Automated simultaneous monitoring of nitrate and nitrite in surface water by sequential injection analysis

Abstract

A fully automated procedure based on Sequential Injection Analysis (SIA) methodology for simultaneous monitoring of nitrate and nitrite in surface water samples is described. Nitrite was determined directly using the Griess diazo-coupling reaction and the formed azo dye was measured at 540 nm in the flow cell of the fibre-optic spectrophotometer. Nitrate zone was passed through a reducing mini-column containing copperised-cadmium. After the reduction of nitrate into nitrite the sample was aspirated by flow reversal to the holding coil, treated with the reagent and finally passed through the flow cell. The calibration curve was linear over the range 0.05–1.00 mg N l −1 of nitrite and 0.50–50.00 mg N l −1 of nitrate; correlation coefficients were 0.9993 and 0.9988 for nitrite and nitrate, respectively. Detection limits were 0.015 and 0.10 mg N l −1 for nitrite and nitrate, respectively. The relative standard deviation (RSD) values ( n=3) were 1.10% and 1.32% for nitrite and nitrate, respectively. The total time of one measuring cycle was 250 s, thus the sample throughput was about 14 h −1. Nitrate and nitrite were determined in the real samples of surface water, and the results have been compared with those obtained by two other flow methods; flow injection analysis based on the same reactions and isotachophoretic determination used in a routine environmental control laboratory.