Hyphenated techniques in speciation analysis of polyoxometalates: identification of individual [PMo12-xVxO40]-3-x (x = 1-3) in the reaction mixtures by high performance liquid chromatography and atomic emission spectrometry with inductively coupled plasma

O V Shuvaeva; A A Zhdanov; T E Romanova; P A Abramov; M N Sokolov

doi:10.1039/c6dt04843a

Hyphenated techniques in speciation analysis of polyoxometalates: identification of individual [PMo_12-xV_xO₄₀]^-3-x (x = 1-3) in the reaction mixtures by high performance liquid chromatography and atomic emission spectrometry with inductively coupled plasma

Dalton Trans. 2017 Mar 14;46(11):3541-3546. doi: 10.1039/c6dt04843a.

Authors

O V Shuvaeva¹, A A Zhdanov², T E Romanova¹, P A Abramov¹, M N Sokolov¹

Affiliations

¹ Nikolaev Institute of Inorganic Chemistry SB RAS, Acad. Lavrentieva ave., 3, 630090, Novosibirsk, Russia. olga@niic.nsc.ru and Novosibirsk State University, 2, Pirogova str., 630090, Novosibirsk, Russia.
² Boreskov Institute of Catalysis SB RAS, Siberian Branch of Russian Academy of Sciences, Acad. Lavrentieva ave., 5, 630090, Novosibirsk, Russia.

PMID: 28240339
DOI: 10.1039/c6dt04843a

Abstract

Unambiguous identification of polyoxometalate (POM) species generated in self-assembly reactions in solution is rather problematic due to close similarity of their properties such as solubility and spectral characteristics. The situation is made more complex by protonation equilibria (which can change their analytical signals) and the lack of individual compounds to serve as standards for individual members of these mixtures. In the present work a new approach to the study of such POMs has been suggested, taking molybdovanadates [PMo_12-xV_xO₄₀]^-3-x as a model. The key feature of this approach consists of generation of so-called "conditional model systems" that include most of the expected components of a mixture formed by self-assembly, tracked down by reliable detection techniques, e.g., ⁵¹V NMR-spectroscopy in this particular case. Then the proposed composition of the mixture is verified and corrected by means of high-performance liquid chromatography coupled with inductively coupled plasma atomic emission spectrometry (HPLC-ICP-AES).