RAPET (Reactions under Autogenic Pressure at Elevated Temperature) method has been used to synthesize lithium titanium phosphate anode material. The prepared compound is characterized by X-ray diffraction analysis. The electrochemical behavior has been studied in different aqueous electrolytes using cyclic voltammetry (CV), galvanostatic charge-discharge and electrochemical impedance spectroscopy (EIS) techniques. CV peak current is proportional to the square root of scan rate. The system satisfies the required conditions for a reversible redox system. LiTi2(PO4)(3) is found to undergo lithium insertion at all concentrations of LiNO3 electrolyte. The values of -Z '' when all the points of the impedance spectra measured in 2 M Li2SO4 electrolyte compared at 5 mHz are found to show a minimum at the potential close to the CV peak potential during charge and discharge. The cell, LiTi2(PO4)(3)/2 M Li2SO4/LiNi1/3Mn1/3Co1/3O2 delivers a discharge capacity of 116 mAh g(-1) in the first cycle at an applied current of 0.2 mA cm(-2) (C/5(rate)) and it retains a capacity of 107 mAh g(-1) over 100 cycles with good rate capability. The non-aqueous cell, Li/1 M LiAsF6/EC-DMC/LiTi2(PO4)(3) delivers a discharge capacity of 125 mAh g(-1) with a voltage plateau around 2.4 V vs Li/Li+. (C) 2012 The Electrochemical Society. [DOI: 10.1149/2.074207jes] All rights reserved.