Sustainable, liquid-assisted grindingmechanochemical synthesisof crucial nutrient containing compounds, namely, Ca-and Mg-struvites (CaNH 4 PO 4 •H 2 O and MgNH 4 PO 4 •6H 2 O) and complex double salts (Ca-(NH 4 ) 2 (HPO 4 ) 2 •H 2 O dimorph B, Mg(NH 4 ) 2 (HPO 4 ) 2 • 4H 2 O dimorph A), was performed. These compounds were synthesized using solid crystalline monoammonium phosphate (NH 4 H 2 PO 4 , MAP) and low solubility common calcium and magnesium minerals, such as hydroxides, carbonates, and oxides. Powder X-ray diffraction showed single crystalline phase materials. Properties of the synthesized compounds were studied by thermogravimetric analysis/ differential scanning calorimetry (TGA/DSC), Raman spectroscopy, and dynamic vapor sorption (DVS). TGA results showed that Ca-struvite was the most thermally robust, followed by Ca-and Mg-complex double salts and Mg-struvite. The decomposition of samples with release of NH 3 was marked by peaks in the DSC profiles at 190 °C for both complex double salts and a broad DSC shoulder at 186 °C was observed for struvites. Raman spectroscopy showed the presence of distorted PO 4 3− bands due to protonation of the phosphate species and multiple binding environments. DVS measurements showed that these compounds deliquesced at very high relative humidity conditions (∼90%), which in some cases led to significant changes in the dominant crystalline phase.