Multinuclear (Al-27, F-19, C-13 andd H-1) NMR measurements at room temperature of aqueous solutions containing 2 M Al(NO3)(3), 2.1 M morpholine, in the presence and absence of 1 M HF, suggest that morpholine is a chemically inactive specie. The proton and carbon chemical shifts of morpholine in the two solutions reveal the same pH dependence, suggesting that morpholine can be used as a probe molecule for pH determination. Moreover, the broad peaks observed in the F-19 and Al-27 NMR spectra are consistent with the formation of multinuclear Al species and Al-F complexes. The observed changes in peak intensities of these same nuclei as a function of pH are in semiquantitative agreement with corresponding intensities calculated from chemical equilibrium reaction models. A more detailed spectral analysis reveals some discrepancies between observed and calculated intensities and is discussed in the text.