Abstract
Electrospray ionization (ESI) time-of-flight mass spectrometry has been used to investigate the pH-dependence of phosphomolybdates in solution from pH = 1.7 to 10.2. Mass spectra are reported for the first time for H<sub>2</sub>Na<sub>2</sub>P<sub>2</sub>Mo<sub>5</sub>O<sub>23</sub><sup>2-</sup>, PMo<sub>9</sub>O<sub>31</sub><sup>3-</sup>, PMo<sub>10</sub>O<sub>34</sub><sup>3-</sup>, and PMo<sub>11</sub>O<sub>37</sub><sup>3-</sup>. The pH dependence of phosphomolybdate species as measured by electrospray is compared with measurements reported for combined potentiometry - <sup>31</sup>P NMR. The pH ranges of most species are similar (±1 pH unit) when measured by these two methods, although some differences are observed. Protonation and solvation of phosphomolybdate species measured by ESI differ from those observed by <sup>31</sup>P NMR. However, the core phosphomolybdate species are measured correctly by ESI.
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