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June 5, 20260 citationsOpen Access

Benchtop NMR Spectroscopy of Pyrolysis Oils From Mixed Plastic Waste: Parameter Optimization for Oil Characterization and Detection of Heteroatom‐Containing Compounds

AGAnika GoeckeJVJonas VogtSTSalar Tavakkol

Key Points

  • This research aims to optimize benchtop NMR spectroscopy for analyzing pyrolysis oils and detecting heteroatom-containing compounds.
  • Analyzed pyrolysis oils using $^1$H-NMR and 2D-correlation spectroscopy (COSY).
  • Optimized measurement and postacquisition parameters to enhance signal-to-noise ratio (SNR).
  • Simulated heteroatom detection with polyolefin-based pyrolysis oils mixed with various organic compounds.
  • Achieved a detection limit of 0.001 wt% for phenylacetaldehyde in a hydrocarbon model mixture (SNR > 3).
  • Detection limits for heteroatom-containing substances in real pyrolysis oils were 1-0.1 wt%, limited by overlapping peaks and low sensitivity.
  • Successful optimization led to faster analysis but highlighted challenges in detecting specific compounds within the complexity of pyrolysis oils.

Abstract

Using pyrolysis oils from plastic waste as an alternative to fossil feedstocks presents a sustainable opportunity for the petrochemical industry. However, depending on feedstock and pyrolysis conditions, the resulting pyrolysis oils differ in chemical composition and may contain heteroatoms exceeding the concentrations limits of petrochemical processes. This publication evaluates benchtop NMR spectroscopy for fast analysis of pyrolysis oils with respect to potential online measurements. The signal-to-noise ratio (SNR) of ¹H-NMR experiments was enhanced by optimizing the measurement and postacquisition parameter on two state-of-the-art spectrometers. To simulate the detection of heteroatoms in an industrial process, two polyolefin-based pyrolysis oils were mixed with ε-Caprolactam, acrylonitrile, benzoic acid, acetophenone, and phenylacetaldehyde in varying concentrations from 10 to 0. 1 wt% and analyzed using ¹H-NMR and 2D-correlation spectroscopy (COSY) experiments. The limit of detection (LOD, SNR > 3) within 35 min measurement time in ¹H-NMR for a concentration series of phenylacetaldehyde in a hydrocarbon model mixture was determined as 0. 001 wt% (equivalent to 0. 64 proton-ppm). However, the detection of the investigated heteroatom-containing substances in real pyrolysis oils remains challenging and the detection limit of 1–0. 1 wt% was much higher due to overlapping peaks in ¹H experiments and comparably low sensitivity of COSY measurements.

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Cite This Study

Goecke et al. (2026) studied this question.

synapsesocial.com/papers/6a22692e763171746d547be2https://doi.org/10.5445/ir/1000193783
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