Sensitive Method for the Oxidation-determination of Trace Hydroxylamine in Environmental Water Using Hypochlorite Followed by Gas Chromatography

Anal Sci. 2017;33(6):691-695. doi: 10.2116/analsci.33.691.

Abstract

We developed a method for quantifying trace NH2OH in brackish- and sea-water samples. Previously reported methods applicable to fresh water cannot be applied to such samples. We determined that interference in seawater owing to the bromide ion can be removed by the addition of phenol. In our procedure, phenol and hypochlorite solutions were added to a sample solution to oxidize NH2OH to N2O. N2O in the sample was then quantified by headspace analysis. The method is not affected by the salt content or ammonia, nitrate, or nitrite at concentrations of 300 μgN L-1 or less. It has a limit of detection of 0.2 μgN L-1, and can quantify NH2OH in natural water samples with a wide range of salinity. It was applied to samples from Lake Nakaumi, a brackish lake located in the eastern part of Shimane Prefecture, Japan.

Keywords: Brackish water; environmental water; estuary; gas chromatography; hydroxylamine; in situ method; nitrous oxide.