Consecutive estimation of nitrate and nitrite ions can be made by electron paramagnetic resonance spectrometry
The basic reaction used in the present study for turning the EPR-silent Fe(dtc)3 to the EPR-active FeNO(dtc)2 complex:
(1)NO2(NO)+Fe(dtc)3→FeNO(dtc)2+…was described previously [34 and 37] and has been used directly for estimation of the N2O4 background concentration in air.
The consecutive estimations of nitrate and nitrite ions were based on:
1. quantitative liberation of NO gas in the reaction of nitrite ion with an acidic solution of FeSO4:
(2)NO2−+nFeSO4+mH2SO4→NO+…In aerobic systems NO gives NO2 (or N2O4). Both NO and NO2 are further trapped by Fe(dtc)3 to give Fe(NO)(dtc)2 according to reaction (1) [34. N.D. Yordanov, V. Terziev and B.G. Zheliazkowa. Inorg. Chim. Acta 58 (1982), p. 213. Abstract | PDF (350 K) | View Record in Scopus | Cited By in Scopus (4)34 and 37];
2. the nitrate present in the acidic solution of FeSO4 quantitatively yields Fe(NO)SO4 in solution according to reaction (3):
(3)NO3−+nFeSO4+mH2SO4→Fe(NO)SO4+…Further addition of Nadtc to this solution gives the EPR-active Fe(NO)(dtc)2, which may be separated by extraction.