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Qualitative characterization of SRM 1597a coal tar for polycyclic aromatic hydrocarbons and methyl-substituted derivatives via normal-phase liquid chromatography and gas chromatography/mass spectrometry

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Abstract

A normal-phase liquid chromatography (NPLC) fractionation procedure was developed for the characterization of a complex mixture of polycyclic aromatic hydrocarbons (PAHs) from a coal tar sample (Standard Reference Material (SRM) 1597a). Using a semi-preparative aminopropyl (NH2) LC column, the coal tar sample was separated using NPLC based on the number of aromatic carbons; a total of 14 NPLC fractions were collected. SRM 1597a was analyzed before and after NPLC fractionation by using gas chromatography/mass spectrometry (GC/MS) with a 50% phenyl stationary phase. The NPLC-GC/MS method presented in this study allowed for the identification of 72 PAHs and 56 MePAHs. These identifications were based on the NPLC retention times for authentic reference standards, GC retention times for authentic reference standards, and the predominant molecular ion peak in the mass spectrum. Most noteworthy was the determination of dibenzo[a,l]pyrene, which could not be measured directly by GC/MS because of low concentration and co-elution with dibenzo[j,l]fluoranthene. The NPLC-GC/MS procedure also allowed for the tentative identification of 74 PAHs and 117 MePAHs based on the molecular ion peak only. This study represents the most comprehensive qualitative characterization of SRM 1597a to date.

NPLC-GC/MS analysis for the six-ring MM 302 Da PAH isomers in SRM 1597a

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Acknowledgements

H. Hugh and A. D. Campiglia acknowledge financial support from The Gulf of Mexico Research Initiative (Grant 231617-00). The views expressed are those of the authors and do not necessarily reflect the view of this organization.

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Authors and Affiliations

  1. Chemical Sciences Division, Material Measurement Laboratory, National Institute of Standards and Technology, 100 Bureau Drive, Mail Stop 8390, Gaithersburg, MD, 20899, USA

    Walter B. Wilson, Lane C. Sander & Stephen A. Wise

  2. Department of Chemistry, University of Central Florida, Orlando, FL, 32816, USA

    Hugh V. Hayes & Andres D. Campiglia

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  1. Walter B. Wilson
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Correspondence to Walter B. Wilson.

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Certain commercial equipment or materials are identified in this paper to specify adequately the experimental procedure. Such identification does not imply recommendation or endorsement by the National Institute of Standards and Technology, nor does it imply that the materials or equipment identified are necessarily the best available for the purpose.

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Wilson, W.B., Hayes, H.V., Sander, L.C. et al. Qualitative characterization of SRM 1597a coal tar for polycyclic aromatic hydrocarbons and methyl-substituted derivatives via normal-phase liquid chromatography and gas chromatography/mass spectrometry. Anal Bioanal Chem 409, 5171–5183 (2017). https://doi.org/10.1007/s00216-017-0464-x

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  • DOI: https://doi.org/10.1007/s00216-017-0464-x

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