Calcium oxalate was synthesized from calcium chloride solution using oxalic acid in the presence of di sodium salt of ethylenediaminetetraacetic acid (EDTA) and commercially available1-hydroxyethylidene-1,1-diphosphonic acid (HEDP), aquasoft having chelating value 330 (AQ 330). The experiments were carried out at three different temperatures 60, 80 and 100 degrees C. The samples were characterized using scanning electron microscope (SEM), powder X-ray diffraction analysis (XRD) and Fourier transform infrared spectroscopy (FTIR) techniques. The morphological studies reveal that the tendency for agglomeration increases with increase in temperature. Interpretation of XRD pattern confirmed that whewellite with monoclinic structured is the most favored structure in the presence of EDTA where calcium oxalate hydrate having orthorhombic structure is most favored structure in the presence of AQ 330. (C) 2011 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.