A spectrophotometric method for nitrite determination in simulated Purex Process solutions is presented, utilizing the Griess reagent for the formation of the coloured azocompound with an absorption maximum at 525 nm. Molar absortivity was 36,262 and the sensitivity of the method 10/sup -6/M for nitrite. The calibration curve is linear in the range of 2 to 30..mu..g NO/sup -//sub 2//25 ml in cells of 1 cm optical path. The method can be used in the presence of uranium up to limits of an U/NO/sup -//sub 2/ ratio of 150. Test solutions were prepared to simulate composition and concentrations as obtained by irradiating standard fuel with a neutro flux of 3.2 x 10/sup 13/ n.s/sup -1/.cm/sup -2/, with a burn-up value of 33,000 Mwd/T and cooling time of two years. Nitrite determinations in these solutions were accurate within limits of 5%.