Magnesium hydrogen phosphate (MHP) and transition metal doped cadmium magnesium hydrogen phosphate (CdMHP) was synthesized in the form of crystalline material by room temperature solution technique known as gel encapsulation technique. The synthesized crystals were then characterized for their structural, mechanical and electrical investigations using various chemical and physical methods. X - ray diffraction analysis (XRD) establishes magnesium hydrogen phosphate and cadmium magnesium hydrogen phosphate belonging to orthorhombic crystal system with space group Pbca. The mechanical behaviour of these crystals was studied by calculating Vicker’s hardness number. The behaviour of microhardness with applied load was observed to be complex. The electrical behaviour was carried out by calculating dielectric constant at different temperatures and for different frequencies. The dielectric constant (ε/) was found to be strongly dependent on temperature and frequency. The transition metal doping of cadmium in magnesium hydrogen phosphate remarkably decrease the value of dielectric constant from 68 to 23. The transition temperature also decreases from 330ËšC in case of magnesium hydrogen phosphate to 310ËšC in case of cadmium magnesium hydrogen phosphate.