In this work, KHSO4:Mn crystals doped with Mn and K2SO4 were synthesized using an aqueous solution method. The samples were exposed to ionizing radiation in order to observe the effects on their physical properties. Raman spectroscopy was used to identify the structure of the crystals by detecting the vibrational frequencies of the crystalline lattice. Electron paramagnetic resonance (EPR) was used to study the creation of paramagnetic centers arising from exposure to ionizing radiation. This new synthesis method produces high quality K2SO4 and KHSO4:Mn crystals and allows control of structural, morphological, optical and magnetic properties. © 2009 Elsevier B.V. All rights reserved.