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Volume 44 Issue 1
Jan.  2022
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Article Contents
Xu Haoming,Song Guodong,Liu Sumei, et al. A sodium hypobromite oxidation-sulfamic acid reduction method for determination of 15\scriptsize $ {\rm{NH_4^+}} $ \normalsize in 15N enrichment sediment slurry incubation samples[J]. Haiyang Xuebao,2022, 44(1):147–154 doi: 10.12284/hyxb2022024
Citation: Xu Haoming,Song Guodong,Liu Sumei, et al. A sodium hypobromite oxidation-sulfamic acid reduction method for determination of 15\scriptsize $ {\rm{NH_4^+}} $ \normalsize in 15N enrichment sediment slurry incubation samples[J]. Haiyang Xuebao,2022, 44(1):147–154 doi: 10.12284/hyxb2022024

A sodium hypobromite oxidation-sulfamic acid reduction method for determination of 15$ {\bf{NH_4^+}}$ in 15N enrichment sediment slurry incubation samples

doi: 10.12284/hyxb2022024
  • Received Date: 2021-07-20
  • Rev Recd Date: 2021-09-26
  • Available Online: 2021-10-20
  • Publish Date: 2022-01-14
  • Dissimilatory nitrate reduction in marine sediment is one of the key nitrogen loss processes in the ocean. Dissimilatory nitrate reduction to ammonium (DNRA), unlike denitrification and anammox by which nitrate is reduced to N2 and removed from the environment eventually, directly reduce nitrate to ammonium, could lead to eutrophication and water hypoxia afterwards. 15N labeled technique is the main method to investigate dissimilatory nitrate reduction processes in sediments. Accurate determination of 15${\rm {NH}}_4^+ $ in isotope enrichment samples is primarily required to evaluate the potential rate of DNRA. The commonly used method for the determination of 15${\rm {NH}}_4^+ $ at present is the hypobromite iodine oxidation-membrane inlet quadrupole mass spectrometer determination method. However, 30N2 as the final analyte of the method has two problems which lead to an analysis error: firstly, 30N2 determined can be significantly overestimated due to the O2 interference; secondly, the low equilibrium rate of 30N2 in the detector could influence the precision of the method and low down the analysis speed. To solve the problems mentioned, a sodium hypobromite oxidation-sulfamic acid reduction method by which 15${\rm {NH}}_4^+ $ is transformed to 29N2 only and detected using membrane inlet quadrupole mass spectrometer afterwards (Redox-MIMS method) is reported in this article. The results indicate that the optical concentration of sulfamic acid is 80−100 mmol/L; the detection limit is 0.5 μmol/L and the precision (RSD) is 0.8%; the dynamic range of standard curve is 0−150 μmol/L. Comparing with the hypobromite iodine oxidation method, the Redox-MIMS method not only has the advantages of mild reaction conditions and easily obtained reagents, the memory effect of 30N2 in the detector can also be solved effectively for most of the produced 15N2 is 29N2 which improves detection efficiency (2 min per sample) meanwhile. Determination results of rates of DNRA and the contribution of DNRA to all dissimilatory nitrate reduction processes in the Laizhou Bay sediments using both hypobromite iodine oxidation and Redox-MIMS methods shows no significant difference. These make the Redox-MIMS method an accurate and high-efficient method for determination of 15${\rm {NH}}_4^+ $ in isotope enrichment samples.
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