Abstract Application of a portable spectrophotometric analysis system for measurement of nitrite in seawater is described in this work. The spectral analysis system (SEAS) used for observations of the primary nitrite maximum (PNM) has an operational depth of 500 m and is capable of fully autonomous data acquisition and analysis. The liquid core waveguides (LCWs) used as optical cells in SEAS allow for optical pathlengths as long as 5 m and provide subnanomolar detection limits for a variety of analytes. The 1-m waveguide used in the present study had an internal volume of 0.52 cm 3 and provided NO 2 − measurement precisions and detection limits on the order of 1.2 and 2.5 nM. The time required for a complete in situ analysis, approximately 3–5 min, allows acquisition of detailed profiles on time scales commensurate with the duration of typical hydrocast operations. NO 2 − profiles in the Gulf of Mexico showed very sharp gradients over a 5–10-m depth range and a primary nitrite maximum between 100 and 130 m. A shoulder was often observed approximately 10 m below the primary maximum, with relatively slowly decreasing NO 2 − concentrations at increasing depth.