Abstract
A definitive method is described for the indirect assay of several tens of milligrams of urea by coulometric titration. Urea was decomposed in concentrated sulfuric acid using a Kjeldahl flask. Subsequently, the formed ammonium ion was titrated with electrogenerated hypobromite ion in a sodium bromide-sodium tetraborate medium of pH 8.6, with amperometric end-point detection. Parameters affecting the pretreatment procedure were evaluated. The optimized conditions included the heating of 2 g of urea at around 300°C for 2 h with 10 cm3 of sulfuric acid. Under the proposed conditions, the assay value with expanded uncertainty (k = 2), 99.870 ± 0.026%, agreed well with the certified value of NIST SRM 912a urea, 99.9 ± 0.1%.
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Kato, J., Koseki, T., Aoki, Y. et al. Coulometric Titration of Urea with Electrogenerated Hypobromite. ANAL. SCI. 29, 753–755 (2013). https://doi.org/10.2116/analsci.29.753
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DOI: https://doi.org/10.2116/analsci.29.753