School of Studies in Chemistry, Pt. Ravishankar Shukla University, Raipur-492 010, India E-mail: debmanas@yahoo.com Manuscript received 17 October 2003, accepted 17 March 2004 A sensitive and simple spectrophutumetric method for determination of NiII with 2-[(5-hromo-2-pyridylazo)]-5- diethylaminophenol (5-Br-PADAP) and N-hydroxy-N,N' -diphenylhenzamidine (HDPBA) is described. The NiII-2-[(5-bromo- 2-pyridylazo)]-5-diethylaminophenol (5-Br-PADAP) complex is extracted with N-hydroxy-N,N' -diphenylbenzamidine (HDPBA) in chloroform at pH range 4.0-6.0 to give red colour complex. Extracted complex shows λmax at 530 nm. Procedure is checked by finding relative standard deviation (RSD, n = 10) value for solutions each containing 2.0 µg mI-1 NiII and the RSD value of the procedure is found to he 1.6%. The system obeyed Beer's law up to 0.5 (.lg ml-1 of nickel and the identification limit of the method is 7.4 x 10-10 g ml-1 on a three times the standard deviation of the blank absorbance basis. The Sandell's sensitivity and molar absorptivity of the complex are 0.00056 µg ml-1 and 1.04 x 105 dm3 mol-1 cm-1 respectively. The effect of foreign ions and other experimental variables are studied.