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Amorphous calcium polyphosphate (CPP) has potential as an implantable drug delivery matrix by virtue of a low temperature gelling protocol that has been shown to eliminate burst release and extend drug release time from the matrix. However, a greater understanding of this material’s interaction with aqueous environments is needed to more fully exploit this application. Variations in aqueous exposure were assessed using as-made amorphous CPP as well as CPP processed using established low temperature protocols. Solid-state 31P-NMR along with thermal and X-ray diffraction analyses were used to track resulting structural changes.