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High field magic-angle spinning (MAS) ³¹P-NMR investigations of novel porous zincophosphates and their cobalt-containing derivatives confirm the framework structure of alternating Zn(Co)O₄ and PO₄ tetrahedra. The MAS NMR spectrum of cobalt-containing products exhibits a large anisotropy manifested in numerous side bands. This effect is attributed to paramagnetic shifts induced by dipolar interactions between the unpaired electrons of Co²⁺ and the ³¹P nuclei. The relative intensity of the side bands is significantly lower in the cobalt-exchanged sample (where the Co²⁺ does not occupy framework sites) than in the cobalt-containing zincophosphates. This shows that ³¹P-NMR measurements can give direct evidence of extra-framework cobalt(II) or of Co(II) incorporation in the zincophosphate lattice.