KDP is a versatile NLOmaterial grown by lowtemperature solution growth. It is used inmany solid-state electronic applications. Single crystals of KDP and (Co,Mg, Li, Ni) doped KDP were grown by the slow evaporation technique. The grown crystals were confirmed by powder XRD technique. The solubility studies indicated that the impurity level at 1 mol% changes the metastable zonewidth and the induction period gets reduced. It was observed that when the (Co, Mg, Li, Ni) dopants were added at 1 mol %, the crystallinity of thematerial was found to increase. FTIR investigations indicated that the impurities played an important role in the spectral characteristics of thematerial. High ResolutionXRD revealed the comparative crystalline nature of the doped crystals.