Diaminobenzene as a Novel Reagent for Nitrite Assay in Environmental Samples: Evidence for Its Mechanistic Aspects

• Published in: Analytical letters Vol. 41; no. 18; pp. 3342 - 3363
• Main Authors: Pandurangappa, M., Venkataramanappa, Y.
• Format: Journal Article
• Language: English
• Published: Philadelphia, PA Taylor & Francis Group 01.12.2008; Taylor & Francis
• Subjects: Ambient nitrogen dioxide; Amines; Analytical chemistry; Applied sciences; Chemistry; cyclization; Dyes; Exact sciences and technology; Global environmental pollution; Mathematical analysis; nitrate; Nitrates; nitrite; Nitrites; Nitrogen dioxide; o-phenylenediamine; Pollution; reductor column; Sodium arsenite; solvent extraction; Spectrometric and optical methods; spectrophotometry; Trapping; Water; sodium arsenite; Chemical analysis; Dyes; Nitrites; Nitrates; NMR spectrometry; nitrate; Solvent extraction; Chemical enrichment; Amine; Sample preparation; Aqueous medium; Detection limit; Sodium ion; reductor column; Acid medium; Cadmium; Ambient nitrogen dioxide; Interference; Absorption coefficient; o-phenylenediamine; Air; Arsenites; Diazotization; Infrared spectrometry; Biological compound; Soils; Organic solvent; Absorption spectrometry; Trapping; nitrite; Cyclization; Sodium; Environment; Nitrogen dioxide; Spectrophotometry; Benzotriazole; Room temperature
• ISSN: 0003-2719; 1532-236X
• DOI: 10.1080/00032710802508123

o-Phenylenediamine has been used as a reagent to quantify nitrites/nitrates in a variety of sample matrices. The method is based on the cyclization reaction between o-phenylenediamine and nitrite in acid medium. The amine undergoes diazotization with nitrite in the presence of acid to form the diazonium ion, which subsequently cyclizes to yield yellowish orange benzotriazole at room temperature with an absorption maximum at 450 nm. The formed dye has been separated, purified, and characterized by IR, NMR, and spectroscopy techniques. The parameters of the reaction between amine and nitrite have been optimized. The effect of interfering ions on the determination of nitrites/nitrates has been described. The developed method has been applied for the determination of residual NO 2 gas present in the ambient air after fixing it as a nitrite ion using sodium arsenite as a trapping medium. The dye formed has been extracted into organic solvent to improve the detection limit during the measurement of low levels of ambient NO 2 in air. The method obeyed Beer's law in the concentration range 0-250 µg in aqueous medium and 0-50 µg in organic medium with molar absorptivity of 4.09 × 10 4  L mol −1  cm −1 and 4.3 × 10 4  L mol −1  cm −1 respectively. Nitrate is determined by reducing it to nitrite after passing through the copperized cadmium reductor column. The developed method has been applied to determine nitrite/nitrate levels in water, soil, and biological samples.