Jump to main content
Jump to site search

Issue 10, 2018
Previous Article Next Article

A HPLC-ICP-AES technique for the screening of [XW11NbO40]n aqueous solutions

Author affiliations

Abstract

The reaction of H3[PW12O40] with (NH4)[NbO(C2O4)2(H2O)2]·3H2O leads to the straightforward incorporation of Nb into a Keggin anion backbone resulting in [PW11NbO40]4− in nearly quantitative yield. Solution behavior of this monosubstituted anion as a function of pH was studied through 31P NMR and HPLC-ICP-AES techniques (a combination of chromatography and ICP-AES). Increasing of the pH leads to the elimination of Nb from the structure with the formation of mixed Nb/W Lindqvist-type anions and monolacunary [PW11O39]7−. In aged solutions of [PW11NbO40]4− the formation of a mixture of [PNb2W10O39]5− isomers was detected. The HPLC-ICP-AES technique was applied for the study of [BW11O39]9− behavior in aqueous solutions at different pH values and for monitoring the [GeW11O39]4− reaction with the niobium oxalate complex. Despite the presence of the nucleophilic Nb[double bond, length as m-dash]O group [PW11NbO40]4− does not coordinate Co2+ in DMF or Ni2+ in CH3CN, producing double [Co(DMF)6][PW11NbO40]·2.6DMF (2) and [Ni(CH3CN)5.5(H2O)0.5]2[PW11NbO40]·1.7CH3CN (3) salts instead.

Graphical abstract: A HPLC-ICP-AES technique for the screening of [XW11NbO40]n− aqueous solutions

Back to tab navigation

Supplementary files

Publication details

The article was received on 30 Nov 2017, accepted on 28 Feb 2018 and first published on 01 Mar 2018


Article type: Paper
DOI: 10.1039/C7NJ04702A
Citation: New J. Chem., 2018,42, 7940-7948
  •   Request permissions

    A HPLC-ICP-AES technique for the screening of [XW11NbO40]n aqueous solutions

    A. A. Shmakova, M. M. Akhmetova, V. V. Volchek, T. E. Romanova, I. Korolkov, D. G. Sheven, S. A. Adonin, P. A. Abramov and M. N. Sokolov, New J. Chem., 2018, 42, 7940
    DOI: 10.1039/C7NJ04702A

Search articles by author

Spotlight

Advertisements