A method for spectrophotometric determination of nitrite and nitrate is described. This method is based on the reduction of phosphomolybdic acid to phosphomolybdenum blue complex by sodium sulfide. The obtained phosphomolybdenum blue complex is oxidized by the addition of nitrite and this causes a reduction in intensity of the blue color. The absolute decrease in the absorbance of the blue color or the rate of its decrease is found to be directly proportional to the amount of nitrite added. The absorbance of the phosphomolybdenum blue complex is monitored spectrophotometrically at 814 nm and related to the concentration of nitrite present. The effect of different factors such as acidity, stability of the complex, time, temperature, phosphate concentration, molybdenum concentration, sodium sulfide concentration and the tolerance amount of other ions have been reported. Maximum absorbance is at 814 nm. The range of linearity using the conventional method is 0.5–2.0 ppm with molar absorptivity of 1.1×104 l mol−1 cm−1. and a relative standard deviation of 2.6% for five measurements. The range of linearity using the reaction rate method is 0.2–3.6 ppm with a relative standard deviation of 2.4% for five measurements. The method is applied for determination of nitrite and nitrate in water, meat products and vegetables.