Interferences in the determination of total nitrogen in natural waters by photo-oxidation to nitrate-nitrite mixture.
The method proposed by Armstrong, Williams and Strickland for the photo-oxidation of total nitrogen in sea-water to nitrate and nitrite has been studied in some detail, to extend its use to fresh and brackish waters, applying a more accurate method for the determination of the reaction products. Variables influencing the yield of nitrate and nitrite are irradiation time, pH and type of buffer, kind of nitrogen compound and its concentration, and the concentrations of oxygen, carbon dioxide, organic matter and salts, especially bromides, even at the low concentrations found in brackish waters. All these variables interact in a rather complicated way. Interferences from halides, organic matter and carbon dioxide are considerably reduced by ensuring that the pH is kept at 8.5-9 during the irradiation. Because pure solutions of many substances give quantitative yields (> or = 98%) in the pH-range 7-9 usually recommended, whereas others require lower pH for maximal oxidation, a method has been developed involving photo-oxidation first at pH 2.1 and then at pH 8.5-9. In the absence of interfering concentrations of halides the relative increase in yield by an initial irradiation at low pH is especially large (10-36%) for proteins, organic nitrogen in fresh waters, uric acid and urea. A comparison is made between determination of total nitrogen in some natural waters by using photo-oxidation and by a Kjeldahl method modified to give total nitrogen. By making use of the optimal conditions presented in this paper, a negative error of less than 8% is expected in the determination of total nitrogen in fresh waters. For saline waters the error will probably be larger, at least at a high ratio of organic to inorganic nitrogen.
Gustafsson
L
L
Department of Analytical Chemistry, University of Uppsala, P.O. Box 531, S-751 21 Uppsala, Sweden.