• Aimad-Eddine Tamen Oles Honchar Dnipro National University, Ukraine
  • Andriy B. Vishnikin Oles Honchar Dnipro National University, Ukraine
  • Mohammed K.E.A. Al-Shwaiyat Zarka University College, Al-Balqa Applied University, Jordan
  • Borys D. Khmelovskii Oles Honchar Dnipro National University, Ukraine



In-vessel headspace liquid phase microextraction, nitrite determination, spectrophotometry, mine waters


A new, simple, highly sensitive and selective method for the spectrophotometric determination of nitrite based on the method of in-vessel headspace liquid-phase microextraction has been developed. It includes the release of iodine vapor in the reaction of nitrite with an excess of iodide and its absorption by 50 μL of 1% potassium iodide. The acceptor phase is located in the headspace above the solution in a specially designed container. Extraction of iodine takes place from 10 mL of an aqueous solution containing 2 mL of 25% H2SO4, after the introduction of 0.25 mL of 1% KI. Full equilibrium is established after stirring the aqueous solution at 1200 rpm for 17 minutes. After that, the triiodide complex formed in the acceptor phase is removed with a microsyringe and transferred into a quartz microcuvette with a volume of 50 μL and an optical path of 10 mm, in which the absorbance of the solution of the acceptor phase is measured at 350 nm. The calibration graph is linear (r2 = 0.9997) in the range from 3 to 120 µg L–1 (as NO2) with a detection limit of 1.0 µg L–1. The developed method was successfully applied to determine the content of nitrite ions in mine waters and is characterized by a higher sensitivity and lower influence of large amounts of metal ions in comparison with the standard method based on the use of the Griess reagent.

Author Biography

Andriy B. Vishnikin, Oles Honchar Dnipro National University

Head of Analytical Chemistry Department h-index (SCOPUS) = 8


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