Mixed crystal, potassium zinc vanadium sulphate was grown from an aqueous solution containing equimolar proportions of K2Zn(SO4)2·6H2O (Tutton’s salt) and VOSO4 by slow evaporation at room temperature. Single crystal XRD analysis reveals that it belongs to monoclinic system with P21/c space group, and cell parameters are a = 9.006, b = 12.163, c = 1.36, and V = 649.6 Å3. The co-existence of VO(II)- and Zn in the Tutton’s salt crystalline matrix was confirmed by atomic absorption spectroscopy and energy dispersive X-ray spectroscopy. Scanning electron microscopy exhibits defect centres and crystal voids. The XRD and FT-IR analyses indicate the stress that the mixed crystal undergoes as a result of incorporation of vanadium. Thermal patterns of Tutton’s salt and the mixed crystal are compared. DTA curve exhibited a sharp endothermic peak at 420 °C for the pure K2Zn(SO)4·6H2O and at 410 °C for the mixed crystal.