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Application of mid-infrared spectroscopy for the quantitative and qualitative analysis of organic matter in Holocene sediment records
Umeå University, Faculty of Science and Technology, Department of Ecology and Environmental Sciences.ORCID iD: 0000-0001-9659-2722
Umeå University, Faculty of Science and Technology, Department of Ecology and Environmental Sciences. Forest Research Institute, Université du Québec en Abitibi-Témiscamingue, Canada.ORCID iD: 0000-0002-8208-496x
Umeå University, Faculty of Science and Technology, Department of Ecology and Environmental Sciences. Department of Environmental Systems Science, ETH Zurich, Switzerland; Department of Water Resources and Drinking Water, Eawag, Switzerland.
Umeå University, Faculty of Science and Technology, Department of Ecology and Environmental Sciences.
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2024 (English)In: The Holocene, ISSN 0959-6836, E-ISSN 1477-0911, Vol. 34, no 3, p. 259-273Article in journal (Refereed) Published
Abstract [en]

The organic matter composition of lake sediments influences important in-lake biogeochemical processes and stores information on environmental changes. Extracting this information is notoriously difficult because of the complexity of the organic matter matrix, which routinely imposes trade-offs between high temporal and analytical detail in the selection of methods of analysis. Here, we demonstrate the potential of diffuse reflectance Fourier transform infrared spectroscopy (DRIFTS) for achieving both of these objectives using untreated bulk samples from two Holocene lake-sediment cores from central Sweden. We develop quantitative models for sediment total organic carbon (TOC) with the same predictive abilities as models based on samples diluted with KBr and qualitatively characterize the organic matter using a spectra processing-pipeline combined with principal component analysis. In the qualitative analysis we identified four organic matter sub-fractions and the interpretation of these is supported and further advanced with molecular data from pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). Within these organic fractions, compound groups such as aromatics, lignin, aliphatics, proteins and polysaccharides were identified by means of DRIFTS and the analyses and processes outlined here enables rapid and detailed quantitative and qualitative analysis of sediment organic matter. The DRIFTS approach can be used as stand-alone method for OM characterization with high temporal resolution in Holocene sediment records. It may also function as a screening process for more specific analyses of sample subsets, such as when coupled with pyrolysis-GC/MS to further tease apart the OM composition, identify sources and determine degradation status.

Place, publisher, year, edition, pages
Sage Publications, 2024. Vol. 34, no 3, p. 259-273
National Category
Environmental Sciences
Identifiers
URN: urn:nbn:se:umu:diva-213750DOI: 10.1177/09596836231211872ISI: 001111087400001Scopus ID: 2-s2.0-85178427803OAI: oai:DiVA.org:umu-213750DiVA, id: diva2:1791924
Funder
Knut and Alice Wallenberg Foundation, 2016.0083Swedish Research Council, 2014-05219
Note

Originally included in thesis in accepted form. 

Available from: 2023-08-28 Created: 2023-08-28 Last updated: 2024-04-26Bibliographically approved
In thesis
1. Molecular analysis of lake-sediment organic matter: long-term dynamics and environmental implications in boreal lakes
Open this publication in new window or tab >>Molecular analysis of lake-sediment organic matter: long-term dynamics and environmental implications in boreal lakes
2023 (English)Doctoral thesis, comprehensive summary (Other academic)
Alternative title[sv]
Molekylär analys av organiskt material i sjösediment : långtidsdynamik och miljöpåverkan i boreala sjöar.
Abstract [en]

Lake sediment organic matter is material composed of residues from plants, algae, animals, fungi and bacteria. Its molecular composition is dependent on the sources as well as secondary biotic and abiotic transformations, which combined generates a highly complex matrix. Considering that organic matter plays a key role in carbon and nitrogen cycle, and its composition affects many different biogeochemical reactions, paleolimnologic studies have payed proportionately little attention to the organic matter composition compared with the other sediment fractions, even though organic matter makes up 20–60 % of the dry sediment mass in boreal and subarctic lakes. This thesis therefore primarily aims to explore and evaluate two methods; pyrolysis-gas chromatography/mass spectrometry (Pyrolysis-GC/MS) and diffuse reflectance Fourier-transform infrared spectroscopy (DRIFTS) for characterisation of bulk organic matter at the molecular level, both which have been extensively used for soils and peat and which balances the need for cost and time-effective analysis and for analytical detail.

With pyrolysis-GC/MS the organic matter composition and long-term dynamics in two neighbouring boreal lakes is explored and compared with the conventional bulk carbon and nitrogen contents and their stable isotopes. Both pyrolysis data and conventional data capture the timing of organic matter compositional changes, but only pyrolysis provides detailed information on how the composition changes, which allows for a deeper understanding of the processes behind the changes. The same two lakes are also analysed with DRIFTS and with this approach information on the major organic compound groups aromatics, lignin, aliphatics, proteins and polysaccharides is extracted. In combination with the rapid analysis time and low cost, DRIFTS emerges as a very useful tool for rapid yet informative organic matter analysis. DRIFTS is then evaluated as a stand-alone tool for sediment characterisation in four mountain lakes. The four lakes all have different sediment composition and as a result of the multi-fraction information obtained with DRIFTS compositional differences can be related and explained in terms of their individual lake and landscape settings. The importance of landscape setting is further highlighted in the synthesis of the long-term dynamics of lake-water quality in seven lakes where development trajectories and responses to different types of disturbances are connected to the extent of peatlands within the lake catchments. This thesis demonstrates the advantages of two different approaches for more detailed lake sediment organic matter characterisation and advances our understanding of the molecular organic matter composition in boreal lakes over the Holocene, and how landscape setting affects both the organic matter composition and the sensitivity of lakes to disturbance.

Place, publisher, year, edition, pages
Umeå: Umeå University, 2023. p. 23
Keywords
Lake sediment, Holocene, organic matter, Pyrolysis-GC/MS, mid-infrared spectroscopy, boreal
National Category
Environmental Sciences
Identifiers
urn:nbn:se:umu:diva-213753 (URN)978-91-8070-144-0 (ISBN)978-91-8070-145-7 (ISBN)
Public defence
2023-09-22, NAT.D.450, Naturvetarhuset, Umeå Universitet, Umeå, 09:00 (English)
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Available from: 2023-09-01 Created: 2023-08-28 Last updated: 2023-08-28Bibliographically approved

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Ninnes, SofiaMeyer-Jacob, CarstenTolu, JulieBindler, Richard

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