A series of sodium borosilicate glasses containing cesium, molybdenum, and chromium was prepared to investigate the partitioning of chromium amongst the glass and phase-separated crystalline molybdates. The precipitates were examined by 133Cs, 23Na, and 95Mo MAS NMR, revealing a phase assemblage consisting of Na2MoO4, Na2MoO4·2H2O, Cs2MoO4, Cs2CrO4, CsNaMoO4·2H2O, and Cs3Na(MoO4)2. 133Cs MAS NMR indicates random substitution of Cr into the Mo sites of Cs3Na(MoO4)2 and provides a quantitative assessment of Cr incorporation. The sample compositions were verified by various analytical techniques and highlight the centrality of NMR in the identification and quantification of heterogeneous crystalline composites, including sensitivity to cationic substitution. The observation and facile interconversion of hydrated phases invites careful consideration of these materials for nuclear waste disposal.
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