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High-pressure synchrotron Mössbauer (SMS) and X-ray emission (XES) spectroscopic measurements were conducted to investigate the spin and valence states of iron in (Al,Fe)-bearing magnesium silicate glass (Mg 0.79 Fe 0.10 Al 0.10 Si 0.96 O 3 ) up to 126 GPa and 300 K. By analyzing the Fe  K β emission spectra using the integrated relative difference (IRD) method, which accounts for the spectral broadening effects, the derived total spin momentum ( S ) of the iron in the glass shows no observable changes with pressure within the experimental uncertainties. A two-doublet fitting model representing two diverse local iron atomic environments was used to satisfactorily simulate the high-pressure SMS spectra of iron in the glass. The doublet with an averaged quadrupole splitting (QS) value of 1.94(±0.25) mm/s and chemical shift (CS) of 1.02(±0.25) mm/s at ambient conditions was assigned to be high-spin Fe2+, whereas the second doublet with QS = 0.83(±0.25) mm/s and CS = 0.49(±0.25) mm/s was assigned to be high-spin Fe 3+ . Increasing pressure continuously elevates the QS of Fe 2+  from  ~ 2 mm/s at ambient pressure to 3.5 mm/s at 126 GPa, while Fe3+ only exhibits a slight increase in the QS to 1.34(±0.25) mm/s. Comparing with previous experimental and theoretical studies on the local geometries and hyperfine parameters of silicate glasses and minerals, we conclude that the occurrence of the extremely high QS of Fe 2+  in our glass above  ~ 40-50 GPa can be associated with the enhanced density and diverse distortions and geometries of the local Fe 2+  environments. Our combined XES and SMS results show that both Fe 2+  and Fe 3+  ions in Al-bearing silicate remain in the high-spin state, rather than undergoing a spin-pairing transition as proposed previously. Assuming that the silicate glass results can be used as an analog for understanding silicate melts, our results here indicate that iron ions likely experience significant changes in the local environments yet remain overall in the high-spin state in silicate melts at the extreme pressure and temperature conditions of the deep mantle.

Spin and valence states of iron in Al-bearing silicate glass at high pressures studied by synchrotron Mössbauer and X-ray emission spectroscopy