Online zinc reduction-sequential injection analysis for the determination of nitrogen species in extracts of riverine sediment

Abstract

Background: The substitution of hazardous analytical reagents such as Cd with benign alternatives for chemical determination is one of the principles of green chemistry. An eco-friendly Zn reduction method for nitrate determination was developed to achieve this end. Methods: Online zinc reduction-sequential injection analysis (ZnR-SIA) protocol was developed for the determination of nitrogen (N) species in the Lagos Lagoon sediments by modification of some standard methods. Results: The novel application of boric acid-borate buffer employed in borate-buffered granular Zn reduction suppressed gas evolution from the Zn micro-column, making the Zn reduction adaptable to online use, unlike the frequently used ammonia-ammonium buffer. Further results showed that the sampling rate for the two-zone stack was 65 h−1. The boric acid-borate buffer offered 5.9-fold and 1.3-fold of the instrument response given by the ammonia-ammonium buffer at 0.50 and 5.0 mg N L−1 respectively. The method detection limits of the ZnR-SIA for the three matrices studied were 24.6 μg N L−1 for reagent water, 0.383 mg N kg−1 for KCl-extractable nitrate, and 3.18 mg N kg−1 for total nitrogen. The average recovery of nitrate-N in matrix samples was 94.7%, and its precision was 4.52%. The average recoveries of total N in blanks and matrix samples were 97.9 and 93.2% respectively. Conclusions: The method accuracies demonstrated the suitability of the ZnR-SIA for sediment N determination. Zn reduction is recommended where sustainable development is desired and is a potential substitute for the standard Cd reduction owing to Cd toxicity.