Unknown isopolyoxovanadate species detected by electrospray mass spectrometry

Reaction Dynamics and Solution Chemistry of Polyoxometalates by Electrospray Ionization Mass Spectrometry

“…The potential of ESI‐MS to resolve aqueous speciation was investigated early on. A comprehensive series of studies was carried out by von Nagy‐Felsobuki and co‐workers, who investigated the solution chemistry of V,22, 23 W,24 Mo,[25] Cr,26 Nb, and Ta polyoxo ions by ESI‐MS 27. In all cases they observed signals which were assigned to new species that have not been reported by other methods.…”

“…The potential of ESI-MS to resolve aqueous speciation was investigated early on. A comprehensive series of studies was carried out by von Nagy-Felsobuki and co-workers, who investigated the solution chemistry of V, [22,23] W, [24] Mo, [25] Cr, [26] Nb, and Ta polyoxo ions by ESI-MS. [27] In all cases they observed signals which were assigned to new species that have not been reported by other methods. While the only homoleptic isopolyoxoniobates that have been unambigiously characterized to date are [Nb 6 O 19 ] 8À , [Nb 10 O 28 ] 6À , and [Nb 20 O 54 ] 8À , [28] the authors also observed species with 4, Figure 5.…”

An unprecedented silver-decavanadate dimer investigated using ion-mobility mass spectrometry

“…In the lower m/z range 1 exhibits a high level of disassembly with cluster fragments ranging from four vanadium atoms, [V 4 O 11 ] 2À , to ten, [V 10 O 26 ] 2À with missing oxo ligands. Many of these fragments are in perfect agreement with the assignments presented by Nagy-Felsobuki et al in a comprehensive study of isopolyoxovanadates in aqueous solution using Electrospray Ionisation (ESI) MS. 21,22 Novel silver-containing vanadate fragments were also detected along with intact clusters including silver(I) or protons (or a mixture of both) for charge balance, see Fig. 3.…”

Use of ion-mobility mass spectrometry (IMS-MS) to map polyoxometalate Keplerate clusters and their supramolecular assemblies

“…It has also been used to study POM self-assembly mechanisms, 5,6 and as a discovery tool to detect new structures present in reaction mixtures prior to isolation. [7][8][9] Unfortunately, deconvolution of these systems can be difficult: use of a narrow range of building blocks, often in vast numbers, yields multiple species of very similar mass-to-charge ratios (m/z), but very different sizes/structures, resulting in overlapping envelopes in the mass spectra. 10 Ion mobility mass spectrometry (IMS-MS) is promising as a means to resolve this plethora of isobaric ions, separating according to their size/shape along with m/z.…”