the formation of new sparingly soluble compounds at the dissolution step, etc. Concerning the problem of incomplete decomposition, the suitability of a particular method for ana
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