Electrospray identification of new polyoxochromate species

Sahureka, Frans; Burns, Robert C.; Nagy‐Felsobuki, Ellak I. von

doi:10.1016/s0020-1693(01)00715-0

Cited by 23 publications

(28 citation statements)

References 29 publications

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“…In this scenario, the cluster would quickly fragment in the coordinating solvent to form the (F) and (G) families of clusters which would gain the neutral fragments necessary to form species with core stoichiometries corresponding to all the larger cluster families. The formation of such polymer like species has previously been observed for titanium alkoxides as well as various polyoxometallate species in solution [18,34,35] and is very likely. These neutral adducts would then be progressively removed from the large species at higher cone voltages to give the appearance of large cluster degradation.…”

Section: Resultsmentioning

confidence: 63%

Characterization of Ti₆O₄(O₂C₄H₅)₈(OCH₂CH₃)₈ by electrospray time of flight mass spectrometry

Khitrov

Strouse

Gaumet³

2004

J. Am. Soc. Mass Spectrom.

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A titanium oxide molecular cluster prepared by hydrolysis of titanium tetraethoxide in the presence of methacrylic acid, can be characterized by electrospray time of flight mass spectrometry (ESMS-TOF). The chemistry of such systems is not well known and ESMS is a powerful technique for studying the reactions of clusters in solution. The fingerprint of the cluster fragmentation suggests formation of Ti(x)O(y) core fragments that represent commonly observed structural constructs in bulk titanium oxide metallates. The fragmentation steps provide insight into the hydrolytic conversion of this molecular sol gel intermediate into bulk TiO(2). While MS has been applied to the study of metal alkoxide hydrolysis mechanisms, mass spectra of isolated individual titanium oxide clusters have not previously been reported.

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Section: Resultsmentioning

confidence: 63%

Characterization of Ti₆O₄(O₂C₄H₅)₈(OCH₂CH₃)₈ by electrospray time of flight mass spectrometry

Khitrov

Strouse

Gaumet³

2004

J. Am. Soc. Mass Spectrom.

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“…Mixed-oxidation-state fragments of polyoxochromate systems have also been identified in solutions during the course of ESI-MS studies. [37] In the case of the anions {M 25 Se} 3 a and {M 36 Se 10 } 4 a, the clusters did not retain their integrity in solution during the course of the MS studies and consequently extensive fragmentation has been observed.…”

Section: Esi-ms Spectroscopymentioning

confidence: 97%

Controlling the Self‐Assembly of a Mixed‐Metal Mo/V–Selenite Family of Polyoxometalates

Corella‐Ochoa

Miras

Long

et al. 2012

Chemistry A European J

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Five mixed-metal mixed-valence Mo/V polyoxoanions, templated by the pyramidal SeO(3)(2-) heteroanion have been isolated: K(10)[Mo(VI)(12)V(V)(10)O(58)(SeO(3))(8)]⋅18 H(2)O (1), K(7)[Mo(VI)(11)V(V)(5)V(IV)(2)O(52)(SeO(3))]⋅31 H(2)O (2), (NH(4))(7)K(3)[Mo(VI)(11)V(V)(5)V(IV)(2)O(52)(SeO(3))(Mo(V)(6)V(V)-O(22))]⋅40 H(2)O (3), (NH(4))(19)K(3)[Mo(VI)(20)V(V)(12)V(IV)(4)O(99)(SeO(3))(10)]⋅36 H(2)O (4) and [Na(3)(H(2)O)(5){Mo(18-x)V(x)O(52)(SeO(3))} {Mo(9-y)V(y)O(24)(SeO(3))(4)}] (5). All five compounds were characterised by single-crystal X-ray structure analysis, TGA, UV/Vis and FT-IR spectroscopy, redox titrations, and elemental and flame atomic absorption spectroscopy (FAAS) analysis. X-ray studies revealed two novel coordination modes for the selenite anion in compounds 1 and 4 showing η,μ and μ,μ coordination motifs. Compounds 1 and 2 were characterised in solution by using high-resolution ESI-MS. The ESI-MS spectra of these compounds revealed characteristic patterns showing distribution envelopes corresponding to 2- and 3- anionic charge states. Also, the isolation of these compounds shows that it may be possible to direct the self-assembly process of the mixed-metal systems by controlling the interplay between the cation "shrink-wrapping" effect, the non-conventional geometry of the selenite anion and fine adjustment of the experimental variables. Also a detailed IR spectroscopic analysis unveiled a simple way to identify the type of coordination mode of the selenite anions present in POM-based architectures.

