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


Reaction of H3[PW12O40] with (NH4)[NbO(C2O4)2(H2O)2]·3H2O leads to straighforward incorporation of Nb into the Keggin anion backbone resulting in [PW11NbO40]4– in nearly quantitative yield. Solution behavior of this monosubstituted anion as a function of pH was studied by 31P NMR and HPLC-ICP-AES techniques (combination of chromatography and ICP-AES). Increasing of pH leads to 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– formation of a mixture of [PNb2W10O39]5– isomers was detected. The HPLC-ICP-AES technique was applied for study of [BW11O39]9– behavior in aqueous solutions at different pH values and for monitoring of [GeW11O39]4– reaction with the niobium oxalate complex. Despite the presence of nucleophilic Nb=O group [PW11NbO40]4– does not coordinate Co2+ in DMF or Ni2+ in CH3CN, producing instead double [Co(DMF)6][PW11NbO40]∙2.6DMF (2) and [Ni(CH3CN)5.5(H2O)0.5]2[PW11NbO40]·1.7CH3CN (3) salts.

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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, Accepted Manuscript
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    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. V. Korolkov, D. G. Sheven, S. A. Adonin, P. A. Abramov and M. N. Sokolov, New J. Chem., 2018, Accepted Manuscript , DOI: 10.1039/C7NJ04702A

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