In order to prepare iron phosphate by waste sludge, we report a method for effective utilization of the sludge obtained from the electrocoagulation treatment of source-separated urine. The sludge was dissolved with hydrochloric acid and pretreated with H2O2 and Na3PO4; finally, NaOH was added to precipitate iron phosphate from the solution. Thermal treatment of the precipitate at 750 A degrees C in air yielded crystalline quartz-like anhydrous FePO4. The precipitate was characterized by a number of thermal techniques such as thermogravimetry/differential thermal analysis, scanning electron microscopy, and X-ray powder diffraction.