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“…(Hao & March, 2001b), but also by the redox reactions which the solvent undergoes at the capillary of the spray (Gatlin, Turecek, & Vaisar, 1994;Wang & Agnes, 1999a,b). Redox reactions may be experienced also by redox-active ligands as N,N-diethyldithiocarbamate and glutathione (Ross, Ikonomou, & Orians, 2000b), and by metal ions as Cu(II) (Xu, Zhang, & Yergey, 1996;Ross et al, 1998;Bartoszek et al, 1999;Lavanant, Hecquet, & Hoppilliard, 1999;Shen & Brodbelt, 1999;Ross, Ikonomou, & Orians, 2000a;Gianelli et al, 2001;Woodcock et al, 2001;Schroder, Weiske, & Schwarz, 2002;Cerchiaro et al, 2004;Lyapchenko et al, 2004;Franski, 2004a), Fe(III) (Mollah et al, 2000;Ross, Ikonomou, & Orians, 2000a;Neubert, Hider, & Cowan, 2002), Cr(VI) (Sahureka, Burns, & von Nagy Felsobuki, 2002), In(III) (Vasca et al, 2003), Co(III) (Ralph et al, 1996b), Ni(II) (Olesik, Thaxton, & Olesik, 1997), Eu(III) and U(IV) (Stewart & Horlick, 1996). Redox reactions may occur also in other parts of the ES chamber and not only at the capillary tip (Gianelli et al, 2001).…”

Section: Possible Solution Perturbationsmentioning

confidence: 99%

“…Bartok et al (2001) identified some new oxonium aluminium species. Sahureka, Burns, & von Nagy Felsobuki (2002) …”

Section: Comparison Between Qualitative Esi-ms and Other Techniques Rmentioning

confidence: 99%

Electrospray mass spectrometry (ESI‐MS) in the study of metal–ligand solution equilibria

Marco¹,

Bombi²

2005

Mass Spectrometry Reviews

326

256

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In the 20 years, since the introduction of electrospray mass spectrometry (ESI-MS), the use of this technique in various fields of inorganic, organometallic, and analytical chemistry has been steadily increasing. In this study, the application of ESI-MS to the study of metal-ligand solution equilibria is reviewed (till 2004 included). In a first section, advantages and drawbacks of ESI-MS in this type of application are described. Subsequently, a list of ca. 300 studies is reported, in which ESI-MS was used to give number and stoichiometry of the species at equilibrium, or also to estimate their stability constants. All studies are classified according to the metal ions under examination. Other related applications, such as host-guest interactions and metal ion-protein binding studies, are briefly reviewed as well.

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Electrospray identification of new polyoxochromate species

Cited by 23 publications

References 29 publications

Characterization of Ti₆O₄(O₂C₄H₅)₈(OCH₂CH₃)₈ by electrospray time of flight mass spectrometry

Characterization of Ti₆O₄(O₂C₄H₅)₈(OCH₂CH₃)₈ by electrospray time of flight mass spectrometry

Controlling the Self‐Assembly of a Mixed‐Metal Mo/V–Selenite Family of Polyoxometalates

Electrospray mass spectrometry (ESI‐MS) in the study of metal–ligand solution equilibria

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Electrospray identification of new polyoxochromate species

Cited by 23 publications

References 29 publications

Characterization of Ti6O4(O2C4H5)8(OCH2CH3)8 by electrospray time of flight mass spectrometry

Characterization of Ti6O4(O2C4H5)8(OCH2CH3)8 by electrospray time of flight mass spectrometry

Controlling the Self‐Assembly of a Mixed‐Metal Mo/V–Selenite Family of Polyoxometalates

Electrospray mass spectrometry (ESI‐MS) in the study of metal–ligand solution equilibria

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Characterization of Ti₆O₄(O₂C₄H₅)₈(OCH₂CH₃)₈ by electrospray time of flight mass spectrometry

Characterization of Ti₆O₄(O₂C₄H₅)₈(OCH₂CH₃)₈ by electrospray time of flight mass spectrometry