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Various metal-substituted ammonium gallophosphates (metal is Zn, Mn, Mg, and Fe) have been synthesized. Characterization by X-ray diffraction (XRD), X-ray absorption spectroscopy (XAS), and 31 P MAS and 71 Ga MAS NMR shows that the structures are similar and isostructural to the known ammonium cobalt gallophosphate hydrate, [NH 4 ][CoGa 2 P 3 O 12 -(H 2 O) 2 ]. It is concluded from a combined in situ XRD/XAS study that the gallophosphate molecular sieves described here are not thermally stable and lose their microporous nature above 350°C.