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A new method uses cation exchange resins to extract ammonium (NH4+) from samples, improving the precision of stable nitrogen isotope (δ15N) measurements. This technique enhances accuracy for low-concentration samples and overcomes matrix interferences in environmental analysis.

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Area of Science:

  • Environmental Chemistry
  • Isotope Geochemistry
  • Analytical Chemistry

Background:

  • Stable nitrogen isotope composition (δ15N) of atmospheric ammonia (NH3) and ammonium (NH4+) is crucial for understanding reduced nitrogen burdens.
  • Existing chemical oxidation methods for δ15N-NH4+ analysis lack precision for low concentrations (< 5 μmol L-1) and are susceptible to matrix interferences.

Purpose of the Study:

  • To develop and validate a robust analytical methodology for the precise determination of δ15N values in ammonium (NH4+) samples.
  • To address limitations of current methods, particularly for low-concentration environmental samples and those with complex matrices.

Main Methods:

  • Implementation of a solid-phase extraction (SPE) pretreatment step utilizing cation exchange resins (Biorad AG-50W) for ammonium (NH4+) extraction and concentration.
  • Optimization of extraction conditions using 0.4 g of resin and 10 mL of 4 M sodium chloride solution for complete NH4+ capture.
  • Validation of the method using reference materials, in-house quality control samples, and real-world atmospheric aerosol samples from diverse locations (China, Hawaii).

Main Results:

  • The SPE method achieved accurate and precise δ15N-NH4+ measurements for concentrations as low as 1.0 μM.
  • Atmospheric aerosol sample analysis showed excellent agreement (R2 = 0.99) between pretreated and non-pretreated samples, confirming method reliability.
  • The pretreatment successfully mitigated matrix effects in samples from Hawaii, enabling quantitative oxidation for subsequent δ15N analysis, with a pooled standard deviation of ± 0.5‰.

Conclusions:

  • The developed solid-phase extraction methodology provides a reliable and accurate approach for determining δ15N values in ammonium (NH4+).
  • This pretreatment step is recommended for all environmental NH4+ samples to enhance the precision and accuracy of stable nitrogen isotope measurements.
  • The method effectively overcomes challenges associated with low concentrations and matrix interferences, improving atmospheric reduced nitrogen studies.