Department of Chemistry, Ravishankar University, Raipur-192 010 Manuscript received 18 March 1982, accepted 28 September 1982 On the basis of diazotization reaction a new sensitive extractive spectrophoto��metric method has been developed for the determination of \(p\)-nitroaniline. \(p\)-Nitro��aniline is diazotized with nitrite in hydrochloric acid medium and subsequently coupled with ��-naphthol to give a purple coloured azo dye in alkaline medium. (��max 580 nm, ��max 3.7 x 104 1. mole-1 cm-1. The azo dye formed is extractable in iso-amyl alcohol. giving a blue coloured extract having molar absorptivity and Sandell's sensiti��vity of 5.2 x 104 1. mole-1 cm-1, 0.0026 ��g cm-2, respectively at ��max 610 nm. Several common species, viz, inorganic cations, phenols, nitrocompounds, aldehydes, ketones, etc. present in polluted water do not interfere. Primary aromatic amines interfere when present in high concentration.