Perturbations produced by electrospray ionization mass spectrometry in the speciation of aluminium(III)/1,6-dimethyl-4-hydroxy-3-pyridinecarboxylate aqueous solutions

2010 ◽  
Vol 24 (7) ◽  
pp. 868-874 ◽  
Author(s):  
Valerio B. Di Marco ◽  
Luca Raveane ◽  
Annalisa Dean ◽  
Pietro Traldi
Keyword(s):  
Mass Spectrometry ◽  
Aqueous Solutions ◽  
Electrospray Ionization ◽  
Electrospray Ionization Mass Spectrometry ◽  
Ionization Mass Spectrometry ◽  
Ionization Mass

Oxygen Exchange During the Reaction of POCl3 and Water

2011 ◽  
Vol 64 (10) ◽  
pp. 1360
Author(s):  
Andrew O. Thomas ◽  
Paul J. Milham ◽  
R. John Morrison ◽  
Robert G. Clark ◽  
Rebeca Alvarez
Keyword(s):  
Mass Spectrometry ◽  
Aqueous Solutions ◽  
Electrospray Ionization ◽  
Electrospray Ionization Mass Spectrometry ◽  
Oxygen Exchange ◽  
Natural Abundance ◽  
Ionization Mass Spectrometry ◽  
Ionization Mass ◽  
O Isotope ◽  
The Way

To investigate O exchange during the reaction of POCl3 and water, natural abundance POCl3 was reacted with water highly enriched in 18O, and the resulting H3PO4 was isolated as KH2PO4. This reaction was conducted with and without tetrahydrofuran (THF) as a solvent, and was controlled in THF and violent in its absence. Approximately 5 × 10–4 M aqueous solutions of the KH2PO4 were analyzed using electrospray ionization mass spectrometry, to estimate the proportions of the mass-clumped 16,17,18O isotope analogues of [H2PO4]–. During analysis, ~29 % of [H2PO4]– dehydrated to [PO3]–, for which the proportions of the O isotope analogues were also measured. These proportions were compared with those predicted for O exchange at either four or three positions on the P atom of POCl3. The data strongly support O exchange at all four positions, whether or not THF was used to moderate conditions during the reaction. This result clears the way for safe, predictable synthesis of heavy-O labelled orthophosphate from POCl3 and 18O enriched water for evaluation as an environmental and biochemical tracer.

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