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Sensitive Detection and Quantification of Oxygenated Compounds in Complex Samples Using GC-Combustion-MS.

Javier García-Bellido1, Montserrat Redondo-Velasco1, Laura Freije-Carrelo2,3

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A novel gas chromatography detector quantifies oxygen-containing compounds without standards. It uses 18O-enriched oxygen for sensitive detection, achieving the lowest-ever detection limit for trace oxygenates in complex samples.

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Area of Science:

  • Analytical Chemistry
  • Environmental Science

Background:

  • Accurate quantification of oxygen-containing compounds in complex matrices is challenging.
  • Existing methods often require specific standards, limiting their applicability.
  • Trace analysis of volatile organic compounds (VOCs) necessitates highly sensitive detection techniques.

Purpose of the Study:

  • To develop a novel element-selective gas chromatography (GC) detector for accurate quantification of oxygen-containing compounds.
  • To enable standard-free quantification of oxygenates in complex samples.
  • To achieve ultra-low detection limits for trace oxygenates.

Main Methods:

  • Utilized a combustion unit operating at 800 °C with 18O-enriched oxygen as the oxidizing gas.
  • Detected natural oxygen in GC-separated compounds via its incorporation into volatile species and subsequent degradation to 16O.
  • Compensated for unspecific signals using m/z 12 measurement from CO2 degradation.
  • Validated the method using a Standard Reference Material (SRM) and spiked hydrotreated diesel samples.

Main Results:

  • Achieved a record low detection limit of 28 pg of injected oxygen (O).
  • Demonstrated equimolarity with various oxygen-containing compounds.
  • Quantification remained accurate (99-103%) and precise (1-4% RSD) even with coeluting matrix compounds.
  • Successfully quantified 33 oxygenates in a complex wood bio-oil sample and spiked diesel samples with high recovery (102 ± 9%).

Conclusions:

  • The developed element-selective GC detector offers a sensitive and accurate method for quantifying trace oxygenates.
  • The standard-free approach simplifies analysis and broadens applicability to diverse complex samples.
  • This technology represents a significant advancement in trace oxygenate analysis for environmental and industrial applications.