Issue 10, 2018

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

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

Supplementary files

Article information

Article type
Paper
Submitted
30 nóv. 2017
Accepted
28 feb. 2018
First published
01 mar. 2018

New J. Chem., 2018,42, 7940-7948

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

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