Abstract: In acidic medium that NO2－ oxidize [Fe(CN)6]4- to [Fe(CN)6]3- and luminol—[Fe(CN)6]3-uric acid chemiluminescence system was coupled together, thus a new method for the determination of trace nitrite was developed. The effect of factors，such as consistency of various substance of reaction, acidity, disturbing ions etc., on the analytical results were studied. The Detection Limit was 5.0×10-5mg/L (3a). The Linear Range was at 0.001~10 mg/L. The parallel determination was done 12 times and the relative standard deviation was no more than 3.6%. The recovery was at the range of 97.5 to 104.