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Improved Polycyclic Aromatic Hydrocarbon and n-Alkane Determination in Speleothems through Cleanroom Sample Processing

  • Elena Argiriadis*
    Elena Argiriadis
    Department of Environmental Sciences, Informatics and Statistics, Ca’ Foscari University of Venice, Via Torino 155, 30172 Venice, Italy
    *E-mail: [email protected]. Tel.: +39 041 234 8658.
  • Rhawn F. Denniston
    Rhawn F. Denniston
    Department of Geology, Cornell College, 600 First Street Southwest, Mount Vernon, Iowa 52314-1098, United States
  • , and 
  • Carlo Barbante
    Carlo Barbante
    Department of Environmental Sciences, Informatics and Statistics, Ca’ Foscari University of Venice, Via Torino 155, 30172 Venice, Italy
    Institute for the Dynamics of Environmental Processes CNR-IDPA, Via Torino 155, 30172 Venice, Italy
Cite this: Anal. Chem. 2019, 91, 11, 7007–7011
Publication Date (Web):May 13, 2019
https://doi.org/10.1021/acs.analchem.9b00767
Copyright © 2019 American Chemical Society

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    Abstract

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    Interest in paleoenvironmental reconstructions from biomarkers in speleothems is increasing, thanks in part to the capacity of speleothems to grow continuously and to resist postdepositional alteration. In particular, the possibility exists to link high-resolution and accurately dated fire and vegetation records with isotopic data of climatic and paleoenvironmental interactions at the local and regional scale. However, the scarcity of existing methods for the quantification of organic molecules in stalagmites, together with the issues of sample availability, contamination, and low concentrations, complicate this approach. In this work, we developed a novel method for the simultaneous determination of 18 polycyclic aromatic hydrocarbons (PAHs) and 26 n-alkanes (C10–C35) and then tested it on “clean” calcite and aragonite stalagmite samples from cave KNI-51 in the Australian tropics. The method involves subsampling by using a hand-held drill, complete dissolution of the matrix in hydrochloric acid, then liquid–liquid extraction, and GC-MS analysis. Sample preparation was carried out in a 10 000 class clean room built entirely in stainless steel to avoid contamination. Detection limits were 0.3–9 ng for PAHs and 6–44 ng for n-alkanes. Measurable concentrations of fire-derived PAH compounds, namely, phenanthrene, pyrene, benzo(e)pyrene, and indeno(123-cd)pyrene, were detected in only one sample, which dates to the year ∼2004 CE, when a fire burned vegetation over the cave; n-alkanes were detected in all samples in the range C23–C35, with no odd–even preference.

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    • Extraction procedure and results table of PAH concentrations in cave sediments (PDF)

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    Cited By

    This article is cited by 8 publications.

    1. Robin R. Dawson, Isla S. Castañeda, Stephen J. Burns, Jeffrey M. Salacup, Nick Scroxton, David McGee, Peterson Faina, Laurie R. Godfrey, Lovasoa Ranivoharimanan. Investigating the application of organic geochemical techniques to tropical Anjohibe (Madagascar) stalagmites. Organic Geochemistry 2024, 91 , 104810. https://doi.org/10.1016/j.orggeochem.2024.104810
    2. Micheline Campbell, Pauline C. Treble, Liza K. McDonough, Sebastian Naeher, Andy Baker, Pauline F. Grierson, Henri Wong, Martin S. Andersen. Combustion Completeness and Sample Location Determine Wildfire Ash Leachate Chemistry. Geochemistry, Geophysics, Geosystems 2024, 25 (5) https://doi.org/10.1029/2024GC011470
    3. Elena Argiriadis, Rhawn F. Denniston, Stefania Ondei, David M.J.S. Bowman, Giulia Genuzio, Huong Quynh Anh Nguyen, Jamie Thompson, Mattia Baltieri, Jonathan Azenon, John Cugley, David Woods, William F. Humphreys, Carlo Barbante. Polycyclic aromatic hydrocarbons in tropical Australian stalagmites: a framework for reconstructing paleofire activity. Geochimica et Cosmochimica Acta 2024, 366 , 250-266. https://doi.org/10.1016/j.gca.2023.11.033
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    5. Micheline Campbell, Liza McDonough, Pauline C. Treble, Andy Baker, Nevena Kosarac, Katie Coleborn, Peter M. Wynn, Axel K. Schmitt. A Review of Speleothems as Archives for Paleofire Proxies, With Australian Case Studies. Reviews of Geophysics 2023, 61 (2) https://doi.org/10.1029/2022RG000790
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