A simple, rapid and reasonable selective Complexometric technique for nickel (II) determination using some selected hydroxytriazene as a metallochromic indicator is reported in the present study. The colour change at the end point was from greenish-yellow/yellow to colourless with sharp end point. The pH ranges were 9.3-9.7, 9.0-9.5, 8.5-9.0, 8.0-8.5 while temperature ranges were 25-60, 25-60, 25-60, 25-50 and 25-50 0 C for reagent (i), (ii), (iii), (iv), and (v) respectively. Nickel(II) was determined accurately up to concentration as low as 3.0x10-3 M for reagents (ii), (iv), and (v)) while for reagents (i) and (iii) the concentration range could be even lowered to 1.0x10-3 M for the determination of nickel (II). The ions such as Cl-, Br, NH4 + , Na + , K + did not show any interference in the determination of nickel (II) even when they were present in tenfold excess. Ba 2+ , Mg 2+ , Ca 2+ , were tolerated up to five-fold excess. However Mn 2+ , Pb 2+ , Hg 2+ , Sn 2+ , Th 4+ , Cd 2+ , Co 2+ , Cu 2+ ,Zn 2+ , interfered even at equivalent amount. The method was used to determine nickel in its synthetic alloy with maximum relative error of 0.78 when using secondary masking agent.