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Atomic Absorption Spectroscopy: Lab01:21

Atomic Absorption Spectroscopy: Lab

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For AAS measurements, samples must be introduced as clear solutions, often requiring extensive preliminary treatment to dissolve materials like soils, animal tissues, and minerals. Common methods for sample preparation include treatment with hot mineral acids, wet ashing, combustion in closed containers, high-temperature ashing, or fusion with reagents.
 Solutions containing organic solvents, such as low-molecular-mass alcohols, esters, or ketones, enhance absorbances by increasing...
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Related Experiment Video

Updated: Jan 13, 2026

Automated, High-resolution Mobile Collection System for the Nitrogen Isotopic Analysis of NOx
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Automated, High-resolution Mobile Collection System for the Nitrogen Isotopic Analysis of NOx

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High-Resolution Mass Spectrometry for Nitrate Aerosol Isotopologue Quantification: Method Development, Calibration,

Wendell W Walters1, Addison Bowen1, Meghan E Weatherly1

  • 1Department of Chemistry and Biochemistry, University of South Carolina, Columbia, South Carolina 29208, United States.

Analytical Chemistry
|January 8, 2026
PubMed
Summary

A new mass spectrometry method allows precise measurement of nitrate (NO3-) isotopes, including "clumped" isotopologues, using smaller samples. This advances atmospheric chemistry research by providing detailed insights into nitrate sources and oxidation processes.

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Area of Science:

  • Environmental Chemistry
  • Atmospheric Science
  • Analytical Chemistry

Background:

  • Stable isotope ratios of nitrate (NO3-) are crucial for understanding atmospheric oxidation and source apportionment.
  • Traditional isotope ratio mass spectrometry (IRMS) methods have limitations, including large sample size requirements and inability to measure "clumped" isotopologues.

Purpose of the Study:

  • To develop and validate a high-resolution electrospray ionization Orbitrap mass spectrometry (ESI-Orbitrap) approach for direct quantification of NO3- isotopologues.
  • To establish an optimized sample preparation workflow to minimize biases in isotopic measurements.
  • To enable the characterization of multiply substituted ("clumped") nitrate isotopologues.

Main Methods:

  • Utilized a novel ESI-Orbitrap mass spectrometry technique for NO3- isotopologue analysis.
  • Implemented an optimized sample preparation workflow involving ion chromatography (IC) purification, automated fraction collection, neutralization, water removal, and methanol reconstitution.
  • Calibrated the method using USGS34 and USGS35 standards for precise δ15N, δ18O, and Δ17O measurements.

Main Results:

  • Achieved precise δ15N, δ18O, and Δ17O values (±0.4-0.6‰) and enabled characterization of clumped isotopologues (Δ15N18O, Δ17O18O, Δ18O18O).
  • Demonstrated excellent agreement with the denitrifier-IRMS method for δ15N and Δ17O in aerosol samples.
  • Preliminary data revealed distinct behaviors of different clumped isotopologues, offering insights into oxidation chemistry and nitrogen sources.

Conclusions:

  • The new ESI-Orbitrap method provides a powerful tool for detailed isotopic analysis of atmospheric NO3-, overcoming limitations of traditional methods.
  • The ability to measure clumped isotopologues expands the constraints available for studying atmospheric chemistry and nitrate sources.
  • This approach lays the groundwork for multi-isotopologue analyses of other oxyanion aerosols.