To provide site specific atomic scale resolution, two dimensional 1 H 31 P heteronuclear correlation (HETCOR) spectroscopy was performed. This correlates the 1 H signals with the neighbouring P resonances, enabling spatial proximities in the physical mixture and composite to be determined. The resulting HETCOR spectra (Fig. ) both show the presence of sets of correlations between the CH (at ~ 6 ppm) / CH3 (at ~ 2 ppm) groups of the ZIF-8 with the Q 2 (-20 ppm) / Q 1 (-10 ppm) / Q 0 (0 ppm) signals of 50(Na2O)-50(P2O5) within the glass-MOF that are not present in the inorganic glass itself (Fig. ). These correlations unequivocally illustrate the presence of close H•••P proximities between ZIF and inorganic glass. Some differences between the HETCOR spectra for the physical mixture and the composite can be discerned, though all broadly point to proton and phosphorous sites being in close proximity. C and N CP MAS NMR spectra have previously been extensively used to confirm the retention of chemical composition and provide evidence for imidazolate linker de-coordination during (ZIF) amorphisation. Both 13 C and N CP MAS NMR ) that are commensurate with crystalline ZIF-8 as expected. Two signals at 13.8 and 14.9 ppm are observed in (ZIF-8)0.3/(IG)0.7 for the methyl group (Fig. ) whilst only one is seen in [(ZIF-8)0.3(IG)0.7] (Fig. ). This may indicate hydrogen bonding between the ZIF-8 protons and the Q 1 , Q 2 and Q 3 terminal oxygens of the IG (by analogy with recent findings on sulfonyl containing ionic liquid in the pores of ZIF-8) or phase separation before heat treatment. Recent work on Zn MAS NMR at very high field has also demonstrated that this low receptive quadrupolar nucleus is very sensitive to short range disorder in several ZIFs. The corresponding Zn spectra for crystalline ZIF-8 at 18.8 T shows a single resonance, broadened to the 2 nd order by the quadrupolar interaction for the crystallographically unique Zn tetrahedron that is largely maintained in the (ZIF-8)0.3/(IG)0.7 physical mixture (Fig. ). Upon thermal treatment and composite formation to [(ZIF-8)0.3(IG)0.7], the 67 Zn MAS NMR spectrum further broaden, slightly with a clear change in 2 nd order quadrupolar lineshape (Fig. ), perhaps identifying an interaction of the inorganic glass with the Zn sites. It is worth pointing out that this broadening is significantly smaller than the one observed for amorphous ZIF-8 (Fig. ), where the lineshape is dominated by structural disorder around the Zn site, highlighting the retention of the short range order in ZIF-8 for the [(ZIF-8)0.3(IG)0.7] composite.